FERTILISER [(INORGANIC, ORGANIC OR MIXED)] (CONTROL) ORDER, 1985

[FERTILISER [1][(INORGANIC, ORGANIC OR MIXED)] (CONTROL) ORDER, 1985]

PREAMBLE

In exercise of the powers conferred by section 3 of the Essential Commodities Act, 1955 (10 of 1955), the Central Government hereby makes the following Order, namely:-

Order - 1. Short title and commencement.

(1)     This Order may be called the Fertiliser [2][(Inorganic, Organic or Mixed)] (Control) Order, 1985.

(2)     It shall come into force on the date of its publication in the Official Gazette.

Order - 2. Definitions.

In this Order, unless the context otherwise requires:

(i)       "Act" means the Essential Commodities Act, 1955 (10 of 1955).

(aa) "Biofertiliser" means the product containing carrier based (solid or liquid) living microorganisms which are agriculturally useful in terms of nitrogen fixation, phosphorus solubilisation or nutrient mobilization, to increase the productivity of the soil and/or crop/

[3][(ab) "biostimulant" means a substance or microorganism or a combination of both whose primary function when applied to plants, seeds or rhizosphere is to stimulate physiological processes in plants and to enhance its nutrient uptake, growth, yield, nutrition efficiency, crop quality and tolerance to stress, regardless of its nutrient content, but does not include pesticides or plant growth regulators which are regulated under the Insecticide Act, 1968 (46 of 1968);]

(ii)      "certificate of source" means a certificate given by a State Government, Commodity Board, manufacturer, + importer, pool handling agency or as the case may be, wholesale dealer indicating therein the source from which fertiliser for purpose of sale is obtained.

(iii)     "Commodity Board" means the Coffee Board constituted under section 4 of the Coffee Act, 1942 (7 of 1942) or the Rubber Board constituted under section 4 of the Rubber Act, 1947 (24 of 1947), or the Tea Board constituted under section 4 of the Tea Act, 1953 (29 of 1953), or as the case may be, the Cardamom Board constituted under section 4 of the Cardamom Act, 1965 (42 of 1965).

(iv)    "compound or complex fertiliser" means a fertiliser containing two or more nutrients during the production of which chemical reaction takes place:-

(v)      "controller" means the person appointed as Controller of Fertilisers by the Central Government and includes any other person empowered by the Central Government to exercise or perform all or any of the powers, or as the case may be, functions of the Controller under this Order.

[4][(ee) "Customised Fertiliser" means a granular multi nutrient carrier which contains Primary, Secondary and /or micro nutrient forms, both from inorganic and/or organic sources, manufactured through a systematic process of Fusion blend granulation [5][or precision blend technology], formulated on the basis of soil fertility data and include 100% water soluble specialty fertilizer as customized combination products;]

(vi)    "dealer" means a person carrying on the business of selling fertilisers whether wholesale or retail or industrial use* and includes a manufacturer, +Importer, and a pool handling agency carrying on such business and the agents of such person, manufacturer, +importer or pool handling agency.

(vii)   Clause 'g' deleted vide S.O. 725 (E) dated 28.7.88.

(viii)  "fertilizer" means any substance used or intended to be used as a fertiliser of the soil and/or crop and specified in Part A of Schedule I and includes a mixture of fertilizer and special mixture of fertilizers provisional fertiliser, customised fertilizer, Bio-fertilizers specified in Schedule III and Organic fertilizers specified in Schedule IV.

[6][(h) "Fertiliser" means any essential substance, either in straight or mixed form and derived from either inorganic, organic or mixed sources, that is used or intended to be used to provide essential plant nutrients or beneficial elements or both for the soil or for the crop or makes essential plant nutrients available to the plants either directly or by biological process or by both in the soil or plant as notified from time to time by Central Government and specified in the schedules appended to this order or as may be notified by the State Governments [7][and includes a biostimulant] [8][and nano fertiliser].

Explanation:-For the purpose of Fertiliser,-

(i)       "the essential plant nutrients" include Primary Nutrients (Nitrogen, Phosphorous and Potassium), Secondary Nutrients (Calcium, Magnesium and Sulphur) and Micro Nutrients (Zinc, Manganese, Copper, Iron, Boron and Molybdenum);

(ii)      "Beneficial element" means any element as notified by the Central Government from time to time.;]

(i) "Form" means a form appended to this Order.

(j) "grade" means the nutrient element contents in the fertiliser expressed in percentage.

(k) "granulated mixture" means a mixture of fertilisers made by intimately mixing two or more fertilisers with or without inert material, and granulating them together, without involving any chemical reaction.

(Kk) "importer" means a person who imports fertiliser in accordance with the Export and Import Policy of the Central Government, as amended from time to time.

I.         "inspector" means an Inspector of Fertilisers appointed under clause 27.

II.       "industrial dealer" means a dealer who sells fertilisers for industrial purposes.

III.     "industrial purposes" means the use of fertiliser for purposes other than fertilisation of soil and Increasing productivity of crops.

(m) "manufacturer" means a person who produces fertilisers or mixtures of fertilisers and the expression "manufacture" with its grammatical variations shall be construed accordingly.

[9][(mb) the mixture of micronutrient are those which are made by mixing of micronutrient notified in Schedule-I under the sub-heading "1(g) MICRONUTRIENTS" of said Order.]

(n) "mixture of fertilisers" ***means a mixture of fertilisers made by physical mixing two or more fertilisers with or without inert material in physical or granular form and includes a mixture of NPK fertilisers, a mixture of micronutrient fertilisers and a mixture of NPK with micronutrient fertilisers.

(nn) Notified Authority "means an authority appointed under clause 26 A.

(n) "offer for sale" includes a reference to an intimation by a person of a proposal by him for the sale of any fertiliser, made by publication of a price list, by exposing the fertilizer for sale indicating the price, by furnishing of a quotation or otherwise howsoever.

[10][(na) "nano fertiliser" means the fertiliser of nano scale complying with the specifications as provided in clause 20 D]

(nna) "Non-edible de-olied cake fertiliser" means substances obtained as residue after oli extraction (by expeller and/ or thought solvent extraction) form crused seeds of non-edible oilseeds [11][including Castor, Neem, Karanj (Pongamiapinnata), Mahua (madhucalongifolia) and Jatropha] for use in soil as fertilizer.

(oo) Organic fertilizer means substances made up of one or more unprocessed materials of a biological nature (plant/animal) and may include unprocessed mineral materials that have been altered through microbiological decomposition process.

(p) 'physical mixture" means a mixture of fertilisers made by physically mixing two or more fertilisers with or without inert material necessary to make a required grade, without involving any chemical reaction.

(pp) "Provisional fertilizer" means fertilizer specified under clause 20 A.

(q) "prescribed standard" means:-

i.         in relation to a fertiliser included in column 1 of Part A of Schedule-I, the standard set out in the corresponding entry in column 2, subject to the limits of permissible variation as specified in Part B of that [12][Schedule and includes all such fertilizers whose standards are specified in such Schedule and are fortified with such micronutrients as given below.

Explanation:- The specification of the fertilizer which shall be fortified with above mentioned micronutrient shall remain the same as specified in Schedule -I.]

ii.        in relation to a mixture of fertilisers, the standard set out in respect of that mixture under sub-clause (1) of clause 13 by the Central Government, subject to the limits of permissible variation as specified in Part B of Schedule-I

iii.       in relation to mixture of fertilisers, standard set out in respect of that mixture under sub-clause (2) of clause 13 by the State Government, subject to limits of permissible variation as specified in Part B of Schedule-I.

iv.       in relation to a Biofertiliser included in column 1 of Part A of Schedule-III, the standard set out in the corresponding entry in column 2, subject to the limits of permissible variation as specified in Part B of that Schedule;

v.        in relation to a Organic fertiliser included in column 1 of Part A of Schedule-IV, the standard set out in the corresponding entry in column 2, subject to the limits of permissible variation as specified in Part B of that Schedule.

vi.       In relation to a non-edible de-oiled cake fertiliser specified in column (2) of Part A of Schedule V, the standard set out in the corresponding entry in column (2) of the said part, subject to the limits of permissible variation as specified in part B of the said Schedule.]

vii.      [13][prescribed standard means in relation to Customised Fertilizers, standards set out in respect of Customised Fertilizers under clause 20B by the Central Government, subject to limits of permissible variation as specified in part B of Schedule I]

viii.    [14][in relation to a biostimulant included in column (2) of Part-A of Schedule VI, the standard set out in the corresponding entry in column (3), subject to the limits of permissible variations as specified in Part-B of the said Schedule;]

ix.       [15][in relation to a nano fertiliser, means the specifications set out under clause 20D;]

(r) "pool handling agency" means an agency entrusted by the Central Government with functions relating to handling and distribution of imported fertilisers.

(s) "registering authority" means a registering authority appointed under clause 26 in respect of mixture of fertilizers and special mixture of fertilizers

(t) "retail dealer" means a dealer who sells fertilisers to farmers or plantations for **agricultural use such as for fertilisation of soil and increasing productivity of crops.

(u) "Schedule" means a Schedule appended to this Order.

(v) "special mixture of fertilisers" means any mixture of fertilisers prepared for experimental purposes in pursuance of a requisition made by any person (including a person engaged in the cultivation of tea, coffee or rubber) for sale to that person in such quantity and within such period as may be specified in such requisition; and.

(w) "wholesale dealer" means a dealer who sells fertilisers otherwise than in retail-for agricultural use such as for fertilisation of soil and increasing productivity of crops.

II. PRICE CONTROL

Order - 3. Fixation of prices of fertilisers.

(1)     The Central Government may, with a view to regulating equitable distribution of fertilisers and making fertilisers available at fair prices, by notification in the Official Gazette, fix the maximum prices or rates at which any fertiliser may be sold by a dealer, manufacturer, importer or a pool handling agency.

 

(2)     The Central Government may having regard to the local conditions of any area, the period of storage of fertilisers and other relevant circumstances, fix different prices or rates for fertilisers having different periods of storage or for different areas or for different classes of consumers.

 

(3)     No dealer, manufacturer +importer or pool handling agency shall sell or offer for sale any fertiliser at a price exceeding the maximum price or rate fixed under this clause.

Order - 4. Display of stock position and price list of fertilisers.

Every dealer, who makes or offers to make a retail sale of any fertilisers, shall prominently display in his place of business:-

(a)      the quantities of opening stock of different fertilisers held by him on each day;

Explanation -The actual stocks at any point of time during the day may be different from that of the displayed opening stocks to the extent of sale and receipt of such fertilisers upto the time of inspection during that day

(b)      a list of prices or rates of such fertilisers fixed under clause 3 and for the time being in force.

Order - 5. Issue of cash/credit memorandum.

(a)      Every dealer shall issue a cash or credit memorandum to a purchaser of a fertiliser in Form M*

III. CONTROL ON DISTRIBUTION OF FERTILISERS BY MANUFACTURER/IMPORTER

Order - 6. Allocation of fertilisers to various States.

The Central Government may, with a view to securing equitable distribution and availability of fertilisers to the farmers in time, by notification in the Official Gazette, direct any manufacturer/importer to sell the fertilisers produced by him in such quantities and In such State or States and within such period as may be specified in the said notification.

IV. AUTHORISATION OR REGISTRATION OF DEALERS"

Order - 7. Registration of Industrial dealers and authorization of other dealers.

No person shall sell, offer for sale or carry on the business of selling of fertilizer at any place as wholesale dealer or retail dealer except under and in accordance with clause 8 :

Provided that a State Government may, if it considers it necessary or expedient, by notification in the Official Gazette, exempt from the provisions of this clause any person selling fertilizer to farmers in such areas and subject to such conditions as may be specified in that notification.

Order - 8. Application for intimation or registration.

(1)     Every person intending to sell or offer for sale or carrying on the business of selling of fertilizer as Industrial Dealer shall obtain a certificate of registration from the controller by making an application in Form A together with the fee prescribed under clause 36 and a Certificate of source in Form O.

(2)     Every person including a manufacturer, an importer, a pool handling agency, wholesaler and a retail dealer intending to sell or offer for sale or carrying on the business of selling of fertilizer shall make a Memorandum of Intimation to the Notified Authority, in Form A1 duly filled in, in duplicate, together with the fee prescribed under clause 36 and certificate of source in Form O.

(3)     On receipt of a Memorandum of Intimation, complete in all respects, the Notified Authority shall issue an acknowledgement of receipt in Form A2 and it shall be deemed to be an authorization letter granted and the concerned person as authorised dealer for the purposes of this Order.

Provided that a certificate of registration granted before the commencement of the Fertiliser (Control) Amendment Order, 2003, shall be deemed to be an authorization letter granted under the provisions of this Order:

Provided further that where the applicant is a State Government, a manufacturer or an importer or a pool-handling agency, it shall not be necessary for it or him to submit Form O.

Provided also that a separate Memorandum of Intimation shall be submitted by an applicant for whole sale business or retail dealership, as the case may be:

Provided also that where fertilizers are obtained for sale from different sources, a certificate of source from each such source shall be furnished in Form O."

[16][Provided also that where the manufacturer of organic fertilizer is a State Government or municipality, it shall not be necessary for it to obtain the authorisation letter:

Provided also that where the manufacturer of vermi-compost, other than a State Government or municipality, has annual production capacity less than 50 metric tonnes, it shall not be necessary for him to obtain the authorisation letter.]

[17][Provided also that the manufacturer of Fermented Organic Manure and Liquid Fermented Organic Manure, shall not be required to obtain the authorisation letter under sub-clause (3) of clause 8 of the said Order for a period of three years from the date of issue of notification.]

(4)     [18][No authorisation letter shall be granted to any applicant for retail dealership, unless the applicant possess the certificate course of fifteen days from any State Agriculture University or Krishi Vigyan Kendras or National Institute of Agricultural Extension Management (MANAGE) or National Institute of Rural Development and Panchayati Raj (NIDPR) or Fetiliser Association of India or any other approved Government Institute:

Provided that a person in possession of Bachelor of Science in Agriculture or chemistry or Diploma in Agriculture Science from a recognised University or Institute or equivalent course having one of the subject on fertiliser or agri inputs, as notified by the State Government shall not be required to possess separate certificate course:

Provided further that a dealer who has been granted authorisation letter before commencement of the Fertiliser (Inorganic, Organic or Mixed) (Control) Fourth Amendment Order, 2018 shall not be required to possess the qualification at the time of renewal of their authorisation letter:

Provided also that the said qualification shall not be applicable for renewal of the authorisation letter of the registered Agricultural Cooperative Societies and State Marketing Federations subject to condition that such Society or Federation shall engage a person who possesses the qualification under this clause.]

Order - 9. Grant or refusal of certificate of registration.

The Controller, shall grant a certificate of registration in Form 'B' within thirty days of the receipt of application to any person who applies for it under clause 8;

Provided that no certificate of registration shall be granted to a person: -

(a)      if his previous certificate of registration is under suspension; or

 

(b)      if his previous certificate of registration has been cancelled within a period of one year immediately preceding the date of application; or

 

(c)      if he has been convicted of an offence under the Act, or any Order made there under within three years immediately preceding the date of making the.

 

(d)      if he fails to enclose with the application a certificate of source ; or

 

(e)      if the application is incomplete in any respect; or

 

(f)       if he makes an application for obtaining the certificate of registration for industrial dealer and, excepting if he is a manufacturer ,+ importer or pool handling agency, holds an authorization letter for wholesale dealer or retail dealer or both, and as the case may be, the vice-versa.

Order - 10. Period of validity of certificate of registration and letter of authorization.

Every certificate of registration granted under clause 9 and every authorization letter issued under clause 8 shall, unless renewed, suspended or cancelled, be valid for a period of [19][five years] from the date of its issue.

[20][Notwithstanding anything contained in the said clause, the letter of Authorisation granted to the manufacture of City Compost issued under clause 8, unless suspended or cancelled is valid in perpetuity.]

Order - 11. Renewal of certificates of registration and authorization letters.

(1)     Every holder of a certificate of registration granted under clause 9 or authorization letter granted or deemed to have been granted under clause 8, desiring to renew such certificate or authorization letter shall, before the date of expiry of such certificate of registration or authorization letter, as the case may be, make an application for renewal to the Controller, in Form C, or to the Notified Authority in Form A1, respectively, in duplicate, together with the fee prescribed under clause 36 for such renewal and a certificate of source as required under clause 8.

 

(2)     On receipt of an application under sub-clause (1), together with such fee and certificate of source, the controller may renew the certificate of registration or the Notified Authority, as the case may be shall issue acknowledgement receipt of renewal in form A 2. Provided that a certificate of registration shall not be renewed if the holder of the same did not sell any fertiliser during the period of one year immediately preceding the date of expiry of the period of validity.

 

(3)     If any application for renewal is not made before the expiry of the period of validity of the certificate of registration or, as the case may be, the authorization letter but is made within one month from the date of such expiry, the certificate of registration or, as the case may be, the authorization letter shall be dealt as provided in sub-clause (2) on payment of such additional fee as may be prescribed under clause 36 in addition to the fee for renewal.

 

(4)     Where the application for renewal of certificate of registration is made within the time specified in sub- clause (1) or sub-clause (3), the applicant shall be deemed to have held a valid certificate of registration until such date as the controller passes orders on the application for renewal.

 

(5)     If an application for renewal of a certificate of registration or authorization letter is not made within one month from the date of expiry of their period of validity, the same shall be deemed to have lapsed on the date on which its validity expired and any business carried on after that date shall be deemed to have been carried on in contravention of clause 7.

V. MANUFACTURE OF MIXTURES OF FERTlLIZERS, ORGANIC FERTILISER AND BIO- FERTILISER

Order - 12. Restriction on preparation of mixtures of fertilizer.

No person shall carry on the business of preparing any mixture of fertilisers or special mixture of fertilizers, Bio-fertilizers or Organic fertilisers except under and in accordance with the terms and conditions of a certificate of manufacture granted to him under clauses 15 or 16.

Order - 13. Standards of mixtures of Fertilisers.

(1)     Subject to the other provisions of the order

(a)      no person shall manufacture any *mixture of fertilisers whether of solid or liquid fertilizers specified in Part a of schedule I unless such mixture conforms to the standards set out in the notification to be issued by the Central Government in the Official Gazette;

 

(b)      no person shall manufacture any biofertiliser unlessl such biofertiliser conforms to the standards set out in the part A of Schedule - III.

 

(c)      no person shall manufacture any Organic fertilizer unless such organic fertilizer conforms to the standards set out in the part A of Schedule IV.

(2)     Subject to the other provisions of this order, no person shall manufacture any "mixture of fertilisers unless such mixture conforms to the standards set out in the notification to be issued by the State Government in the Official Gazette;

Explanation- For the purposes of this sub-clause, mixture of fertilizers shall not include liquid fertilizers and 100% water soluble fertilizers, containing N,P,K.

(3)     [omitted]

(4)     No Certificate of manufacture shall be granted in respect of any fertiliser which does not conform to the standards set out in the notification referred in sub- clause (1) or (2);

(5)     Nothing in this clause shall apply to special mixtures of fertilisers

Order - 14. Application for certificate of manufacture of mixtures of fertilisers.

(1)     Every person desiring to obtain a certificate of manufacture for preparation of any mixture of fertilisers or special mixture of fertilisers shall possess such mixture, *and possess the minimum laboratory facility as specified in clause 21A of this Order.

(2)     An applicant for a certificate of manufacture for preparation of mixture of fertilisers or special mixture of fertilisers shall make an application to the registering authority

(a)      if he is an applicant for a certificate of manufacture for any mixture of fertilisers in Form D, in duplicate, together with the fee prescribed there for under clause 36; or,

(b)      if he is an applicant for a certificate of manufacture for any special mixture, in Form E, in duplicate, together with the fee prescribed there for under the said clause 36 and an attested copy of the requisition of the purchaser.

(3)     Every person desiring to obtain a Certificate of Manufacture for preparation or organic fertilizer or biofertiliser shall make an application in Form D, in duplicate, together with a fee prescribed therefore under clause 36, to Registering authority.

[21][Provided that where the manufacturer of organic fertilizer is a State Government or a municipality, it shall not be necessary for it to obtain the Certificate of Manufacture:

Provided further that where the manufacturer of vermi-compost, other than a State Government or municipality, has annual production capacity less than fifty metric tonnes, it shall not be necessary for him to obtain the Certificate of Manufacture for preparation of vermi-compost.]

Order - 15. Grant or refusal of certificate of manufacture for preparation of mixtures of fertilizers, Biofertilisers or Organic fertilizer..

(1)     On receipt of an application under clause 14, the registering authority shall, by order in writing, either grant or refuse to grant the certificate of manufacture in respect of any mixture of fertilizer, Biofertiliser, Organic fertiliser or special mixture of fertilizer and shall, within forty-five days from the date of receipt of the application, furnish to the applicant a copy of the order so passed;

(2)     Where an application for a certificate of manufacture for mixture of fertilizers, Biofertiliser, Organic fertiliser is not refused under sub-clause (1), the registering authority shall grant a certificate of manufacture in Form F and where an application for a certificate of manufacture for a special mixture is not refused under that sub-clause, *[such authority shall within forty five dates from the date of receipt of the application, ]grant a certificate of manufacture to the applicant in Form G

Order - 16. Conditions for grant of certificate of manufacture in respect of special mixture of fertilisers and period of validity of such certificate.

(1)     No certificate of manufacture in respect of any special mixture of fertilisers shall be granted to an applicant unless he holds a valid certificate of manufacture under this Order for any mixture of fertilisers.

(2)     Every certificate of manufacture granted in respect of any special mixture of fertilisers shall be valid for a period of six months from the date of its issue;

Provided that the registering authority may, if it is satisfied that it is necessary so to do, extend the said period to such further period or periods as it may deem fit, so however, that the total period or periods so extended shall not exceed twelve months.

Order - 17. Period of validity of a certificate of manufacture for preparation of mixtures of fertilizers, Biofertilisers or Organic fertilizer.

Every certificate of manufacture granted under clause 15 for preparation of a mixture of fertilizers, Biofertiliser or Organic fertilizers shall, unless suspended or cancelled, be valid for a period of three years from the date of issue.

Order - 18. Renewal of certificate of manufacture for preparation of mixtures of fertilizers, Biofertiliser or Organic fertiliser.

(1)     Every holder of a certificate of manufacture for preparation of a mixture of fertilizers, Biofertiliser, Organic fertiliser desiring to renew the certificate, shall, before the date of expiry of the said certificate of manufacture make an application to the registering authority in Form D in duplicate, together with the fee prescribed for this purpose under clause 36.

 

(2)     On receipt of an application for renewal as provided in sub-clause (1), and keeping in view the performance of the applicant and other relevant circumstances, the registering authority may, if he so decides, renew the certificate of manufacture by endorsement on Form F and in case the certificate of registration is not renewed, the registering authority shall record in writing his reasons for not renewing the certificate of manufacture.

 

(3)     If an application for renewal is not made before the expiry of the certificate of manufacture but is made within one month from the date of expiry of the certificate of manufacture, the certificate of manufacture may be renewed on payment of such additional fee as may be prescribed by the State Government for this purpose.

 

(4)     Where the application for renewal is made within the time specified in sub-clause (1) or sub-clause (3), the applicant shall be deemed to have held a valid certificate of manufacture until such date as the registering authority passes order on the application for renewal.

 

(5)     If an application for renewal of a certificate of manufacture is not made within the period stipulated under sub-clause (1) or, as the case may be, under sub-clause (3), the certificate of manufacture shall be deemed to have expired immediately on the expiry of its validity period, and any business carried on after that date shall be deemed to have been carried on in contravention of clause 12.

VI. RESTRICTIONS ON MANUFACTURE/ IMPORT, SALE, ETC. OF FERTlLISER

Order - 19. Restriction on manufacture/import, sale and distribution of fertilisers.

No person shall himself or by any other person on his behalf:-

(a)      manufacture/import for sale, sell, offer for sale, stock or exhibit for sale or distribute any fertlliser which Is not of prescribed standard;

(b)      manufacture/Import for sale, sell, offer for sale, stock or exhibit for sale, or distribute any mixture of fertilisers, which is not of prescribed standard** (subject to such limits of permissible variation as may be specified from time to time by the Central Government) or special mixture of fertilisers which does not conform to the particulars specified In the certificate of manufacture granted to him under this Order in respect of such special mixture.

(c)      sell, offer for sale, stock or exhibit for sale or distribute:-

(i)       any fertiliser the container whereof is not packed and marked in the manner laid down In this Order

(ii)      any fertiliser which is an [imitation of or] a substitute for another fertiliser under the name of which It Is sold;

(iii)     any fertiliser which Is adulterated;

Explanation:- A fertiliser shall be deemed to be adulterated, If It contains any substance the addition of which is likely to eliminate or decrease Its nutrient contents or make the fertiliser not conforming to the prescribed standard.

(iv)    any fertiliser the label or container whereof bears the name of any individual firm or company purporting to be manufacturer/Importer of the fertiliser, which individual, firm or company Is fictitious or does not exsist.

(v)      any fertiliser, the label or container whereof or anything accompanying therewith bears any statement which makes a false claim for the fertiliser of which s false or misleading in any material particular.

(vi)    any substance as a fertiliser which substance is not, in fact, a fertiliser; or

(vii)   any fertiliser without exhibiting the minimum guaranteed percentage by weight of plant nutrient.

[22][Provided that specifications of city compost in Schedule IV shall, in case of municipalities, be applicable only when it is traded in packaged form for use in agriculture:

Provided further that the specifications of vermi-compost in Schedule IV shall be applicable only in such cases where it is sold in packaged form and for agricultural purposes.]

Order - [19A.

In cases where the samples were drawn from the dealers out of original sound bags (without any mark of tempering) and are found non-standard, then in such circumstances both dealer and manufacturer shall be made party for filling the case in the concerned court under the Act and proceedings under clause 31 of this Order.][23]

Order - 20. Specifications In respect of imported fertilisers.

Notwithstanding anything contained in this Order, the Central Government may by an order, published in the Official Gazette, fix separate specifications in respect of imported fertilisers [24][which shall valid for a period not exceeding three years].

Order - 20A. Specification in respect of provisional fertilizer

Notwithstanding anything contained in this Order, the Central Government may, by order published in the Official Gazette, notify specifications, valid for a period not exceeding three years, in respect of fertilizers to be manufactured by any manufacturing unit for conducting commercial trials.

Order - 20B.[Specification in respect of Customised Fertiliser.-

(i)       Notwithstanding anything contained in this Order, the Central Government may by notification in the Official Gazette notify the General specification of customised fertiliser [25][which shall valid for a period not exceeding four years][26].

(ii)      No person shall manufacture any grade of Customised Fertiliser unless such customised fertiliser conforms to the standards set out in the notification to be issued by the Central Government in the Official Gazette under sub-clause (i):

Provided that the grades of customized fertiliser, which the company will manufacture, must be based on the soil fertility data maintained by the Ministry of Agriculture and Farmers Welfare or State Governments:

Provided further that in case, the data for a district for which the company intending to formulate the grade is not available or still under process by the State Government, then the company shall use the scientific data obtained from soil testing results generated by testing in their own laboratories.

(iii)     No person, except with the prior permission of Controller shall, manufacture any particular grade of customized fertilizer formulated as per the General specification notified under sub-clause (i).

(iv)    Every person, desirous of obtaining a specific product approval of any particular grade of customised fertilizer, shall make an application in form Q in duplicate to the Controller of Fertiliser, Government of India.

(v)      On receipt of application under clause (ii), the Controller shall by order in writing either grant or refuse to grant the permission, in respect of manufacturing of any particular grade of customised fertiliser and shall within three months from the date of receipt of application shall furnish a copy of order so passed to the applicant:

Provided that on completion of three years or earlier, manufacturing company of customised fertiliser shall again submit an application for approval for manufacturing of the said grade:

Provided further that the permission for manufacture and sale of Customised Fertiliser shall be granted to only such Fertiliser Companies whose annual production of fertilisers other than CFs is 5.00 lakh metric tonne:

Provided also that such manufacturing companies, having annual production of 5 LMT of fertilizer other than CFs, can set up manufacturing units of CF either on their own or through subsidiaries or joint venture through a minimum stake of 51% in such joint ventures.]

Order - [20C. Specifications in respect of biostimulants.

(1)     Notwithstanding anything contained in this Order, the specifications of biostimulants, including its name, active ingredients or where it is not possible to indicate its active ingredients, then its chemical composition, name of the crop to which it may be applied, its benefits and the method of analysis for determination of its active ingredients or chemical composition shall be specified by the Central Government in Schedule VI.][27]

(2)     The biostimulants specified in Schedule VI shall be classified under any of the following categories, namely:

(i)       botanical extracts, including seaweed extracts;

 

(ii)      bio-chemicals;

 

(iii)     protein hydrolysates and amino acids;

 

(iv)    vitamins;

 

(v)      cell free microbial products;

 

(vi)    antioxidants;

 

(vii)   anti-transpirants;

 

(viii)  humic and fulvic acid and their derivatives

(3)     Notwithstanding anything contained in this order, every manufacturer or importer of a biostimulant shall make an application to the Controller in Form G along with the following data relating to such product for specifying it as a biostimulant in Schedule VI, namely;

A.        Chemistry:

(1)     Source (natural extracts of plant/microbe/animal/synthetic)

 

(2)     Product Specification (with analysis from Good Laboratory Practice (GLP) or National Accreditation Board for Testing and Calibration Laboratory (NABL) accredited laboratory, Physical  and Chemical properties of active ingredients and adjuvants, if any.

 

(3)     Method of analysis conforming to the specifications.

 

(4)     Shelf-life;

B.        Bio-efficacy Trials:

1.        Agronomic Bio-efficiency trials shall be conducted at National Agricultural Research System, including Indian Council of Agricultural Research, State Agricultural Universities.

2.        Bio-efficacy trials shall be conducted at minimum three different doses for one season at three agro-ecological locations;

C.        Toxicity: Name of the Institute (where the manufacturer of biostimulant obtained the certificate)

The test report along with recommendation of following five basic acute toxicity tests (i) to (v) and four Eco toxicity tests (vi) to (ix) of GLP accredited laboratory shall be submitted along with the application, namely:-

(i)       Acute oral (Rat)

 

(ii)      Acute dermal (Rat)

 

(iii)     Acute Inhalation (Rat)

 

(iv)    Primary skin Irritation (Rabbit)

 

(v)      Eye irritation (Rabbit)

 

(vi)    Toxicity to bird

 

(vii)   Toxicity to Fish (Freshwater)

 

(viii)  Toxicity to honeybee

 

(ix)    Toxicity to earthworm

Note:-Long-term chronic studies as in case of pesticides are not needed to be conducted;

D.       Heavy metal analysis report;

E.        The sample of the product along with an Affidavit by the manufacturer or importer on non-judicial stamp paper of rupees ten stating that the product is not laced with pesticide beyond permissible limit of 0.01ppm

Provided that in case of a biostimulant having natural origin or other, the requirement of necessary data shall be as decided by the Central Biostimulants Committee as per the guidelines formulated by it in this regard:

Provided further that every manufacturer or importer of a biostimulant shall, notwithstanding that such biostimulant has been specified in Schedule VI, be required to make an application under this sub-clause

(4)     Notwithstanding anything contained in this order, any person manufacturing [28][or importing] a biostimulant as on the date of publication of this order for which no standards have been specified, may, subject to making an application for grant of provisional registration under sub-clause (5), [29][continue to manufacture or import] for sale, sell, offer for sale, stock or exhibit such biostimulant for a period of two years [30][four years] from the date of publication of this order.

(5)     The manufacturer [31][or importing] referred to in sub-clause (4) shall, [32][31st March, 2023], submit an application to the Controller for grant of provisional registration in Form G-1 along with

(a)      details of the product, its specifications, label and such other particulars as may be required;

(b)      a certificate issued by the State Government in Form G-2 to the effect that

(i)       the product is available in the market prior to the publication of the said order; and

(ii)      no incident has come to its notice about harmful effect of the product.

(6)     On receipt of an application under sub-clause (5) for provisional registration, the Controller shall, by an order in writing, grant a provisional certificate of registration of biostimulant in Form G-3.

(7)     No person shall manufacture or import any biostimulant unless such biostimulant is included in schedule VI.

(8)     The Controller shall, by notification in the Official Gazette, publish the name of the manufacturer or importer of the biostimulant included in Schedule VI.

(9)     No biostimulant shall contain heavy metals content over and above the following maximum limit prescribed for various metals, namely,

(10)   No biostimulant shall contain any pesticide beyond the permissible limit of 0.01ppm.]

Order - [20D.

(1)     "Notwithstanding anything contained in this Order, the Central Government may, by order published in the Official Gazette, notify specifications, valid for a period not exceeding three years, conforming to the general specifications as specified in Schedule VII, in respect of nano fertilisers to be manufactured by such manufacturing unit, as may be specified therein.

 

(2)     No person shall manufacture any nano fertiliser unless such fertiliser conforms to the standard set out in the order issued under sub-clause (1).

 

(3)     Every person, desirous of obtaining approval of any nano fertiliser shall make an application in Form-G-4 in duplicate to the Controller along with a report of the State Agriculture University or of the Indian Council of Agricultural Research on multi-locational and multi crop bio-efficacy trial of minimum one season and also a report from any of the NABL accredited laboratories on biosafety, biotoxicity and quality trial as per the guidelines issued by the Department of Bio-Technology.

 

(4)     Every manufacturer shall inform the Central Government and the Director (Agriculture) of the concerned State Government as to where it intends to make said fertiliser available to the farmers.

 

(5)     Every manufacturer shall ensure training to farmers on the safety aspects of the use of nano fertiliser.

 

(6)     Every manufacturer shall print necessary precautions on the label of the container of the nano fertiliser or on a separate leaflet to be packed with the nano fertiliser.

 

(7)     Every manufacturer shall provide to the Central Government a test report of each batch from any of the NABL accredited Laboratories before its distribution or dispatch of nano fertiliser.

 

(8)     Every manufacturer shall print the batch number on the container or shall have the label securely affixed on the container having weight less than 5 litre.][33]

Order - 21. Manufacturers/Importers pool handling agencies to comply with certain requirements in regard to packing and marking, etc.

every manufacturer/importer and pool handling agency shall, in regard to packing and marking of containers of fertilisers, Biofertiliser or Organic fertiliser comply with the following requirements, namely:-

(a)      Every container in which any fertiliser is packed shall conspicuously be superscribed with the word "FERTILISER" and shall bear only such particulars and unless otherwise required under any law nothing else, as may from time to time, be specified by the Controller in this behalf, and;]

(aa) Every container in which any Biofertiliser or Organic fertilizer is packed shall conspicuously be superscribed with the word "BIO-FERTILISER/ ORGANIC FERTILISER" and shall bear only such particulars and unless otherwise required under any law nothing else, as may from time to time, be specified by the Controller in this behalf,

Provided that in case of containers the gross weight of which is 5 kg or less, no such printing of superscription and other particular shall be necessary if such super superscription and other particulars are printed on a separate label which is securely affixed to such container.

(b)      Every container shall be so packed and sealed that the contents thereof cannot be tampered with without breaking the seal;

Provided that where fertilizer manufactured in India are packed in bags stitched on hand, such bags shall bear lead seals, so that the contents thereof cannot be tampered with without breaking the seals;

Provided further that lead sealing shall not be necessary:-

(i)       if such bags are machine stitched in such a manner that contents thereof cannot be tampered with without a visible break in the stitching; and

(ii)      in the case of fertilizers imported from abroad and packed a in bags stitched in hand, in such a manner that the contents thereof cannot be tampered with without visible break in the stitching.

Provided also that in case fertilizer bags are in cut, torn or damaged condition during transportation or mishandling during loading or unloading operation, the manufacturer of such fertilizer may, under intimation to the State Government and the Central Government, repack he fertilizer in new bags or restandardise the quantity in terms of declared weight.

(c)      Every fertiliser bag in which any fertiliser is packed for sale shall be of such weight and size as may be specified by the Central Government from time to time in this behalf

(d)      [34][every container in which any biostimulant is packed shall be conspicuously superscribed with the word "Biostimulant" and shall bear only such particulars as the Central Government may, by notification in the Official Gazette, specify in this behalf, unless any other particulars are required under any other law for the time being in force.]

Order - 21A. Manufacturers to comply with certain requirements for laboratory facilities.

Every manufacturer shall, in order to ensure quality of their product, possess minimum laboratory facility, as may be specified from time to time by the Controller.

Order - 22. Bulk sale of fertilisers.

Notwithstanding anything contained In this Order:-

(a)      a retail dealer may retain at any time one bag or container of each variety of fertiliser in an open and unsealed condition for the purpose of sale;

 

(b)      a manufacturer/importer may sell the fertiliser manufactured/imported by him in bulk to a manufacturer of mixture of fertilisers, compound / complex fertilisers or special mixture of fertilisers; and

 

(c)      the Central Government may by notification published in the Official Gazette in this behalf authorise a manufacturer/importer to sell any fertiliser manufactured/ imported by him In bulk also direct to farmers for such period as may be specified in that notification: 

[35][Provided that where the municipality is the manufacturer of city compost, it shall not for the Central Government to notify it for bulk sale;

Provided further that a certificate indicating the minimum guaranteed percentage of plant nutrients is issued by the manufacturer/importer to each farmer at the time of such sale.]

Order - 23. Disposal of non-standard fertilisers.

(1)     Notwithstanding anything contained In this Order, a person may sell, offer for sale, stock or exhibit for sale or distribute, [any fertiliser except any fertiliser imported by the Central Government] which, not being an adulterated fertiliser, does not conform to the prescribed standard (hereinafter in this Order referred to as non-standard fertiliser) subject to the conditions that:

(a)      the container of such non-standard fertilizer is conspicuously superscribed in red colour with the words "non-standard" and also with the sign "X"; and

 

(b)      an application for the disposal of non-standard fertilisers in Form H is submitted to the [Notified authority] to grant a certificate of authorisation for sale of such fertilisers and a certificate of authorisation with regard to their disposal and price is obtained in Form I.

 

(c)      such non-standard fertiliser shall be sold only to the manufacturers of mixtures of fertilisers or special mixtures of fertilisers or research farms of Government or Universities or such bodies.

(2)     The price per unit of the non-standard fertiliser shall be fixed by the [notified authority] after satisfying itself that the sample taken is a representative one, and after considering the nutrient contents in the sample determined on the basis of a chemical analysis of the non-standard fertilizer.

(3)     The Central Government may, by notification in the official Gazette and subject to the conditions, if any, laid down in that notification, and subject to guidelines issued in this regard by the Central Government exempt such pool handling agencies, as it deems fit, from complying with conditions laid down in paragraphs (a) and (b) of the sub-clause (1)

(4)     Where any fertiliser imported by the Central Government is found to be of non-standard and the Central Government decides that the fertilizer cannot be permitted for direct use in agriculture, it may permit the use of such fertiliser by manufacturers of complex fertilisers, mixture of fertilisers or special mixture of fertilisers to be sold at such price as may be fixed by the Central Government.

(5)     If a manufacture or importer detects or as reasonable doubt about the standard of the fertilizer manufactured or imported by him, and dispatched for sale as deteriorated in quality during transit due to natural calamity and is not of the prescribed standards, he may, within fifteen days from the date of dispatch from factory or port, apply with detailed justifications to the Central Government for obtaining permission for reprocessing the same in a factory to meet the prescribed standards and the Central Government may, after considering the facts, permit the re-processing of such fertilizer on the terms and conditions as may be notified by the Central Government in this behalf.

Provided that no such application for permission to reprocess the fertilizer by the manufacturer or importer shall be accepted by the Central Government after the expiry of the said period of fifteen days.

[36][6. Disposal of Biofertilizers (non-standard or expired)

Notwithstanding anything contained in this (Order), every manufacturer shall recycle the carrier based biofertiliser after sterilisation of the stock lying at manufacture's site, is not of prescribed standard (hereinafter referred as non-standard), or can dispose solid or liquid biofertiliser or both by spraying or by sprinkling over the compost piles or windrows; in case of liquid biofertiliser it shall be destroyed by autoclaved first and then spread or sprinkled on the soil in nearby fields.]

Order - [23A. Reprocessing of fertiliser damaged during storage.-

(1)     Notwithstanding anything contained in this order, where the stock of fertiliser damaged during its storage, the manufacturer or the importer of such fertiliser may make an application for grant of certificate of reprocessing in Form I-1 along with prescribed fee to the Notified Authority for reprocessing such fertiliser in the manufacturing unit of such manufacturer or the unit mentioned by the importer in his application.

(2)     The Notified Authority may, on being satisfied, allow the application made under sub-clause (1) and grant the certificate of reprocessing in Form-I-2, subject to the following conditions, namely:-

(a)      the container of such damaged material shall be conspicuously superscribed in red color with the word "Damaged" and also with sign "X".

(b)      the damaged fertiliser shall be moved from the godown within one week from the date of grant of certificate of reprocessing.][37]

Order - [23B. Disposal of Damaged and Expired stock of Bio-fertilisers/Organic fertilisers.-

(1)     Notwithstanding anything contained in this order where the stock of biofertiliser damaged during storage or expired or does not conform to the prescribed standard at dealer end or during transit from manufacturing unit to dealer end, such material shall be taken back by manufacturer or returned by dealer by intimating to the Notified authority within seven days, in case where the material is damaged during transit or in case where the material get expired, the manufacturer shall intimate the authority within seven days from the date of expiry for transacting the material for its disposal as per the procedure prescribed in sub-clause (6) of clause 26.

Provided that the material of such damaged material shall be conspicuously superscribed in red color with word damaged and also with sign "X";

(2)     Notwithstanding anything contained in this order where the stock of organic fertiliser damaged during storage or during transit and does not conform to the prescribed standard, such material shall be taken by manufacturer for reprocessing it by mixing with fresh biomass or in case where it is non-standard due to heavy metal content then the manufacturer immediately with draw the material for reprocessing by mixing with fresh biomass or such material shall be used in gardens, golf courses etc. or sent to landfills. If stock is at dealers end, it shall be taken back or returned to the manufacturer for disposal as mentioned above.

(3)     The manufacturer shall intimate to the Notified authority within seven days in case where the material is damaged during transit or, within seven days in case the material damaged or not of prescribed standard during storage at any dealer level or in storage godown:

Provided that such damaged material shall be conspicuously superscribed in red color with word damaged and also with sign "X".][38]

Order - 24. Manufacturers/Pool handling agencies to appoint officers responsible with compliance of the Order.

Every manufacturing organization, ***importer and pool handling agency shall appoint in that organization and in consultation with the Central Government, an officer, who shall be responsible for compliance with the provisions of this Order.

Order - 25. Restriction on sale/use of fertilisers.

(1)     No person shall, except with the prior permission of the Central Government and subject to such terms and conditions as may be imposed by such Government, sell or use fertiliser, for purposes other than fertilisation of soils and increasing productivity of crops.

Provided that the price of fertilisers permitted for sale for industrial use shall be no profit no loss price, excluding all subsidies at the production, import, handling or on sale for agricultural consumers;

Provided further that wherever customs or excise duties are chargeable, these may be added to the price so fixed.

Provided also that in the case of non-standard fertilisers, reductions shall be made from the no profit no loss price, indicated above, proportionate to the loss of nutrient contents.

(2)     Notwithstanding anything contained in sub-clause (1), no prior permission for use of fertiliser for industrial purposes shall be necessary when the fertiliser for such purposes is purchased from the Industrial dealer possessing a valid certificate of registration granted under clause 9.

(3)     Any person possessing a valid certificate of registration for Industrial dealer, unless such person is a State Government, a manufacturer/importer or a pool handling agency, shall not carry on the business of selling fertilisers for agricultural purposes, including a wholesale dealer or a retail dealer. However, in case of a State Government, a manufacturer or a importer or a pool handling agency possessing a valid certificate of registration for sale of fertiliser for industrial use, and also for sale of fertiliser for agricultural use, whether in wholesale or retail or both, shall not carryon the business of selling fertilisers both for Industrial use and agricultural use In the same premises.

VII. ENFORCEMENT AUTHORITIES

Order - 26.

Appointment of registering authority The State Government may, by notification in the Official Gazette, appoint such number of persons, as it thinks necessary, to be registering authorities for the purpose of this Order and may, in any such notification define the limits of local area within which each such registering authority shall exercise his jurisdiction.

Order - 26A. Notified Authority-

The State Government may, by notification in the Official Gazette, appoint such number of persons, as it thinks necessary, to be Notified Authorities for the purpose of this Order and define the local limits within which each such Notified Authority shall exercise his jurisdiction.

Order - 27. Appointment of inspectors.

The State Government, or the Central Government may, by notification in the Official Gazette appoint such number of persons, as it thinks necessary, to be inspectors of fertilisers for the purpose of this Order, and may, in any such notification, define the limits of local area within which each such inspector shall exercise his jurisdictions.

Order - 27A. Qualifications for appointment of fertiliser Inspectors.

No person shall be eligible for appointment as Fertiliser Inspector under this Order unless he possesses the following qualifications, namely:-

(1)     Graduate In agriculture or science with chemistry as one of the subjects, from a recognised university; and

(2)     Training or experience in the quality control of fertilisers and working in the State or Central Government Department of Agriculture.

Order - 27AA.[Regular training of Fertiliser Inspectors.

Every Fertiliser Inspector shall undergo training after every three years in the Central Fertiliser Quality Control and Training Institute or any Regional Fertiliser Quality Control Laboratory at Mumbai, Kalyani or Chennai.][39]

Order - 27B. Qualifications for appointment of fertiliser Inspectors for Biofertiliser and Organic Fertiliser.

No person shall be eligible for appointment as inspector of biofertiliser and Organic fertilizer under this Order unless he may possess the following qualifications, namely:

(1)     Graduate in agriculture or science with chemistry/microbiology as one of the subject; and

(2)     Training or experience in the field of quality control of biofertilisers/organic fertilizers.

Order - 28. Powers of Inspectors.

(1)     An inspector may, with a view to securing compliance with this Order:-

(a)      require any manufacturer, importer, pool handling agency, wholesale dealer or retail dealer to give any information in his possession with respect to the manufacture, storage and disposal of any fertilizer manufactured or, in any manner handled by him

(b)      draw samples of any fertiliser in accordance with the procedure of drawal of samples laid down in Schedule II. Provided that the inspector shall prepare the sampling details in duplicate In Form J, and hand over one copy of the same to the dealer or his representative from whom the sample has been drawn;

(ba) draw samples of any biofertilisers in accordance with the procedure of drawl of samples laid down in schedule III.

(bb) draw samples of any organic fertilisers in accordance with the procedure of drawl of samples laid down in schedule IV.

(c)      enter upon and search any premises where any fertiliser is manufactured/ Imported or stored or exhibited for sale, if he has reason to believe that any fertiliser has been or is being manufactured/imported, sold, offered for sale, stored, exhibited for sale or distributed contrary to the provisions of this Order;

 

(d)      seize or detain any fertiliser in respect of which he has reason to believe that a contravention of this Order has been or is being or is [attempted] to be committed;

 

(e)      seize any books of accounts or documents relating to manufacture, storage or sale of fertilisers, etc. in respect of which he has reason to believe that any contravention of this Order has been or is being or is about to be committed;

Provided that the Inspector shall give a receipt for such fertilisers or books of accounts or documents so seized to the person from whom the same have been seized;

Provided further that the books of accounts or documents so seized shall be returned to the person from whom they were seized after copies thereof or extracts thereform as certified by such person, have been taken.

(2)     Subject to the proviso to paragraphs (d) and (e) of sub-clause (1), the provisions of the Code of Criminal Procedure, 1973 (2 of 1974) relating to search and seizure shall, so far as may be, apply to searches and seizures under this clause.

Provided also that the inspector shall give the stop sale notice in writing to the person whose stocks have been detained and initiate appropriate action as per the provisions of this order within a period of twenty one days. If no action has been initiated by the inspector within the said period of twenty one days from the date of issue of the said notice, the notice of stop sale shall be deemed to have been revoked.

(3)     Where any fertiliser is seized by an inspector under this clause, he shall forthwith report the fact of such seizure to the collector whereupon the provisions of sections 6A, 6B, 6C, 6D and 6E of the Act, shall apply to the custody, disposal and confiscation of such fertilisers.

(4)     Every person, if so required by an inspector, shall be bound to afford all necessary facilities to him for the purpose of enabling him to exercise his powers under sub-clause (1).

Order - [28A. Appointment of officer for keeping the sample in custody

The State Government may, by notification in Official Gazette, appoints an officer not below the rank of Joint Director of Agriculture Department for keeping the samples in its custody and for sending the second part for analysis to National test House and the third part for referee analysis.][40]

Order - [28B. Sample drawn by the Inspector

(1)     Out of three parts made by the Inspector drawn under sub- clause (6) of clause 28, the first part shall be sent to any of the State Government notified lab by the state Inspector under intimation to the officer notified under clause 28 A and the second part and third part shall be kept in custody of officer nominated by the State Government.

(2)     The company or dealer, from whom sample is drawn may request to such authority within one week from the date of drawal of sample, to send the second part of the sample to any of the National Test House Laboratories on payment of fees as provided by the Central Government from time to time and in case, there is variation in the results of the first and second analysis, then the said authority invariably shall send the third part of the sample to Central Fertiliser Quality Control and Training Institute, Faridabad for final referee analysis.

(3)     In case where the sample is drawn by the Central Government Inspector then out of three parts made by the Inspector, the first part shall be sent to any of the Regional Quality Control Laboratory at Mumbai, Kalyani or Chennai and, the second part and third part shall be kept in custody of incharge of the Regional Fertiliser Quality Control Laboratory at Chennai, Kalyani or Mumbai as the case may be.

(4)     The company or dealer, from whom sample is drawn may request within one week to such authority to send the second part of the sample to any of the National Test House Laboratories on payment of fees as provided by the Central Government from time to time and in case, there is variation in the result of the first and second analysis, then such authority invariably send the third part of the sample to Central Fertiliser Quality Control and Training Institute, Faridabad for final referee analysis.

(5)     The referee analysis report received from the laboratory shall be treated as final.

(6)     In case, where the appeal of non- standard fertiliser under sub-clause (3) of clause 32 and sub -clause (3) of clause 32A have not been considered then the report of the regional fertiliser Quality Control Laboratory or the notified Fertiliser Testing Laboratory, as the case may be shall be treated as final.][41]

Order - [28C. Inspection Team

The Central Government shall constitute a Inspection team or teams headed by an officer not below the rank of Director or equivalent and comprising of four other officers not below the rank of Assistant Section Officer or equivalent:

Provided that one of the member shall possess the minimum qualification and training prescribed for Fertiliser Inspector in clause 27 A of FCO.

Order - 28D. Power of Inspection Team

The Inspection team shall exercise all the power assigned to Fertiliser Inspector under item (a), (b), (c), (d) and (e) of sub-clause (1) of clause 28 and sub-clauses (2), (3), and (4) of clause 28 of the Fertiliser (Inorganic, Organic or Mixed) (Control) Order, 1985.][42]

VIII. ANALYSIS OF SAMPLES

Order - 29. Laboratory for analysis.

[43][(1) A fertilizer sample drawn by an Inspector [44][Inspection team constituted by Central Government], shall be analysed in accordance with the instructions contained in Schedule II-

(a)      in regional fertilizer control laboratories at Mumbai, Chennai or Kalyani (Kolkata) and the National Test House Laboratories at Mumbai, Chennai, Kolkatta, Ghaziabad and Jaipur as per sub- clause (2) of clause 28B; or

(b)      in any laboratory notified for this purpose by the State Government with the prior approval of the Central Government and the National Test House Laboratories at Mumbai, Chennai, Kolkatta, Ghaziabad and Jaipur as per sub- clause (4) of clause 28B;]

(1A) Biofertiliser samples, drawn by an inspector, shall be analyzed in accordance with the instructions contained in Schedule III in the [45][Regional centre of Organic farming at Bengaluru, Bhubaneswar, Ghaziabad, Imphal, Jabalpur, Nagpur and Panchkula] or in any other laboratory notified by the Central or State Government.

(1B) Organic fertiliser samples, drawn by an inspector, shall be analyzed in accordance with the instructions contained in Schedule IV in the [46][Regional centre of Organic farming at Bengaluru, Bhubaneswar, Ghaziabad, Imphal, Jabalpur, Nagpur and Panchkula] or in any other laboratory notified by the Central or State Government.

[47][(1C) A biostimulant sample drawn by an inspector shall be analysed in accordance with the procedure contained in Part C of Schedule VI in the Central Fertiliser Quality Control and Training Institute, Faridabad or its regional laboratories or in any other laboratory notified for this purpose by the State Government with prior approval of Central Government.]

(2)   Every laboratory referred to in sub-clause (1) shall, in order to ensure accurate analysis, of fertiliser samples, possess minimum equipment and other laboratory facilities, as may be specified from time to time by the Controller in this behalf.

[48][(3) Every fertiliser testing laboratories specified or notified by the State Government under sub-clause (1) shall be required to obtain the accreditation of the National Accreditation Board for Testing and Calibration Laboratories within a period of [49][six months] from 28th day of September, [50][2023].]

Order - 29A. Qualifications for appointment of fertiliser analyst in the fertiliser control laboratories.

No person shall be eligible for appointment as fertiliser analyst for analysis of fertiliser samples in the laboratories notified under clause 29 of the Order, unless he possesses the following qualifications, namely:-

(1)     graduate in Agriculture or Science with chemistry as one of the subjects from a recognised university; and

 

(2)     training In fertiliser quality control and analysis at Central Fertilizer Quality Control and Training Institute, Faridabad.

Provided that the fertiliser analysts appointed before the commencement of this Order, who do not possess the requisite training, shall undergo prescribed training, within a period of three years, in the Central Fertiliser Quality Control " and Training Institute, Faridabad from the date of commencement of this Order.

Order - 29AA.[Regular training of Fertiliser Analysts.

Every Fertiliser Analyst shall undergo training after every three years in the Central Fertiliser Quality Control and Training Institute or any Regional Fertiliser Quality Control Laboratory at Mumbai, Kalyani or Chennai.][51]

Order - 29AB.

[52][No person shall be eligible to be notified as analyst for analysis of sample of Biofertiliser, Organic fertiliser and non edible de-oiled cake fertilizers in the laboratories notified under sub clauses (1A) and (1B) of clause 29, unless the analyst possesses the following qualifications, namely:-

(a)      Postgraduate degree in Agriculture Chemistry and Soil Science or Microbiology or Plant Pathology or Chemistry or Biotechnology or Horticulture or Bio-Engineering;

(b)      training in analysis of Biofertiliser, Organic fertiliser and non edible de-oiled cake fertilizers at National Centre of Organic Farming or at a recognized laboratory or Institute:

Provided that the analyst who has been appointed prior to the date of commencement of this Order, but does not possess the requisite training or experience in analysis of Biofertiliser, Organic fertiliser and non edible de-oiled cake shall undergo prescribed training at the National Centre of Organic Farming or at a recognized lab or Institute within a period of three years from the date of such commencement.]

Order - [29B.

The Central Fertiliser Quality Control and Training Institute, Faridabad shall be designated as referee laboratory for the purpose of analysis of any sample of fertiliser under sub-clauses (1), (2) and (3) of clause 28 B.][53]

Order - [29C. Laboratories for referee analysis of Biofertiliser.

(1)     [54][Regional centre of Organic Farming at Bengaluru, Bhubaneswar, Ghaziabad, Imphal, Jabalpur, Nagpur and Panchkula] and every laboratory referred to in clause 29 (1A) shall be designated as referee laboratory for the purpose of analysis of any sample of Biofertiliser:

Provided that no such laboratory which carried out the first analysis of fertiliser sample shall be so designated in respect of that sample:

Provided further that in respect of any sample the analysis of which has been challenged, may be sent for referee analysis to any one of the other laboratories except those which are located in the state or where the first analysis has been done: 

Provided that [55][Regional centre of Organic Farming at Bengaluru, Bhubaneswar, Ghaziabad, Imphal, Jabalpur, Nagpur and Panchkula] shall be considered as one group of laboratories and a sample first analysed by any one of them, shall not be sent for referee analysis to any other in that group, but only to any other laboratory notified by a State Government or Central Government.][56]

(2)     Notwithstanding anything contained in this Order, the Appellate Authority as specified in sub-clause 1 of clause 32A in case of sample collected by the state Government laboratory, or the Controller, in case of sample collected by [57][Regional centre of Organic Farming at Bengaluru, Bhubaneswar, Ghaziabad, Imphal, Jabalpur, Nagpur and Panchkula], as the case may be, shall decide and send, one of the two remaining samples, for reference analysis as provided under sub-clause (1).

Order - 29D. Laboratories for referee analysis of Organic fertilizer.

(1)     [58][Regional centre of Organic Farming at Bengaluru, Bhubaneswar, Ghaziabad, Imphal, Jabalpur, Nagpur and Panchkula] and every laboratory referred to in clause 29 (1A) shall be designated as referee laboratory for the purpose of analysis of any sample of Organic fertiliser Provided that no such laboratory which carried out the first analysis of fertiliser sample shall be so designated in respect of that sample;

Provided further that in respect of any sample the analysis of which has been challenged, may be sent for referee analysis to any one of the other laboratories except those which are located in the state or where the first analysis has been done;

Provided that [59][Regional centre of Organic Farming at Bengaluru, Bhubaneswar, Ghaziabad, Imphal, Jabalpur, Nagpur and Panchkula] shall be considered as one group of laboratories and a sample first analysed by any one of them, shall not be sent for referee analysis to any other in that group, but only to any other laboratory notified by a State Government or Central Government.

(2)     Notwithstanding anything contained in this Order, the Appellate Authority as specified in sub-clause 1 of clause 32 A in case of sample collected by the State Government laboratory, or the Controller, in case of sample collected by [60][Regional centre of Organic Farming at Bengaluru, Bhubaneswar, Ghaziabad, Imphal, Jabalpur, Nagpur and Panchkula], as the case may be, shall decide and send, one of the two remaining samples, for reference analysis as provided under sub-clause (1)]

Order - 30. Time limit for analysis, and communication of result.

(1)  Where sample of a fertlliser has been drawn, the same shall be dispatched alongwith a memorandum in Form K and in case of Organic fertilizers and Biofertilisers in Form KI to the laboratory for analysis within a period of [61][three working days] from the date of its drawal.

[62][(2) The laboratory shall analyse the sample and forward the analysis report to the authority specified in the memorandum referred to in sub-clause (1) in the following manner, namely:-

(a)      in case of fertiliser, other than biofertilizer, organic fertilizer and de oiled cake fertilizer, the analyzing report shall be in Form L and forwarded within fifteen days;

(b)      in case of the sample of organic fertilizer, the analysis report shall be in Form L1, and forwarded within thirty days;

(c)      in case of biofertilizer, the analysis report shall be in Form L2 and forwarded within forty-five days;

(d)      in case of deoiled cake fertilizer, the analysis report shall be in Form L3 and forwarded within thirty days from the date of receipt of sample in the laboratory.]

(3)   The authority to whom the analysis report is sent under sub-clause (2) shall communicate the result of the analysis to the dealer/manufacturer/Importer/pool handling agency from whom the sample was drawn within [63][seven days] from the date of receipt of the analysis report of the laboratory.

IX. MISCELLANEOUS

Order - 31.Suspension, Cancellation Or Debarment.

(1)     A Notified Authority, registering authority, or as the case may be, the controller may, after giving the authorized dealer or the holder of certificate of registration or certificate of manufacture or any other certificate granted under this Order, an opportunity of being heard, suspend such authorization letter or certificate or debar the dealer from carrying on the business of fertilizer on one or more of the following grounds, namely:-

(a)      that the authorization letter or certificate of registration or certificate of manufacture, as the case may be, has been obtained by wilful suppression of material facts or by misrepresentation of relevant particulars:

(b)      that any of the provisions of this Order or any terms and condition of the Memorandum of Intimation or certificate of registration or the certificate of manufacture, as the case may be, has been contravened or not fulfilled:

Provided that while debarring from carrying on the business of fertiliser or canceling the certificate, the dealer or the certificate holder thereof may be allowed for a period of thirty days to dispose of the balance stock of fertilizers, if any, held by him:

Provided further that the stock of fertilizer lying with the dealer after the expiry of the said period of thirty days shall be confiscated.

(2)     Where the contravention alleged to have been committed by a person is such as would, on being proved, justify his debarment from carrying on the business of selling of fertilizer or, cancellation of authorization letter or certificate of registration or certificate of manufacture or any other certificate granted under this Order to such person the Notified Authority or registering authority or, as the case may be, the controller may, without any notice, suspend such certificate, authorization letter, as an interim measure:

Provided that the registering authority, Notified Authority or, as the case may be, the controller shall immediately furnish to the affected person details and the nature of contravention alleged to have been committed by such person and, after giving him an opportunity of being heard, pass final orders either revoking the order of suspension or debarment within fifteen days from the date of issue of the order of suspension:

Provided further that where no final order is passed within the period as specified above, the order of interim suspension shall be deemed to have been revoked without prejudice, however, to any further action which the registering authority, Notified Authority or, as the case may be, the controller may take against the affected person under sub-clause (1).

(3)     Wherever an authorization letter or certificate is suspended, cancelled or the person is debarred from carrying on the business of fertiliser, the Notified Authority, registering authority, or as the case may be, the Controller shall record a brief statement of the reasons for such suspension or, as the case may be, cancellation or debarment and furnish a copy thereof to the person whose certificate or authorization letter has been suspended or cancelled or business has been debarred.

(4)     Wherever the person alleged to have committed the contravention is an industrial dealer, the Notified Authority may take action against the holder of such certificate of registration under sub-clause (1) and sub-clause (2):

Provided that where such certificate is suspended or cancelled, the Notified Authority shall, within a period of fifteen days from the date of issue of such order of suspension or cancellation, furnish to the controller also, besides sending the same to the person whose certificate has been suspended or cancelled, a detailed report about the nature of contravention committed and a brief statement of the reasons for such suspension or, as the case may be, cancellation:

Provided further that the controller, shall, in case of the order for suspension passed by the Notified Authority, on receipt of the detailed report and after giving the person an opportunity of being heard, pass final order either revoking the order of suspension or canceling the certificate of registration, within fifteen days from the date of receipt of the detailed report from the Notified Authority, failing which the order of interim suspension passed by the Notified Authority shall be deemed to have been revoked, without prejudice however, to further action which the controller may take against the holder of certificate under sub-clause (1):

Provided also that the order of cancellation passed by the Notified Authority shall remain effective as if it had been passed by the controller till such time the Controller, on receipt of the detailed report from the Notified Authority, and if deemed necessary, after giving the person a fresh opportunity of being heard, pass the final order either revoking or confirming the order of cancellation.

Order - 32. Appeals at Central Government level.

(1)     In any State, where the fertiliser allocation is made by the Central Government under this Order and if the suspension or cancellation of authorization letter of the manufacturer and or pool handling agency or debarment of business, in any way, has an effect of dislocating the said allocation and if the Central Government is of the opinion that it is necessary or expedient so to do for maintaining the supplies, may direct the concerned State Government to furnish detailed report about the nature of contravention and a brief statement of the reasons for such suspension or cancellation and pass such order as it may think fit, confirming, modifying or annulling the order of State Government

Provided that if the report called by the Central Government is not received from the State Government within a period of fifteen days from the date of issue of the communication, the Central Government may decide the case without the report, on merit.

(2)     [64][****]

(3)     [65][in cases where the company or dealer has not applied for the second analysis due to some valid reason then the company or dealer may made an appeal to the Controller, as the case may be, within seven days from the date of receipt of analysis report of first part of the sample and the Controller shall decide on the grounds of the facts whether the matter qualifies to be considered for third analysis.]

Provided that in case where the sample is declared as non-standard both in the first analysis report and referee analysis report but in different parameters or there is wide variation in the analysis report of first analysis and referee analysis, as the case may be, the aggrieved person may appeal to the controller for third analysis within thirty days from the date of receipt of the report of referee analysis on payment of such charges as may be required for such analysis.

(4)     The Controller after providing an opportunity to the aggrieved party of being heard may send the third sample for analysis to the Laboratory and specified under sub-clause (3) of clause 29 B.

(5)     The result of the third analysis referred to in sub-clause (4) shall supersede the first analysis and referee analysis report and shall be treated as final.]

Order - 32A. Appeal at the State Government level.

(1)     The State Government shall, by notification in the Official Gazette, specify such authority as the Appellate authority before whom the appeals may be filed within 30 days from the date of the order appealed against by any person, except by an industrial dealer, aggrieved by any of the following Orders or action of registering authority or a Notified Authority, namely:

(i)       Refusing to grant a certificate of manufacture for preparation of mixture of fertilisers or special mixture of fertilizers; or

 

(ii)      Suspending or canceling a certificate of manufacture; or

 

(iii)     Suspending or canceling authorization letter or debarring from carrying on the business of selling of fertilizer, or

 

(iv)    non-issuance of certificate of manufacture within the stipulated period; or

(v)      non-issuance of amendment in authorization letter within the stipulated period.

(2)     [66][****]

(3)     [67][In cases where the company or dealer has not applied for the second analysis due to some valid reason then the company or dealer may made an appeal in the Fertiliser (Inorganic, Organic or Mixed) (Control) Order, 1985 to the Appellate authority and the Appellate Authority shall decide on the grounds of the facts whether the matter qualifies to be considered for third analysis.]

(4)     The appellate authority after providing an opportunity to the aggrieved party of being heard may send the third sample for analysis to the laboratory specified under sub-clause (3) of clause 29B.

(5)     The result of the third analysis referred to in sub-clause (4) shall supersede the report of first analysis and referee analysis and shall be treated as final.]

Order - 33. Grant of duplicate copies of [authorization letter or Certificate of manufacture] certificate of registrations, etc.

Where [authorization letter or] a certificate of registration or a certificate of manufacture or any other certificate granted or, as the case may be, renewed under this Order is lost or [defaced, the notified authority] registering authority or, as the case may be, the Controller may, on an application made in this behalf, together with the fee prescribed for this purpose under clause 36, grant a duplicate copy of such certificate.

Order - 34. Amendment of certificate of registration.

The Notified Authority, registering or controller, as the case may be, may, on application being made by the holder of an authorization letter, a certificate of registration or certificate of manufacture, together with the fee prescribed for the purpose under clause 36, amend an entry in such authorization letter, certificate of registration or certificate of manufacture as the case may be.

Order - 35. Maintenance of records and submission of returns, etc.

(1)     The controller may by an order made in writing direct the dealers. manufacturers/ importers, and pool handling agencies:-

(a)      to maintain such books of accounts, records, etc. relating to their business in Form 'N' [68][or maintain digital stock register in the form which clearly exhibits the date wise stock position, opening balance, receipts during the day, sales during the day and closing stock]. And

(b)      to submit to such authority, returns and statements in such form and containing such information relating to their business and within such time as may be specified in that order.

(2)     Where a person holds certificates of registration for retail sale and wholesale sale of fertilisers, he shall maintain separate books of accounts for these two types of sales made by him.

(3)     Where a State Government, a manufacturer, +an importer and a pool handling agency holds valid certificates of registration for sale of fertilisers in, wholesale or retail or both and also for sale for industrial use, he shall maintain separate books of accounts for these two or three types of sales made by him.

(4)     Every importer shall inform the Director of Agriculture of the State in which he intends to discharge the imported fertilizer, under intimation to the Central Government, before the import is made or within a period of fifteen days after an indent for import is placed, the following details, namely ;-

(i)       name of fertilizer

 

(ii)      name of country of import.

 

(iii)     name of manufacturer.

 

(iv)    quantity to be imported

 

(v)      date of arrival of the consignment.

 

(vi)    name of the discharge port.

 

(vii)   other information

Order - 36. Fees.

(1)     The fees payable for grant, amendment or renewal of a [n authorization letter] or certificate of registration or certificate of manufacture [69][or certificate of authorisation for sale of non-standard fertiliser or certificate for reprocessing of fertiliser damaged during storage] a duplicate of such certificates or, renewal thereof under this Order shall be such as the State Government may, from time to time fix, subject to the maximum fees fixed for different purposes by the Central Government and different fees may be fixed for different purposes or for different classes of dealers or for different types of mixtures of fertiliser or special mixture.

 

(2)     The authority to whom and the manner in which the fee fixed under sub-clause (1) shall be paid, shall be such as may be specified by the State Government by notification in the Official Gazette.

 

(3)     Any fee paid under sub-clause (1) shall not be refundable unless the grant or renewal of any certificate of registration or certificate of manufacture or duplicate copy of such certificate or renewal under this Order has been refused.

 

(4)     The fees payable for grant, amendment, renewal or duplicate copy of certificate of registration for industrial dealer and the authority to whom and the manner in which such fee shall be paid, shall be such as may be specified by the Controller from time to time by notification in the Official Gazette*.

Order - 37. Service of orders and directions.

Any order or direction made or issued by the controller or by any other authority under this order shall be served in the same manner as provided in sub-section (5) of section 3 of the Act.

Order - 38. Advisory Committee.

(1)     The Central Government may by notification in the Official Gazette and on such terms and conditions as may be specified in such notification, constitute a Committee called the Central Fertiliser Committee consisting of a Chairman and not more than ten other persons having experience or knowledge in the field, who shall be members of the Committee, to advise the Central Government regarding:

(i)       inclusion of a new fertiliser, under this Order;

 

(ii)      specifications of various fertilisers;

 

(iii)     grades/formulations of physical/granulated mixtures of fertilisers that can be allowed to be prepared in a State;

 

(iv)    requirements of laboratory facilities in a manufacturing unit, including a unit manufacturing physical/granulated mixtures of fertilisers;

 

(v)      methods of drawal and analysis of samples.

 

(vi)    any other matter referred by the Central Government to the Committee.

(2)     The Committee may, subject to the previous approval of the Central Government, make bye-laws fixing the quorum and regulating its own procedure and the conduct of all business to be transacted by it.

(3)     The Committee may co-opt such number of experts and for such purposes or periods as it may deem fit, but any expert so co-opted shall not have the right to vote.

(4)     The Committee may appoint one or more sub-committees, consisting wholly of members of the Committee or or partly of the members of the Committee and partly of co-opted members as it thinks fit, for the purpose of discharging such of its functions as may be delegated to such subcommittee or sub-committees by the Central Fertiliser Committee.

(5)     The State Government may by notification in the Official Gazette and on such terms and conditions as may be specified in such notification, constitute a Committee called the State Fertiliser Committee consisting of a Chairman and not more than 4 other members, having experience or knowledge in the field, including a representative from State Agricultural University, the Fertiliser Industry and Indian Micro Fertilisers Manufacturers Association to advise the State Government regarding the grades/formulations of *mixture or of fertilisers.

Order - [38A. Central Biostimulant Committee.

(1)     The Central Government may, by notification in the Official Gazette, constitute a Committee to be called 'Central Biostimulant Committee' with the Agriculture Commissioner as its Chairperson and seven other members, subject to such terms and conditions, as may be specified therein.

(2)     The Central Biostimulant Committee shall advise the Central Government on the following issues, namely:

(i)       inclusion of a new biostimulant;

 

(ii)      specifications of various biostimulants;

 

(iii)     methods of drawing of samples and its analysis;

 

(iv)    minimum requirements of laboratory;

 

(v)      method of testing of biostimulants;

 

(vi)    any other matter referred to the Committee by the Central Government.

(3)     The Committee may, subject to the previous approval of the Central Government, make bye-laws fixing the quorum and regulating its own procedure and the conduct of all business to be transacted by it.

(4)     The committee may co-opt such number of experts and for such purposes or periods as it may deem fit, but any expert so co-opted shall not have the right to vote.

(5)     The committee may appoint one or more sub-committees, consisting wholly of its members or partly of its members and co-opted members, as it thinks fit, for the purpose of discharging such for its functions as may be delegated to such sub-committee.

(6)     The Central Biostimulants Committee shall frame guidelines laying down the requirements of toxicology testing and other related tests.][70]

Order - 39. Repeal and saving.

(1)     The Fertiliser Control) Order, 1957 is hereby repealed except as respects things done or omitted to be done under the said Order before the commencement of this Order.

(2)     Notwithstanding such repeal, an order made by any authority, which is in force immediately before the commencement of this Order and which is consistent with this Order, shall continue in force and all appointments made, prices fixed, certificates granted and directions issued under repealed Order and in force immediately before such commencement shall likewise continue in force and be deemed to be made, fixed, granted or issued in pursuance of this Order till revoked.

[71][Schedule I

Part A

[See clause 2 (h) and (q)]

SPECIFICATIONS OF FERTILISERS

 

 

 

 

 

 

 

 

 

 

 

 

[122][3. Chelated Zinc as Zinc-Glycine (liquid)

4. Chelated Calcium as Calcium-Glycine (liquid)

5. Chelated Boron as Boron-Glycine (liquid)

[123][6. NK 6:0:18 Fortified with Calcium, Magnesium & Boron (suspension)

7. NPK 11: 11: 8 Fortified with Zinc & Boron (suspension)

8. Calcium Nitrate Fortified with Magnesium (suspension)

[124][9. Potassium Thiosulphate (K₂S₂O₃)

10. Calcium Thiosulphate (CaS₂O₃)

[125][11. Fortified NP (7-21-0) Liquid

12. Fortified Calcium Suspension

 

 

 

 SCHEDULE II

(See clause 28 (1) (b) and 29)

PART A

PROCEDURE FOR DRAWAL OF SAMPLES OF FERTILIZERS

1. General requirement of sampling

In drawing samples, the following measures and precautions should be observed.

(a)      Samples shall not be taken at a place exposed to rain/sun;

 

(b)      The sampling instruments shall be clean and dry when used;

 

(c)      The material being sampled, the sampling instrument and the bags of samples should be free from any adventitious contaminations;

 

(d)      To draw a representative sample, the contents of each bag selected for sampling should be mixed as thoroughly as possible by suitable means;

 

(e)      The sample should be kept in suitable, clean dry and air tight glass or screwed hard polythene bottle of about 400 gm capacity or in a thick gauged polythene bag. This should be put in a cloth bag which may be sealed with the Inspector's seal after putting inside the detailed description as specified in Form "J" Identifiable details may also be put on the cloth bag like sample No./Code No. or any other details which enables its identification;

 

(f)       Each sample bag should be sealed air tight after filling and marked with details of sample, type and brand of fertilizer, name of dealer/manufacturer/importer and the name of Inspector who has collected sample.

2. Sampling from bagged material

(i)       Scale of sampling

(a)      Lot (for manufacturers/importers)

All bags in a single consignment of the material of the same grade and type drawn from a single batch of the manufacturer/importer shall constitute a lot. If a consignment is declared to consist of different batches of manufacturer/import, all the bags of each batch shall constitute a separate lot. In the case of a consignment drawn from a continuous process,2000 bags (or 100 tones) of the material shall constitute a lot.

(b)      Lot (for dealers)

The lot is an identifiable quantity of same grade and type of fertilizer stored at an identifiable place subject to a maximum limit of 100 tones. The lot shall be identified by the inspector based on visible appearance of bags, their packing and storage conditions. The stock of less than 100 tones with a dealer may also constitute one or more lots, if the material (fertilizer) of different sources and brand is available in such quantities.

(c)      Selection of bags for sampling

The number of bags to be chosen from a lot shall depend upon the size of the lot as given in the table below.

All the bags of a lot should be arranged in a systematic manner. Start counting from any bag randomly, go on counting as 1,2,3,- up to r and so on, r being equal to the integral of N/n. Thus every rth bag counted shall be withdrawn and all bags shall constitute the sample bags from where the sample is to be drawn for preparing a composite sample.

(ii)      Sampling from big godowns/high stackings.

If the procedure given in Para 2(i) (c) is not possible to be adopted, the sample should be drawn from the randomly selected fertilizer bags from different layers, from top and from all open side in a zig fashion.

(iii)     Sampling from small godowns

All the fertilizer bags of the same grade and type of each manufacturer though received on different dates shall be segregated and properly stacked. All bags of same grade and type of fertilizer manufactured by a particular manufacturing unit may be considered as one lot based on their physical conditions and the sample shall be drawn as per procedure laid in Para 2(i) (c) and 4.

(iv)    Sampling from damaged stock.

(a)      In case of torn or lumpy bags, damaged fertilizer bags or sweepings, the stock should be arranged according to identifiable lots. From each lot the number of bags shall be selected as per procedure 2(i)(c). If the bags allow the use of sampling probe conveniently, the samples should be drawn by sampling probe.

(b)      In case it is not possible to use the sampling probe, the bags may be opened and fertilizer material mixed together uniformly by hammering the big lumps or putting pressure, if required and then samples drawn by using suitable sample device.

3. Sampling probe

(i)       An appropriate sampling instrument to be used by the Inspectors for collection of a representative sample is called sampling probe. The probe may comprise of a slotted single tube with soil cone tip made of stainless steel or brass. The length of the probe may be approximately 60 to 65 cms and the diameter of the tube may be approximately 1.5 cm and the slot width 1.2 to 1.3 cms. The probe may be use if the physical condition of the fertilizers and the packing material permits it use. 

(ii)      In case of High Density Polyethylene packing and also when the fertilizer material is not in free flowing condition, the use of sampling probe may not be possible. In such a case, selected bags for drawing samples may be opened and the fertilizers may be taken out of the bags and spread on a clean surface and samples drawn with the help of a suitable Sampling device which may be made of stainless steel or brass cup.

4. Drawal of samples from bags.

(i)       Drawal of sample and preparation of composite samples. Draw, with an appropriate sampling instrument, (sampling probe) small portions of the material from the selected bags as per procedure in para 2(i) (b) 2(ii) 2(iii)and 2 (iv) (a). The sampling probe shall be inserted in the bag from one corner to another diagonally and when filled with fertilizer, the probe is withdrawn and fertilizer is emptied in a container/or on polythene sheet/or on a clean hard surface and made into one composite sample.

(ii)      If the bags do not permit the use of sampling probe, empty the contents of the bags on a level, clean and hard surface and draw a composite sample by the process of quartering as described under para 3 (ii) or 5.+(iii) In case of chelated micro-nutrients and mixtures of micro-nutrients, the three identical containers of the batch, grade, type and manufacturer, shall be selected which shall constitute the composite samples, provided it is not possible to draw a composite sample of the size given under para 4A (iii)."

4A. Weight of one sample

One sample of fertilizer shall have the approximate weight, as specified below:-

                              (i)          For straight micro-nutrient fertilizers- 100gms.

                             (ii)         For chelated micro-nutrient fertilizers and 50gms or mixtures of micro-nutrients the maximum  packing size of similar quantity.

                            (iii)         For other fertilizer and mixtures of fertilizers 400 gms.

[127][(iv) For 100 % Water Soluble fertiliser and 100% water soluble Mixture of fertiliser 100g.]

5. Preparation of composite sample

If the composite sample collected from the different selected bags is large than required weight, its size shall be reduced by method of quartering as detailed below:-

Spread the composite sample on a level, clean, hard surface, flatten it out and divide it into four equal parts. Remove any diagonally opposite parts. Mix the tow remaining parts together to form a cone, flatten out the cone and repeat the operation of quartering till a composite sample of required weight is obtained.

6. Preparation of test sample and reference sample

              (i)          The composite sample obtained above shall be spread out on a clean, hard surface and divided into three approximately equal proportions + each of the weight as specified in Para 4A. Each of these samples shall constitute the test sample.

             (ii)         Each test sample shall be immediately transferred to a suitable container as defined under para 1(e). The slip with detailed description may be put inside the sample bag. Each bag shall also be properly labeled as mentioned in Para 1(f)

            (iii)         Each test sample container shall then be sealed with the seals of the inspector. If possible, seal of the manufacturer/importer/dealer or purchaser as the case may be, may also be affixed.

            (iv)        [128][****]

7. Sampling from the bulk fertilizers in ships, bulk carriers and bulk containers.

              (i)          Sampling equipments

(a)      Sampling cup

The sampling cup can be fabricated from non-corrosive metal, Inside dimensions of cup mouth may be 3/4" X 10" as per he diagram of the sampling cup given in Figure -1.

(b)      Sampling probe for bulk fertilizers.

The sampling probe should be made of non-corrodable material such as stainless steel or brass. It may be slotted double tube with solid cone tip having a length of about 4 1/2'-5' and diameter of about 1 1/4" to 1 1/2".

[129][(c) Sampling cup or scoop:

The samples from the wharf or silo, as the case may be, can be collected by a sampling cup or a suitable scoop made of stainless steel or brass.]

             (ii)         Sampling procedure

(a)      Drawal of samples from the ship of bulk fertilizers

A.        Sampling from conveyor belt.

When the material is unloaded from the ships transported to temporary/storage godowns through conveyor belts, the sample can be drawn by passing the sampling cup through the entire stream of material as the material drops from a transfer belt or spout. The long slot in the top of sampling cup should be perpendicular to the falling stream. pass the cup through the complete stream at a uniform speed, so that the cup will collect approximately equal amounts in each pass but will never overflow.

A minimum of 10 equally timed and speed stream must be taken during the transfer operation. However, the stream samples are not applicable unless uniform continuous flow of fertilizer is maintained for more than 3 minutes while lot is being sampled.

B.        [130][Sampling from ship

1.        Draw the samples, from the fertilizer being discharged from the ship on the wharf or silo as the case may be, periodically at the regular interval of five hours on first and last day of discharge and three hours on intermediate days. All the samples drawn on a particular day shall be mixed together to make day composite sample. If the day composite sample is larger than required weight, its size shall be reduced by method of quartering as described in Paragraph 5 of Schedule II of Part A.

2.        Then the ship composite sample shall be prepared by mixing part of each day composite. Further test sample and reference sample shall be prepared as given in Paragraph 6 of Schedule II of Part A.]

(b)      Drawal of samples from bulk carriers-trucks etc. The sample can be drawn as per vertical probing procedure of Association of Official Analytical Chemists. The sampling probe should be about 4 1/2' to 5' length. Draw 10 Vertical cuts from the following locations relative to the entire top of the conveyance. The 10 vertical cores are combined into a composite sample.

(c)      Drawal of samples from bulk material in storage.

 

(A)     The bulk storage piles (level or flat) up to 100 tones could be sampled as per Figure 2. Take 10 cores to the maximum possible depth of the probe from the position indicated in the Figure 2 and cores are composited.

(B)     A one sided or slopped pile may be sampled at the points illustrated in Figure3. Withdraw one vertical core of material from location 1 & 6 and two cores at locations 2, 3,4 & 5 composite all the probe samples and prepare the composite sample for analysis as per procedure laid down in para 1,5 & 6. (Figure 2- Sample points for coned or ridged pile)

[131][(d) Drawl of samples from containers

(1)     Minimum 5 bags shall be selected randomly from each container.

(2)     In case of large number of containers containing similar material, the containers shall be selected randomly as per following criteria:

(3)     The samples shall be drawn from the bags selected from each container as per the procedure given in Paragraph 4 of Schedule II of Part A. All the samples drawn from each bag of the selected container shall be mixed together to make container composite sample. If the container composite sample is larger than required weight, its size shall be reduced by method of quartering as described in Paragraph 5 of Schedule II of Part A.

(4)     All the container composite samples shall be mixed together and test sample and reference sample shall be prepared as given in Paragraph 6 of Schedule II of Part A.]

8. Method of sampling of anhydrous ammonia

(i)       Scope

This method is for use obtaining samples of anhydrous ammonia. The method is based on the assumption that the material to be sampled is as claimed and contains only a small amount of impurity primarily water. It is recommended that duplicate samples be taken form each tank or vessel sampled.

(ii)      Apparatus

(a)      Tubes for sampling tubes, heat resistant glass, conical centrifuge type 200ml with lower 100 ml graduated from 0.2 ml in 0.05 ml divisions, 2-4 ml in 0.1 division, 4-10 ml in 0.5 ml divisions and 10-100 ml in 1.0mldivisions. Tube type is shown in figure 5.

 

(b)      Stoppers for tubes, rubber, with bent tube vent as in Figures 5.

 

(c)      Samples carrier, constructed of plywood or aluminum as in Figure 5.

 

(d)      Sampling line and connection assembly constructed as in Figure 4, with flexible steel sampling nose 48" long, 1/4" NPT coupling at each end and 1/8" insulated steel tubing delivery tip at one end.

 

(e)      Sample tube adapter, constructed from rubber stopper and 6mm D. D. glass or steel tubing as in Figure 5.

 

(f)       Protective equipment: Rubber or other non-porous gloves, offering complete protection to the hands lower arms, full coverage goggles or approved gas mask.( Figure 4)

(iii)     Reagents

Charcoal, reagent, 14-20 mesh.

Note: If the sample is expected to contain excessive amount of water (one percent or more) one piece of the charcoal may be added to each tube before introduction of the sample

(iv)    Procedure

(a)      Place two dry, clean sampling tubes in the sample carrier

 

(b)      Connect the sampling line connection assembly to the unloading valve of the tank, vessel, or line to be sampled.

 

(c)      Open the valves slowly and purge the sampling line connection assembly thoroughly by venting 3 to 4 liters of ammonia. Close the sample line globe valve.

 

(d)      Remove the vented stoppers from the tubes and insert the adopter end of the sampling line connection assembly.

 

(e)      Open the sample line valve and slowly fill the sampling tube to the100ml mark, close the sample line valve.

 

(f)       Remove the sampling line adopter and insert the vented stopper in the sampling tube.

 

(g)      Repeat steps, d, e, and f and fill the second tube.

 

(h)     close tank discharge valve and remove the sampling line connection assembly.

 

(i)       Either know or note the vessel, container, or line pressure of material sampled.

 

(j)       Tag the collected samples for identification and submit to the laboratory for processing by following methods in this section

(v)      Precaution

(a)      Liquid anhydrous ammonia causes severe burns on contact. It evaporates readily releasing the gas which may cause varying degrees of irritation of the skin and mucus membrane and may injure severely the respiratory mucosa with possible fatal outcome.

 

(b)      Avoid contacting liquid ammonia. In case of contact, immediately flush the affected parts with plenty of water for atleast 15 minutes. Get medical attention at once in case of burns, especially to the eyes, nose and throat, or if the victim is unconscious.

 

(c)      Ammonium gas in concentrations of 6,000 to 10,000 ppm (by volume) is lethal within a few minutes. Irrigation of the eyes, respiratory tract and throat results from concentrations as low as 500 to 1,000 ppm' a concentration of 2,000 ppm produces convulsive coughing and may be fatal after a short exposure i.e. less than half an hour. The maximum concentration tolerated by the skin for more than few seconds is 2 percent (i.e. when suitable respiratory protection is worm) The maximum allowable concentration for 8 hour working exposure is 50 ppm. This is the least detectable order.

 

(d)      Obtain medical attention if exposure to the gas produce distress of any type.

 

(e)      Rubber or other no porous gloves, offering complete protection to the hands and lower arms must also be worn to protect the eyes unless an approved gas mask is used. The gas mask need only to be used if sampling can not be done without possible inhalation of the vapours.

PART B

METHOD OF ANALYSIS OF FERTILIZERS

1. Preparation of sample for analysis in the laboratory

(i)       Procedure.

(a)      Reduce gross sample to quantity sufficient for analysis or grind not < 250 Gm of reduced sample without previous sieving.

 

(b)      For fertilizer materials and moist fertilizer mixtures, that form a paste on putting pressure, grind in porcelain pestle and mortar to pass sieve with 1mm circular openings or No. 20 standard sieve.

 

(c)      For dry mixtures that tend to segregate, grind in a porcelain pestle and mortar to pass No. 40 standard sieve [132][in case of Potassium Magnesium Calcium Sulphate, the sample shall pass through 0.150 mm IS sieve to 0.180 mm IS sieve].

 

(d)      Grind as rapidly as possible to a avoid loss or gain of moisture during operation.

 

(e)      Mix thoroughly and store in tightly stoppered bottles.

2. Determination of moisture

(Not applicable to samples that yield volatile substances other than water at drying temperature)

(i)       Procedure

(a)      Weight to the nearest mg about 2gm of the prepared sample in a weighed, clean, dry squat form weighing bottle.

 

(b)      Heat in an oven for about 5 hours at 99-101 C to constant weight Cool in a desicator and weigh.

 

(c)      In case of sodium nitrate ammonium sulphate and potassium salts heat to constant weight at 129-131 C.

(d)      Report percentage loss in weight as moisture at temperature used.

Calculations

100(B-C)

Free moisture percent by weight = 100(B-C)/B-A

A= Weight of the bottle

B= Weight of bottle plus material before drying.

C= Weight of the bottle plus material after drying. (Reference - Methods of analysis. AOAC 1965)

(ii)      Moisture in ammonium chloride.

(a)      Weigh accurately about 5gm of prepared sample in a weighed shallow porcelain dish and dry for 24 hours in a vacuum desicator over sulphuric acid and re-weight.

(b)      Preserve the dried material for subsequent tests.

Calculations

Moisture percent by weight = 100 x W1/W3

W1= loss in weight in gm on drying and

W3= Weight in gm of the prepared sample taken for the test.

(iii)     Samples like urea, diammonium phosphate and ammonium nitrate which yield volatile substances other than water at drying temperature. the Karl Fischer method given below is use for the determination of moisture.

(iv)    Reagents

(a)      Iodine solution -add 125 gm of iodine to a mixture of 650 ml of methanol and 200 ml of pyridine contained in a flask, and immediately close the flask tightly.

(b)      Sulphur dioxide solution-pass dry sulphur dioxide into 100 ml of pyridine contained in a 250 ml graduated cylinder and cooled in an ice bath, until the volume reaches 200 ml.

(c)      Fisher Reagent- Slowly add iodine solution to the cooled sulphur dioxide solution stopper immediately and shake well until the iodine is dissolved. Transfer the solution to an automatic pipette, protected from absorption of moisture by a drying agent and allow to stand for 24 hours before standardizing. The reagent deteriorates continuously and it should be standardized within one hour before use.

(v)      Procedure.

(a)      Determination of end point in Karl Fischer Titration- In many cases, the end point can be detected visually by the change of colour

(b)      Sulphur dioxide solution -pass dry sulphur dioxide into to 100 ml of pyridine contained in a 250 ml graduated cylinder and cooled in an ice bath, until the volume reaches 200 ml.

(c)      Fisher reagent-Slowly add iodine solution to the cooled sulphur dioxide solution stopper immediately and shake well until the iodine is dissolved. Transfer the solution of moisture by a drying agent and allow to stand for 24 hours before standardizing. The reagent deteriorates continuously and it should be standardized within one hour before use.

(d)      Standard water solution- Measure exactly 2ml of water into a thoroughly dry 1 liter volumetric flask, dilute to volume with methanol. retain sufficient quantity of the same methanol for blank determination. Keep the solution in tightly closed containers.

(vi)    Procedure

(a)      Determination of end point in Karl Fischer Titration- In many cases, the end point can be detected visually by the change of colour from a light brownish yellow to amber. But when the end point is not clearly defined, the electrometric method for determining the end point should be adopted. Adjust the potentiometer so that when a small excess 90.02 ml) of the reagent is present a current of 50 to 150 microampers is recorded. The solution should be continuously and vigorously stirred. At the beginning of the titration, a current of only a few microampers will flow. After each addition of regent, the pointer of the micrometer deflected but rapidly returns to the original position. At the end point deflection is obtained which endures for a longer period.

(b)      Standardization of the Fischer reagent-Pipette exactly 10ml or methanol into a dry titration flask and titrate with the Fischer reagent to the end point (V1) Pipette exactly 10ml of the standard water solution into the flask and titrate to the end point (V2).

(c)      Titration of the material-Transfer 25ml. of methanol to the titration flask and titrate to the end point (V3) with the Fischer reagent. Do not record the volume consumed. Quickly transfer to the titrated liquid an accurately weighed quantity of the material containing 10 to 50 mg. of water, stir vigorously and titrate to the end point.

Calculation

Moisture percent by weight = 0.1 x W(V3 2.5V1) / (V2- V1)A

Where W= Weight in mg. of water contained in 10ml of standard

water solution.

V3= Total volume in ml of the reagent use in titration in (c)

V1= Volume in ml of reagent used in titration of methanol in(b)

V2= Total volume in ml of the reagent use in titration in (b)

A= Weight in gm. of the material taken for the test in (C)

(Reference- I.S. Specification for urea. technical and pure I.S. 1781-1961)

3. Determination of nitrogen

Methods of determination of total nitrogen have been described separately in this section. These methods can be adopted both for straight and mixed fertilizers. Scope of each method with various combinations have also been described with each method.

The relevant methods of analysis which have been described are as given below:

(i)       Total nitrogen--for nitrate free samples.

 

(ii)      Total nitrogen--for nitrate containing samples.

 

(iii)     Total nitrogen--for materials with high Cl: No3 ration and to materials containing only water soluble nitrogen.

 

(a)      Total nitrogen--for nitrate free samples.

 

(iv)    Determination of ammoniacal nitrogen.

 

(v)      Determination of ammoniacal and nitrate nitrogen.

 

(vi)    Determination of nitrate nitrogen.

 

(vii)   Determination of water insoluble nitrogen.

 

(viii)  Determination of urea nitrogen.

[133][(i) Determination of Cyanamide nitrogen;]

                                              (i)          Detection of nitrate

For adopting a specific method as described above, it is necessary to detect the presence of nitrates in the sample before a particular method is adopted. The procedure for detection of nitrates is given below:-

(a)      Mix 5gm sample with 25ml hot water and filter.

 

(b)      To one volume of this solution add 2 volume of sulphuric acid, free from HNO3 and oxides of N and let it cool.

 

(c)      Add a few drops of concentrated FesO4 solution in such a manner that fluids do not mix.

 

(d)      If the nitrates are present junction shows at first purple, afterward brown, or if only minute quantity is present, reddish colour.

 

(e)      To another portion of solution add 1ml. 1 percent Na NO3 and test as before to determine whether enough H2SO4 was added in the first test.

(Reference -methods of analysis. AOAC 1965)

                                             (ii)         Reagents for determination of total nitrogen.

(a)      Sulphuric acid - 93-98 percent H2SO4 N free.

(b)      Copper sulphate - Cu SO45H2O reagent grade. N free.

(c)      Potassium sulphate (or anhydrous sodium sulphate)-reagent grade.

(d)      Salicylic acid- reagent grade, N free.

(e)      Sulphide or the sulphate solution- Dissolve 40 gm. commercial K2S in liter distilled water. (Solution- of 40gm Na2S or 80gm Na2S2O3.5H2O in 1 liter may be use)

(f)       Sodium hydroxide- pellets or solution, nitrate free. for solution dissolve approximately 450 gm solid NaOH in distilled water and dilute to 1 liter (Sq. gr. of solution should be 1.36 or higher)

(g)      Zinc granule-- reagent grade.

(h)     Zinc dust-- Impalpable powder.

(i)       Methyl red indicator- Dissolve 1gm. methyl red in 200 ml. alcohol.

(j)       Hydrochloric or sulphuric acid standard solution,--0.5 N or 0.1 N when amount or N is small.

(k)      Sodium hydroxide standard solution-- 0.1 N(or other specified concentration)

(1)     Standardize each standard solution with primary standard and check one against another.

(2)     Test reagents before using, by blank determination with 2 gm. sugar which insures partial reduction of any nitrates present.

Caution: Use freshly opened sulphuric acid or add dry P2O5 to avoid hydrolysis of nitrites and cyanates. Ratio of salt to acid (wt: Vol) should be approximately 1:1 at end of digestion for proper temperature control. Digestion may be incomplete at lower ration, N may be lost at higher ration.

                                            (iii)         Apparatus

(a)      For digestion-- Use Kjeldahl flask of hard moderately thick, well annealed glass with total capacity approximately 500-800 ml. Conduct digestion over heating device, adjusted to bring 250 ml. water at 25C to rolling boil in a approximately for 5 minutes. Add 3-4 boiling chips to prevent superheating.

(b)      For distillation- Use Kjeldahl or other suitable flask of 500--800 ml. capacity filled with rubber stopper through which passes. lower end of efficient scrubber bulb or trap to prevent mechanical carryover of NaOH during distillation. Connect upper end of bulb tube to condenser tube by rubber tubing. Trap outlet of condenser in such a way as to insure complete absorption of ammonia distilled over into acid in receiver.

                                            (iv)        Total nitrogen (in nitrate free samples)

(a)      Procedure.

(1)     Place weighed sample (0.7-2.2gm.) in digestion flask.

(2)     Add 0.7 gm. copper sulphate, 15 gm. powdered K2SO4 at anhydrous Na2 SO4 and 25ml.H 2SO4.

(3)     If sample more than2.2 gm. is used, increase sulphuric acid by 10 ml. for each gm. sample.

(4)     Place flask in inclined position and heat gently until frothing ceases (if necessary add small amount of paraffin to reduce frothing)

(5)     Boil briskly until solution clears and then for at least 30 minutes longer (2 hours for sample containing organic material).

(6)     Cool add approximately 200ml. distilled. water, cool below 25C.

(7)     Add to the flask a layer of sodium hydroxide (25 gm. solid reagent or enough solution to make contents strongly alkaline ) without agitation.

(8)     Immediately connect flask to distilling bulb or condenser and with tip of condenser immerse in standard acid in receiver.

(9)     Rotate flask to mix contents thoroughly, then heat until all amonia has distilled (a least 150 ml. distillate)

(10)   Titrate excess standard acid in distillate with standard sodium hydroxide solution, using methyl red as an indicator.

(11)   Correct for blank determination on reagents.

Calculation: Percent nitrogen =(A Na-BNb)x0.01401 x 100 / W

A= ml. of standard acid used.

B= ml. of standard NaOH used.

Na = Normality of standard acid.

Nb = Normality of standard NaOH.

W= Weight of the sample taken in grams.

(Reference- Methods of Analysis, AOAC, 1965)

                                             (v)         Total nitrogen (for nitrate containing samples)

(Note applicable to samples containing high concentrations of nitrate nitrogen and chlorides)

(a)      Procedure.

(1)     Place weighed sample (0.7-2.2 gm) in digestion flask.

(2)     Add 40ml. H2SO4 containing 2 grams salicylic acid. Shake until thoroughly mixed and let stand, with occasional shaking, 30 minutes or more.

(3)     Then add (i) 5 grams Na2S2O3.5H2O or (ii) 2grams zinc dust (as impalpable powder not granulated zinc or filings)

(4)     Shake the flask and let it stand for five minutes. then heat over low flame until forthing ceases.

(5)     Turn off heat, add 0.7 grams copper sulphate.15 gm. powdered K2SO4) and boil briskly until solution clears, then at least 30 minutes longer (2 hours for samples containing organic material).

Proceed further as in 6-11 of 3 (iv)

Calculations: Same as in 3 (iv)

(Reference- Methods of Analysis, AOAC, 1965).

                                            (vi)        Total nitrogen (for materials with high Cl: NO3 ration and to materials containing only water soluble nitrogen).

(a)      Reagents

Reduced iron powder electrically reduced N.F. (National Formulary).

For other reagents see 3 (ii)

(b)      Procedure

Mixed fertilizers

(1)     Place 0.5-2.0 gm. sample in Kjeldahl flask and add 2-5 grams reduced Fe(5gms. is enough for 0.185 grams. NO3).

 

(2)     Add approximately 25ml. distilled water, rotating flask at angle to wash down the sample.

 

(3)     Let it stand for 15 minutes with occasional agitation, to insure complete solution of all soluble salts.

 

(4)     While rotating flask add 25ml. cold H2SO4 (1+1) and let it stand until visible reaction ceases, (use hood or vented digestion unit)

 

(5)     Add boiling chips and boil 15-20 minutes, but do not take to dryness (For samples containing organic matter use 50ml. cold H2SO4 (1+1) boil for 15-20 minutes add 0.7 gm. MgO and heat again for 40 minutes) Cool and proceed further as in 6-11 of 3 (iv).

Calculations: Same as in 3 (iv)

(Reference-methods of Analysis, AOAC 1965).

                                            (vii)        Determination of ammoniacal nitrogen (Distillation Method) (This method is for the determination if nitrogen present or available in the sample as ammonium ion. This method assumes that Urea is absent from the sample. Not applicable to MgNH4 PO4 and Fe4PO4)

(a)      Procedure

(1)     Place 0.7-3.5 grams according to HN3 content of the sample in distillation flask with approximately 300 ml. water and 2 grams of freshly ignited carbonate free MgO or NaOH solution.

(2)     Connect the flask to condenser by Kjeldahl connecting bulb.

(3)     Distill 100 ml. liquid into measured quantity of standard acid and titrate with standard NaOH solution, using methyl red as an indicator

Calculations: Percent nitrogen = (ANa -BNb) x 0.01401 x 100 / W 

A= ml. of standard acid used.

B= ml. of standard NaOH.

Na = normality of acid.

Nb = normality of NaOH.

W= weight of the sample taken in gm.

(Reference -Recommended analytical methods of the

National Plant Food Institute, Washington. D.C. 1961)

                                           (viii)       Determination of ammoniacal and nitrate nitrogen (Devarda Method) (This method is for the determination of total nitrogen when only nitrate or mixture of nitrate and ammoniacal nitrogen is present. This method assumes the absence of urea, calcium Cyanamid and organic matter from the sample.)

(a)      Procedure

(1)     Place 0.35-0.5 gms. sample in600-700ml. flask and add 300ml. water, 3 grams devarda Alloy, and 5ml. NaOH solution (42 percent by weight pouring later down side of flask so that it does not mix at once with contents)

 

(2)     Allow the flask to stand for 15 minutes.

 

(3)     By means of Davison [ J. Ind. Eng. Chem. 11,465 (1919)] or other suitable scrubbing bulb, that will prevent passing over of any spray, connect with condenser tip of which always extends beneath surface of standard acid in receiving flask.

 

(4)     Mix contents of distilling flask by rotating.

 

(5)     Heat slowly at first and then at a rate to yield 250 ml. distillate in 1 hour.

 

(6)     Collect distillate in measured quantity of standard acid and titrate with standard NaOH solution using methyl red as an indicator.

 

(7)     In analysis of nitrate salts dissolve 3.5 or 5.0 grams in water, to 250 ml. and use 25ml. aliquot.

Calculation: Same as in 3 (iv)

(reference- Methods of Analysis, AOAC, 1965)

                                            (ix)        Determination of nitrate nitrogen

(Applicable in presence of calcium Cyanamid and urea in the mixture)

(a)      Procedure

(1)     Determine total nitrogen as in 3(v)

 

(2)     Determine water insoluble N as in 3(x) but use 2.5 grams sample. Dilute to 250ml.

 

(3)     Determine ammoniacal N in 50ml filtrate as in (vii).

 

(4)     Place another 50ml. portion filtrate in 500 ml. Kjeldahl flask and 2 grams FeSO4.7H2O and 20ml. H2SO4 (if total N is 5percent use 5gm. Fe SO4.7H2O) Digest over hot flame until all water is evaporated and transparent fumes appear and continue digestion at least ten minutes to drive off nitrate N. If severe bumping occurs add 10-15 glass beads. Add 0.65 grams Hg or 0.7 grams HgO and digest until all organic matter is oxidized, cool, dilute add the K2S solution and complete determination as 3 (iv) Before distillation add pinch of mixture of zinc dust and granular "20 mesh". zinc to each flask to prevent bumping.

Calculations: Total N (a)-- water insoluble N(b)- water soluble N. Water Sol.

N-- N obtained in (d)- nitrate N.

(Reference -Methods of analysis, AOAC, 1965)

                                             (x)         Determination of water insoluble nitrogen

(a)      Procedure

(1)     Place 1 or 1.4 grams sample in 50ml. beaker, wet with alcohol.

(2)     Add 20ml. water and let it stand for 15 minutes stirring occasionally.

 

(3)     Transfer supernatant liquid to 11 cm. Whatman No. 42. paper in 60 long stem funnel 2.5" diameter and wash residue 4 or 5 times by decanting with water at room temperature (20-25C)

 

(4)     Finally transfer all residue to filter and complete washing until filtrate measures 250ml.

 

(5)     Determine N as in 3(iv)

                                            (xi)        Determination of urea nitrogen

(This method is for the determination of urea content of any mixed fertilizers.)

(a)      Reagents

(1)     Neutral urease solution - shake 1gm. jack bone meal with 100ml. water for 5 minutes. Transfer 10ml solution to 250 ml. Erlenmeyer flask, dilute with 50ml. water and add 4 drops methyl purple indicator. Tiltrate with 0.1 N NaOH. From difference in ml. calculate amount of 0.1 N HCL require to neutralize remainder of solution (usually approximately 2.5 ml. per 100ml.) add this amount of acid

(b)      Procedure

(1)     Weight 10+0.01 gm. sample and transfer to 15cm. Whatman No. 12 fluted filter paper.

 

(2)     Leach with approximately 300ml. water into 500ml. volumetric flask.

 

(3)     Add 75-100 ml. saturated barium hydroxide solution to precipitate phosphates.

 

(4)     Let it settle and test for complete precipitation with few drops of saturated barium hydroxide solution.

 

(5)     Add 20ml 10 percent sodium carbonate solution to precipitate excess barium and any soluble calcium salts.

 

(6)     Let it settle and test for complete precipitation.

 

(7)     Dilute to volume, mix and filter through 15cm. Whatman. No. 12 fluted paper.

 

(8)     Transfer 50ml. aliquot (equivalent to 1gm. sample)to 200 or 250 ml. Erlenmeyer flask and add 1 to 2 drops methyl 1 purple indicator.

 

(9)     Acidify solution with 2N HCl and add 2 to 3 dorps excess.

 

(10)   Neutralize solution with 0.1 N NaOH to first change in colour indicator.

 

(11)   Add 20ml. neutral urease solution, close flask with rubber stopper and let it stand for 1 hour at 20-25C.

 

(12)   Cool the flask in ice water slurry and titrate at once with 0.1 N HCl to full purple colour, then add approximately 5ml. excess.

 

(13)   Record total volume added, back titrate excess HCl with 0.1N NaOH to neutral end point.

Calculations: Percentage urea =(ml. 0.1 N HCl - ml 0.1 N NaOH) x0.3003 wt. of sample.

(Reference- methods of Analysis, AOAC, 1965)

[134][(xi a) Determination of Cyanamide nitrogen

Cyanamide nitrogen is precipitated as a silver complex and estimated in the precipitate by Kjeldahl's method.

(a)      Reagents:

                                                                              (i)          Ammonical Silver Nitrate Solution-Mix 500 ml of 10% silver nitrate (AgNO3) solution in water with 500 ml of 10% ammonia solution.

 

                                                                             (ii)         Glacial acetic acid

 

                                                                            (iii)         Remaining reagents as given in 3(ii).

(b)      Procedure:-

                                                                              (i)          Weigh 2.5 g (W) sample and place it in a small glass mortar.

 

                                                                             (ii)         Grind the sample 3 times with water, pouring off the water after each grinding into a 500 ml volumetric flask.

 

                                                                            (iii)         Transfer quantitatively the sample into 500 ml volumetric flask, washing the mortar, pestle and funnel with water.

 

                                                                            (iv)        Make up volume to approximately 400 ml.

 

                                                                             (v)         Add 15 ml of glacial acetic acid.

 

                                                                            (vi)        Shake on rotary shaker for 2 hours.

 

                                                                            (vii)        Make up the volume to 500 ml with water, mix and filter.

 

                                                                           (viii)       Transfer 25 ml of filterate into 250 ml beaker.

 

                                                                            (ix)        Add ammonia solution until slightly alkaline & add 20 ml of warm ammoniacal silver nitrate. Yellow precipitate will form.

 

                                                                             (x)         Leave over night. Filter using Whatman No. 40 filter paper and wash the precipitate with cold water until it is completely free of ammonia.

 

                                                                            (xi)        Place the filter& precipitate in a Kjeldahl flask.

 

                                                                            (xii)        Add 0.7 g copper sulphate, 15 g Potassium sulphate and 30 ml of H2SO4.

 

                                                                           (xiii)       Place flask in inclined position and heat gently.

 

                                                                           (xiv)       Boil bristly until solution becomes clear or pale green.

 

                                                                            (xv)        Continue digestion for 30 minutes more.

 

                                                                           (xvi)       Remove from burner and cool.

 

                                                                          (xvii)       Transfer the contents of Kjeldahl flask to 1 litre capacity, distillation flask, make volume to about 350 ml with water and a pinch of zinc dust. Mix and cool.

 

                                                                          (xviii)      Distill ammonia by adding 10 ml of NaOH (40%) and collect the distillate in receiver conical flask containing 25 ml of 0. 1N HCI or H2SO4 containing 5 drops of Methyl red indicator.

 

                                                                           (xix)       Titrate the contents in receiver conical flask with 0.1N NaOH & calculate the volume of 0.1 N HCl consumed (V).

 

                                                                            (xx)        Determine blank on reagents using same quantity of standard acid in receiver conical flask.

(c)      Calculation:

Cyanamide Nitrogen % (by weight) =Blank-V x 2.8./W]

                                            (xii)        Determination of biuret.

(a)      Reagents.

(1)     Alkaline tartarate solution-- Dissolve 40gm NaOH in 50ml. water cool, add 50gm. of NaK C4H4O64HP2Oand dilute to 1 liter. Let. it stand for one day before use.

 

(2)     Copper Sulphate solution - Dissolve 15 gm. CuSO4.5H2O in CO2P free water and dilute to 1 liter.

 

(3)     Biuret standard solution- 1mg./ml. Dissolve 100gm. reagent grade biuret in CO2free water and dilute to 100ml.

 

(4)     Ion exchange resin. Fill 50ml. burette with 30cm. column of Amberlite IR 120 (H) resin on glass wool plug.

Regenerate column after each use by passing 100ml. H2SO4 (1+9) or HCL (1+4) through the column approximately 5ml.per minute and then washing with water until pH of effluent is 6.0.

(b)      Preparation of standard curve.

(1)     Transfer series of aliquotes, 2-50 ml. of standard biuret solution to 100ml. volumetric flask.

 

(2)     Adjust volume to approximately 50ml with CO2 free water. Add one drop of methyl red and neutralize with 0.1 NH2SO4 to pink colour.

 

(3)     Add with swirling 20ml alkaline tartarate solution and then 20ml. CuSO4 solution.

 

(4)     Dilute to volume. Shake for 10 seconds and place in water bath for 15 minutes at 30+5C.

 

(5)     Also prepare reagent blank.

 

(6)     Determine absorbance of each solution against blank at 555 mw (instrument with 500-570 mw filter is also satisfactory ) with 2-4cm. cell. and plot standard curve.

(c)      Procedure.

A.        In urea.

(1)     Stir continuously 2-5 gm sample in 100ml. approximately 50C water for 30 minutes.

 

(2)     Filter and wash into 250 ml. volumetric flask and dilute to volume.

 

(3)     Transfer 25ml. aliquot to 100ml. volumetric flask and proceed as given under preparation of standard curve 3 (xii).

B.        In mixed fertilizers.

(1)     Stir continuously 10-20gm. sample in 150 ml. approximately (50 C) hot water for 30 minutes.

 

(2)     Filter and wash into 250ml volumetric flask and dilute to volume.

 

(3)     Transfer 25 ml aliquot to column 3 (xii) (a) (4) and adjust flow to 4- 5 ml./minute.

 

(4)     Receive elute in 100ml. beaker.

 

(5)     When liquid level falls to top of resin bed. wash with two 25ml portion water.

 

(6)     To eluate and washings add two drops of methyl red and then 0.1 N NaOH to yellow colour.

 

(7)     Add 0.1 NH2 SO4 until solution just turns pink .

 

(8)     Transfer to 100ml. volumetric flask and dilute to volume with CO2 free water.

 

(9)     Transfer 50ml. aliquot to 100ml. volumetric flask and proceed as in preparation of standard curve given above.

Calculation: From standard curve determine concentration of biuret in final dilution. then percent of

Biuret = C x 100 / W

Where C= concentration in mg/ml of biuret in final dilution obtained from standard curve.

W= Concentration of original sample in final dilution expressed as mg/ml.

(Reference -Methods of analysis, AOAC, 1965)

                                           (xiii)       Determination of free acidity in ammonium sulphate (as H2SO4)

(a)      Reagents

(1)     Standard sodium hydroxide solution- 0.02 N.

 

(2)     Methyl red indicator--Dissolve 0.15 gm. of water soluble methyl red in 500 ml. water.

 

(3)     Methyl red-- Methyl blue mixed indicator solution- prepared by mixing equal volumes of 0.2 percent solution in rectified spirit of methyl red and 0.1 percent solution in rectified spirit of methylene blue.

(b)      Procedure.

(1)     Dissolve about 20mg. of prepared sample, accurately weighed in about 50ml. cold natural water.

 

(2)     Filter and make up the volume to about 200ml.

 

(3)     Titrate with standard sodium hydroxide solution, using one or two drops of methyl red as indicator.

 

(4)     If satisfactory end point with methyl red is not obtained, methylene red-- methylene blue mixed indicator may be used.

 

(5)     Use- preferably a micro biuret for this titration.

The filtering medium shall be neutral and shall not contain any alkaline material which would neutralize free acid.

Calculations: Free acidity as H2SO4 percent by weight =4.904AN /W

A= Volume of ml. of standard NaOH solution.

N= Normality of standard NaOH Solution.

W= Weight in gm of prepared sample taken for the test.

(Reference - Specification of ammonium sulphate, fertilizer grade IS:826- 1967)

                                           (xiv)       Determination of arsenic in ammonium sulphate (A2O3)

(a)      Reagents

(1)     Lead acetate solution- prepare 10percent solution of lead acetate with sufficient acetic acid added to clear the solution.

 

(2)     Dry lead acetate paper-Cut filter paper (Whatman No.1 or equivalent) into strips 70x50 mm and keep them permanently suspended in lead acetate solution in a glass stopped bottle, Before use, take out the strips and cry them in an atmosphere free from hydrogen sulphide.

 

(3)     Mercuric bromide solution-- Dissolve 5gm of mercuric bromide in 100ml rectified spirit.

 

(4)     Sensitized mercuric bromide paper strips-- cut filter paper (Whatman NO. 1 or equivalent) into strips 120x2.5 mm. Keep the strips permanently suspended in dark in a glass stoppered cylinder or amber bottle having mercuric bromide solution. Before use take out a strip, press it between sheets of filter paper and dry it in an atmosphere free from hydrogen sulphide.

 

(5)     Dilute sulphuric acid- approximately 5N.

 

(6)     Concentrated hydrochloric acid.

 

(7)     Potassium iodide solution-15 percent.

 

(8)     Stannous chloride solution- Dissolve 80gm. of stannous chloride in 100ml. water containing 5ml. of concentrated hydrochloric acid and boil until clear solution is obtained. Add some metallic tin to the solution to prevent oxidation.

 

(9)     Zinc- It is recommended that zinc rods prepared as described below should be used for routine work. however, pellets described may be used.

(b)      Preparation of zinc rods.

(1)     Take a clean and dry hard glass test tube of 10mm internal diameter and 20 cm. length.

 

(2)     Heat the test tube over a flame of bunsen or blow pipe burner and add slowly arsenic free granulated zinc in small portion (1 to 2 gm at a time) the next portion being added after the first one has completely melted.)

 

(3)     Continue heating and adding zinc until the melt is about 10cm. high.

 

(4)     Heat the clean melt for half an hour and then cool to room temperature.

 

(5)     Break the tube to obtain the rod of zinc.

 

(6)     Cut rod into pieces 20mm long.

 

(7)     Coat the plane ends of the pieces with a paste of magnesium carbonate and gum arabic solution and dry.

 

(8)     Coat the pieces all over with 1.5 mm. thick layer or paraffin wax.

 

(9)     When required for use, scrap off the wax from the place ends with a knife, protecting wax colour round the rods.

 

(10)   Remove the paste from the plane ends by soaking in water and activate the exposed surface by dipping in a solution containing one part of stannous chloride solution and seven parts of concentrated hydrochloric acid.

(c)      Preparation of zinc pellets.

Treat zinc shots passing through IS sieve 570 (aperture 5660 microns) and retained on IS sieve 280 (aperture 2818 microns)with concentrated hydrochloric acid until the surface of zinc becomes clean and dully. Weight and keep under water, preventing contamination with dust.

(d)      Standard sodium hydroxide solution-- approximately 20 percent.

(e)      Standard arsenic trioxide solution.

(1)     Dissolve 1.0 gm. of resublimed arsenic trioxide (AS2 O3) in 25 ml. sodium hydroxide solution and neutralize with dilute sulphuric acid.

(2)     Dilute with freshly distilled water containing 10ml of concentrated sulphuric acid per liter and make up the volume to 1 liter.

(3)     Again dilute 10ml. of this solution to 1 liter with water containing sulphuric acid and finally dilute 100ml. of this solution to 1 liter with water containing sulphuric acid. One ml. of this solution contains 0.001 mg. of arsenic trioxide (AS2O3) the dilute solution shall be prepared freshly when required.

(f)       Procedure.

(1)     Dissolve 1.0 gm. of the prepared sample in 20ml water.

 

(2)     Place dry lead acetate paper in the lower portion of the tube B (in Figure 6) and glass wool moistened with lead acetate solution in its proper portion.

 

(3)     Place the sensitized strips of mercuric bromide paper in tube A and connect the tubes together with a rubber stopper.

 

(4)     Introduce the solution of the material into the bottle C (120 ml) and then add 10ml of dilute sulphuric acid. Add 0.5 ml. of stannous chloride solution 5ml. potassium iodide solution and make up the volume with water to about 50ml. (Figure No. 6- Modified Gutzet Method of test for arsenic.) 

 

(5)     Mix the contents and drop about 10mg. of zinc. Immediately fit in position the rubber stopper carrying the tube B.

 

(6)     Place the bottle.

 

(7)     At the end of two hours remove the test strip by means of tweezers.

 

(8)     Carry out the test prescribed above using a volume of standard arsenic trioxide solution containing 0.1 mg. of arsenic trioxide in place of the solution of the material and compare the stain produced with the material with that produced with arsenic trioxide solution.

 

(9)     The limit prescribed in the material specification shall be taken as not having been exceeded if the length of the stain as well as the intensity of its colour produced in the test with the material is not greater than those produced with the arsenic solution.

(Reference- Modified Gutzet Method of test for arsenic , IS-2088, 1962)

                                            (xv)        Determination of calcium nitrate (for calcium ammonium nitrate and nitrophosphates.)

(a)      Reagents

(1)     N-Amyl Alcohol.

 

(2)     Dilute hydrochloric acid- approximately 4N.

 

(3)     Standard calcium Solution-- weigh 1.0 gm of calcium carbonate dried at 1200+50C and dissolve in the minimum quantity of dilute hydrochloric acid. Dilute the solution to 1 litre in a graduated flask.

 

(4)     Ammonium chloride- ammonium hydroxide buffer solution . Dissolve 67.5 gm. ammonium chloride in a mixture of 570ml. of ammonium hydroxide (sp. gr. 0.92) and 250 ml. water. Also dissolve separately a mixture of 0.931 gm. of disodium ethylene diamine tetra-acetate dihydrate and 0.616 gm of disodium ethylene diamine tetra-acetate dihydrate and 0.616 gm of magnesium sulphate (Mg. SO4. 7H2O) in about 50ml. of water. Mix the two solutions and dilute to 1 liter.

 

(5)     Standard disodium ethylene diamine tetra-acetate (EDTA) solution- weight. 3.72gm. of disodium ethylene diamine tetraacetate dihydrate in water and dilute in a graduated flask to 1 liter. The solution shall be standardized frequently against standard calcium solution following the procedure given below.

 

(6)     Eriochrome black-T Indicator solution- Dissolve 0.1 gm in 20ml of rectified spirit. The solution shall be used for not more than a week.

(b)      Procedure.

(1)     Grind quickly about 5gm. of the material, accurately weighed, with about 50ml. of amyl alcohol in a pestle and mortar and transfer the contents to a conical flask.

 

(2)     Wash the pestle and mortar with a few ml. of amyl alcohol and add the washings to the flask.

 

(3)     Shake the content of the flask manually or in a mechanical shaker for about half an hour and then filter.

 

(4)     Transfer the filtrate to a separating funnel and extract calcium nitrate completely with water in five to six instalments.

 

(5)     A few drops of dilute hydrochloric acid may be added during the extraction with water to avoid formation of an emulsion of amyl alcohol with water.

 

(6)     Concentrate the water extract at low temperature to nearly half its volume.

 

(7)     Transfer the concentrated solution to a conical flask add 5ml. of ammonium chloride- ammonium hydroxide buffer solution, 5 drops of eriochrome black-T indicator solution and titrate against standard EDTA solution to a pure blue end point.

Calculations: Calcium nitrate percent by weight = 8.2 NV / W

Where N= Normality of standard EDTA solution

V= Volume in ml. of standard EDTA solution used in the titration and

W= Weight in gm. of the material taken for test.

(Reference--IS specifications of CAN IS: 2409-1963)

                                           (xvi)       Determination of chlorides other than ammonium chloride.

(a)      Reagents

(1)     Standard silver nitrate solution- 0.1N.

 

(2)     Concentrated nitric acid- conforming to IS:264-1950

 

(3)     Ferrous ammonium sulphate solution saturated in water and stabilized by addition of 50ml nitric acid.

 

(4)     Standard ammonium thiocyanate solution - 0.1 N.

(b)      Procedure.

(1)     Dissolve about 0.2 gm. of the prepared sample, previously dried as in procedure for determination of moisture and accurately weighted in about 40ml water.  

 

(2)     Add exactly 50ml. of standard silver nitrate solution and 5ml. of concentrated nitric acid.

 

(3)     Add 0.5 ml. of nitrobenzence and make up the volume of the mixture to exactly 100ml. with water.

 

(4)     Take exactly 50ml.. of the solution and add 2ml. of ferric ammonium sulphate solution.

 

(5)     Titrate the excesses of silver nitrate in this portion with standard ammonium thiocyanate solution.

 

(6)     Carry out a blank test following the procedure given as above but without using the material.

Calculations: Total chlorides (as Cl) percent = 7.07 (V1- V2)N

by weight (on dry basis) W

Where

V1= Volume in ml. of standard ammonium thiocyanate used in the blank determination.

V2= Volume in ml. of standard ammonium thiocyanate

solution used in the test with the material.

N= Normality of standard ammonium thiocyanate solution.

W= Weight in gm. of the drived prepared sample taken forthe test.

Express the ammoniacal nitrogen content percent by weight of the material determined earlier in terms of Cl as follows.Chloride equivalent of the ammoniacal nitrogen content percent by weight = 2.531 x A .....Y where A is the ammoniacal nitrogen content determined earlier. Balanced chloride equivalent to sodium chloride

(NaCl) percent by weight=1 - 648 x (X-Y)

(x-y) = Balanced chlorides other than ammonium chloride

(Reference- IS Specification for ammonium chloride Fertilizers grade (Revised) IS: 1114 -1964 calculations modified.)

                                          (xvii)       [135][Determination of oil in Neem Coated Urea

Principle :--Oil present in Neem coated urea is extracted with [136][a binary mixture of n-hexane and acetone] and separated from the aqueous phase. The solvent layer is then evaporated and the residue is weighed as oil.

Reagents : (i) [137][a binary mixture of n-hexane and acetone]

(ii) Dilute HCl: Prepare 1 : 1 HCl by adding 100 ml. conc. HCl to 100 ml. distilled water.

Procedure: (i) Weigh accurately about 200 gm Neem coated urea and transfer it to a 1000 ml separating funnel.

(ii) Add about 250 to 300 ml warm distilled water and shake gently to dissolve urea.

(iii) Add 50 ml [138][a binary mixture of n-hexane and acetone] and acidify with 5 ml dil. HCl. Mix well and separate the oily [139][a binary mixture of n-hexane and acetone] layer.

(iv) Repeat the extraction of oil from the aqueous layer with fresh 50 ml [140][a binary mixture of n-hexane and acetone] and mix the oily [141][a binary mixture of n-hexane and acetone] layer with that obtained in step (iii).

(v) Give washings to this oily [142][a binary mixture of n-hexane and acetone] with warm distilled water till it is completely free from urea.

(vi) Transfer the [143][a binary mixture of n-hexane and acetone] layer to an oil free 100 ml beaker. Give 2-3 washings to the separating funnel with about 10 ml [144][a binary mixture of n-hexane and acetone] each time to transfer completely the oil from the separating funnel to the beaker. '

(vii) Heat the contents in the beaker on a water bath to break any emulsion formed. Filter this oily layer into another previously weighed 100 ml beaker. Give two to three, 10 ml [145][a binary mixture of n-hexane and acetone] washings to the filter paper to transfer the oil completely into the weighed beaker. (viii) Evaporate [146][a binary mixture of n-hexane and acetone] by keeping beaker on a water bath at 105°C for about two hours. Cool in a dessiccator and weigh the contents to a constant weight. Find out the weight of this oil in the beaker.

(ix) Carry out a blank test with [147][a binary mixture of n-hexane and acetone] (with equivalent amount consumed in the test) for oily content present, if any, and subtract the same from the test results.

Calculation: [148][binary mixture of n-hexane-acetone soluble] (oil), ppm = 1000 x (W-Wb)/W

[149][binary mixture of n-hexane-acetone soluble] (oil), % = (W-Wb )/10 W

Where W is the weight of the oil in the beaker, in mg Wb in the weight of oil (in mg) in the blank, and W is the weight of the sample taken in gm.]

                                          (xviii)      [150][Method of Analysis for determination of Meliacin of Neem Oil in Neem Coated Urea by High Performance Liquid Chromatography.

1.        Take 2 kg of Urea sample in 5 ltr. capacity borosilicate glass beaker and add approximately 1 litre. of a binary mixture of n hexane and acetone so as to immerse completely the 2.0 kg Urea with n-hexaneacetone and keep it for 4-6 hours, preferably overnight with intermittent stirring the solution with a glass rod.

 

2.        Filter the content of the beaker containing urea dissolved in the n-hexane-acetone through Whatman filter paper no 41 with repeated washings of n hexane and acetone to complete washing of neem oil content from the Urea.

 

3.        Evaporate the collected n hexane and acetone soluble Neem extract by vacuum distillation maintaining temperature below 50oC and reduce the quantity of n-hexane-acetone to about 15 to 20 ml of Neem Oil extract, the temperature of flask should be maintained so that it should not be dried.

 

4.        Transfer the volume of n-hexane-acetone Soluble Extract from the distillation flask to the pre-weighed beaker of 100 ml capacity. Again evaporate the n hexane and acetone from the Neem Oil Extract at a controlled temperature on water bath.

 

5.        Add 5 ml of Methanol : Water (90:10) mixture to the beaker consisting Neem Oil Extract covered with Aluminum foil to check the spillage during the sonicating.

 

6.        Keep the beaker on sonicator and sonicate it for 10 minutes.

 

7.        Transfer the content of beaker into Centrifugal tube and centrifuge it at 2500 rpm for 10 minutes.

 

8.        Collect the upper layer and pass it through C-18 solid phase extraction Cartridge (Supelco or equivalent).

 

9.        Now analyze the Neem Oil Extract derived from the Neem Coated Urea to determine the Azadirachtin, Nimbin and Salannin content by HPLC of following main configuration :

Column : C-18

Detector : UV - Vis

Temp : Ambient

Wave length : 215 nm

Mobile phase : Aceto nitrile : Water (isocratic or gradient flow)

10.     Before analysis of sample standardize the HPLC using the good purity (>90%) Standard Reference Material of Azadirachtin (A & B,) Nimbin, Salannin, 6-deacetyl Nimbin and 3-deacetyl Sallanin.

11.     After calibration of the instrument, inject the 20 micro ltr. sample by Syringe or Loop into the HPLC. Wavelength 215 nm acetonitrile water

12.     Identify the peak of Azadirachtin (A & B) Nimbin, Salannin, 6-deacetyl Nimbin and 3-deacetyl Sallanin with their retention time.

13.     Measure the area of peak and calculate the content of Azadirachtin (A & B) Nimbin, Salannin, 6-deacetyl Nimbin and 3-deacetyl Sallanin with multiplying the dilution factor as per BIS-14299 1995.

Preparation of Reference standard : Weigh accurately approx 2.0 mg standard reference material (Azdirachtin, Nimbin & Salannin ) of known purity into 50 ml volumetric flask and dissolve in Methanol: Water (90:10). Make up to mark and shake well. Take 2 ml of this solution and transfer in solid phase extraction cartridge and elute it in to 10 ml volumetric flask with repeated washing with Methnaol : Water (90:10). Make upto mark and use for calibration of HPLC.

Calculation:

4. Determination of phosphates.

Methods of determination of total phosphates, [151][water soluble phosphorus, citrate soluble phosphates (available phosphorus)], citrate insoluble phosphates and citric acid soluble phosphates have been described separately in this section. These methods are applicable to straight as well as mixed phosphatic fertilizers.

(i)       Preparation of solution of the samples. (Separate methods of preparing solutions of the samples have been described according to the nature of the sample.)

(a)      Reagent

Magnesium nitrate solution- Dissolve 950mg.

P-free Mg(NO3)2 6H2 in water and dilute to 1litre.

(b)      Procedure.

(1)     Treat 1gm sample by (A), (B), (C), (D) or (E) method depending on the nature of the sample.

(2)     Cool solution transfer to 200 to 250ml. volumetric flask dilute to volume, mix and filter through dry filter.

(A)     (Suitable for materials containing small quantities of organic matter) Dissolve in 30ml. HNO3 and 3-5 ml. HCl and boil until organic matter is destroyed.

 

(B)     (Suitable for fertilizers containing much Fe or Al phosphate and basic slag). Dissolve in 15-30 ml. HCl and 3-10 ml. HNO3.

 

(C)     (Suitable for organic material like cotton seed meal alone or in mixture). Evaporate with 5ml. Of the Mg. (NO3)2 solution, ignite and dissolve in HCl.

 

(D)     (Generally applicable to materials or mixtures containing large quantities of organic matter). Boil with 20-30 ml. H2SO4 in 200ml.flask adding 2-4 gm of NaNO3 or KNO3at beginning of digestion and small quantity after solution is nearly colourless, or adding the nitrate in small portions from time to time. When solution is colourless, cool, add 150 ml. Water and boil for few minutes. Before adding NaNO3 or KNO3 let mixture digest, at gentle heat if necessary, until violence of reaction is over.

 

(E)     (Suitable for all fertilizers). Boil gently for 30-45 minutes with 20-30ml. HNO3 in a suitable flask (preferably a Kjeldahl for samples containing large quantities of organic matter to oxidize all easily oxidizable matter) Cool and add 10-20 ml. of 70-72 percent nearly so and transparent dense fumes appear in flask. Do not boil to dryness at any time (danger). (with samples containing large quantities of organic matter temperature should be raised to fuming point approximately 170C over a period of 1 hour at least) Cool slightly, add 50ml. water and boil for few minutes.

(ii)      Gravimetric quinoline, molybdate method for determination of total phosphorus.

(a)      Reagents.

(1)     Citric molybdic acid reagent- Dissolve 54 gm. 100 percent molybdic anhydride (MoO3) and 12gm. NaOH with stirring in 400ml. hot water and cool. Dissolve 60gm. citric acid in mixture of 140 ml. HCL and 300ml. water and cool. Gradually add molybdic solution to citric acid solution with stirring. Cool, filter and dilute to 1litre. (Solution may be green or blue colour depends on exposure to light). If necessary add 0.5 percent KrO3 solution drop by drop until green colour becomes pale. Store in dark in polyethylene bottle.

 

(2)     Quinoline solution -Dissolve 50ml. synthetic quinoline with stirring in mixture of 60ml. HCl and 300ml Water. Cooldilute to 1 litre, and filter. Store in polyethylene bottle.

 

(3)     Quimociac reagent- Dissolve 70gm. of sodium molybdate dihydrate in 150 ml. water Dissolve 60gm citric acid in mixture of 85ml. HNO3 and 150ml. water and cool. Gradually add molybdate solution to citric acid-nitric acid mixture with stirring. Dissolve 5ml. synthetic quionoline in mixture of 35nl. HNO3 and 100ml. water Gradually add this solution to molybdate citric -nitric acid. solution mix and let it stand for 24 hours. Filter add 28 ml. acetone. dilute to 1 litre with water and mix well. Store in polyethylene bottle.

(b)      Procedure.

(1)     Treat 1mg. sample as prescribed in 4(1) and dilute it to 200ml.

(2)     Pipette into 500ml erlenmeyer flask aliquot containing not more than 25mg. P2O5 dilute to approximately 100ml with water.

Proceed with one of the following methods.

A.        Add 30ml. citric molybdic acid reagent and boil gently for 3 minutes. (Solution must be precipitate free at this stage) Remove from heat and swirl carefully. Immediately add from burette 10ml quinoline solution with continuous swirling (Add first 3-4 ml drop wise and remainder in steady steam) or

B.        Add 50ml quimociac reagent, cover with watch glass place on hot plate in well ventilated hood and boil for 1 minute. After treatment with A or B cool to room temperature, swirl carefully 3-4 times during cooling filter into gooch with glass fibre filter paper previously dried at 250 C and weighed, and wash five times with 25ml. portion of water. Dry cruicible andcontents for 30 minutes at 250C. cool in desiccator to constantweight as (C9H7N) 3H3PO4.12 MoO3 subtract weight reagent blank.

Multiply by 0.03207 to obtain weight of P2O5. Report as percent P2O5.

(iii)     Determination of water soluble phosphorus

(a)      Procedure

(1)     Place 1gm sample on 9cm filter paper and wash with small portion of water until filtrate measure approximately 259ml.

 

(2)     Let each portion pass through filter before adding more and use suction if washing would not otherwise be complete within 1 hour.

 

(3)     If the filtrate is turbid, add 1-2 ml. HNO3dilute to 250ml and mix.

 

(4)     Pipette into 500ml. Erlenmeyer flask aliquot containing not more than 25mg. P2O5.

 

(5)     Dilute if necessary to 50ml.

 

(6)     Add 10ml. HNO3 (1plus 1) and boil gently for 10minutes. Cool and dilute to 100ml. and proceed as 4(ii) (b)(2) (B).

(reference- methods of analysis AOAC, 1965)

(iv)    Citrate insoluble phosphorus.

(a)      Reagents.

1.        Ammonium citrate solution - should have specific gravidity of 1.09 at 200C and pH of 7.0 as determined electometrically.

Dissolve 370 gm crystalline citric acid in 1.5 litre distilled water and nearly neutralize by adding 345 ml. NH4OH (28-29% NH3) if concentration of ammonia is less than 28 percent add correspondingly larger volume, and dissolve citric acid in correspondingly smaller volume of water, cool and check pH. Adjust with NH4 OH (1 plus 7) or citric acid solution to pH 7.Dilute solution if necessary to specific gravity of 1.09 at 200 C(Volume will be approximately 2 litres) Keep in tightly stoppered bottles and check pH from time to time. If pH has changed from 7.0 readjust.

2.        Other reagents and solutions as in 4(i) and 4(ii)

(b)      Procedure (acidulated samples and mixed fertilizers)

(1)     After removing water soluble P2O5. in 4(iii) transfer filter and residue within 1 hour to 200or 250 ml flask containing 100ml. ammonium acetate solution previously heated to 650C.

 

(2)     Close flask tightly with smooth rubber stopper.

 

(3)     Shake vigorously until paper is reduced to pulp and relieve pressure by removing stopper momentarily.

 

(4)     continuously agitate contents of stopper flask in apparatus equiped to hold contents of flask at exactly 650C. (Action of apparatus should be such that dispersion of sample in citrate solution is continually maintained and entire inner surface of flask and stopper is continually bathed with solution).

 

(5)     Exactly 1 hour after adding filter and residue, remove flask from apparatus and immediately filter contents by suction as rapidly as possible through Whatman No. 5 paper or equivalent. using buchner or ordinary funnel with platinum or other cone.

 

(6)     Wash with distilled water and at 650C until volume of filtrate is approximately 350ml. allowing time for through draining before adding more water.

 

(7)     If material is one that will yield cloudy filtrate wash with 2 percent NH4 NO3 solution.

 

(8)     Determine P2O5. in citrate insoluble residue by one of the following methods.

A.        Dry paper and contents transfer to crucible ignite until all organic matter is destroyed and digest with 10-15 ml. HCl until all phosphate dissolve or.

B.        Treat wet filter and contents a s in method prescribed in 4(i) (b) (2) (A) (C) (D) or (E) Dilute solution to 250ml. or other suitable volume, mix well filter through dry paper and determine P2O5. as in 4 (ii)

(Reference - methods of Analysis, AOAC, 1965)

(v)      Citrate soluble phosphorus [152][(Available Phosphorus)]

(Reference S.O. 403 (E) dated 23 May, 1990)

Subtract citrate insoluble P2O5. from total P2O5.to obtain citrate soluble P2O5. in fertilizers other than basic slag.

(a)      Reagents.

(1)     Concentrated hydrochloric acid.

 

(2)     Concentrated citric acid.

 

(3)     Calcium carbonate finely ground

 

(4)     5 N Sodium hydroxide solution.

 

(5)     Dilute hydrochloric acid- Dilute 240 ml or concentrated hydrochloric acid with water to 1 litre.

 

(6)     Citric molybdic acid solution- Stir 54 gm of molybdic anhydride (MoO3) with 200ml. of water add 11gm of sodium hydroxide and stir the mixture whilst heating to boiling point until the molybdic whilst heating to boiling point until the molybdic anhydride dissolves. Dissolve 60gm of citric acid in about 250to 300 ml of water and add 140 ml of concentrated hydrochloric acid. Pour the molybdate solution into the acid solution. Which is stirred solution through paper pulp pad. Dilute the solution to 1 litre. If the solution is slightly green or blue in colour add dropwise a dilute (0.5 to 1.0 percent) solution of potassium bromate until the colour is discharged. This reagent should be kept in dark.

 

(7)     Quinoline solution- Measure 60ml of concentrated hydrochloric acid and 300 to 400 ml of water into 1 litre beaker and warm to 700C-800C pour 50ml. of quinoline in a thin stream into the dilute acid while stirring. When quinoline has dissolved. cool the solution dilute acid to 1 litre and if necessary filter through a paper pulp filter.

 

(8)     Sodium hydroxide solution- 0.5 N carbonate free.

 

(9)     Indicator solution- Mix three volumes of thymol blue solution and two volumes of phenolphthalein solution prepared as follows.

A.        Thymol blue solution- Dissolve 250mg. thymol blue in 5.5 ml of 0.1 N sodium hydroxide solution and 125 ml of industrial methylated spirit. Dilute with water to 250ml.

B.        Phenolphthalein solution- Dissolve 250mg. phenolphthalein in 150 ml of industrial methylated spirit and dilute with water to 250ml.

(10)   Hydrochloric acid- 0.5N.

 

(11)   Sodium hydroxide solution- 0.1N.

 

(12)   Hydrochloric acid- 0.1 N.

 

(13)   Surface active agent- 0.5 percent solution of sodium dodecyi benzene sulphonate suitable.

(b)      Preparation of solution.

(1)     Weigh to the nearest mg. about 5gm. of the sample and transfer to a stoppered bottle of about 1 litre capacity.

 

(2)     Dissolve 10gm. of pure crystallized citric acid (monohydrate) in water dilute to 500ml and adjust the temperature to 200C.

 

(3)     Add the solution to the sample in the bottle, shaking so as to avoid the possibility of caking.

 

(4)     Shake the bottle continuously for 30 minutes.

 

(5)     Pour whole of the liquid at once on to a large medium fine filter. and collect the filtrate. If the filtrate is not clear, pass it again through the same filter.

(c)      Procedure.

(1)     Transfer a volume of the solution prepared according to procedure given above containing less than 70mg. of phosphoric acid and preferably about 50mg. to a 500ml stoppered conical flask marked at 150ml.

 

(2)     Dilute the solution with water to 100ml.

 

(3)     If the sample does not contain calcium add 100 to 200mg. of calcium carbonate.

 

(4)     Then add 5 N sodium hydroxide solution dropwise until a faint permanent turbidity or precipitate is formed.

 

(5)     Dissolve the precipitate by the dropwise addition of dilute hydrochloric acid but avoid an excess.

 

(6)     Dilute to 150 ml and add 50ml of the citric-molybdic acid reagent and heat the solution to incipient ebullition, maintain it at this temperature for 3 minutes and then bring it to the boiling point.

 

(7)     From burette slowly add 25ml of the quinoline solution with constant swirling throughout the first few ml. being added dropwise, the rest in slow stream.

 

(8)     Keep the solution gently boiling during the addition.

 

(9)     Immerse the flask in boiling water for 5 minutes, then cool it to 150C in funning water.

 

(10)   Filter with suction the contents of the flask on a paper pulp pad, and wash the flask precipitate and filter with successive small washes of cold water until they are free from acid.

 

(11)   Transfer the filter pad and precipitate to the original flask, rinse the funnel with water and collect the rinsings in the flask.

 

(12)   If necessary, wipe the funnel with small piece of damp filter paper to ensure complete removal of the precipitate and place the paper in the flask.

 

(13)   Add water to a total of about but not exceeding 100ml Stopper the flask and shake it vigorously until the pulp and precipitate are completely dispersed.

 

(14)   Remove the stopper and wash it with water returning the washing of the flask.

 

(15)   Add a measured volume of 0.5 N sodium hydroxide solution sufficient to dissolve the precipitate and leave a few ml. in excess.

 

(16)   Shake the flask vigorously until all the precipitate dissolves. (To facilitate the dispersal of the precipitate, after the addition of 0.5 N sodium hydroxide solution a few drops of the surface active agent may be added if necessary)

 

(17)   Add 0.5 -1.0 ml of the indicate solution and titrate the excess of sodium hydroxide with 0.5 N hydrochloric acid until the indicator changes from violet to green-blue and then very sharply to yellow at the end point.

 

(18)   Deduct the number of ml of 0.5 N hydrochloric acid used from the number of ml. 0.5 N sodium hydroxide equivalent to the phosphoric acid.

 

(19)   Carry out a blank determination on all the reagents. omitting only the sample and using 0.1 N standard alkali and acid instead of 0.5 N for the titration. Calculate the blank in terms of 0.5 N alkali and subtract it from the original result.

 

(20)   Calculate the amount of phosphoric acid in the portion taken for analysis from the factor 1.0ml. of 0.5 N Sodium hydroxide = 1.366 mg P2O5

(Reference -Statutory Instruments 1960 No. 1165 Agriculture, the fertilizer and feeding stuffs Regulations. 1960)

(vi)    Free phosphoric acid as (P2O5)

(a)      Reagents.

(1)     Acetone-conforming to IS:170-1950 specification for acetone.

 

(2)     Standard sodium hydroxide solution-0.1 N

 

(3)     Bromocresol green indicator solution- dissolve 0.1 gm of bromocresol green in 100ml of rectified spirit conforming to IS323-1959specification for rectified spirit (Revised).

(b)      Procedure.

(1)     Weigh accurately about 2.5 mg of the prepared sample and transfer to a soxhlet extract or

 

(2)     Add about 100ml of acetone and extract for three hours.

 

(3)     Cool and distil off the acetone as far as possible.

 

(4)     Take up the residue with water and make up the volume to 250ml.

 

(5)     Pipette out exactly 100ml of this solution and titrate with standard sodium hydroxide solution, using bromocresol green as indicator until colour just changes from yellow to blue.

Calculations: Free phosphoric acid (as P2O5)

Percent by weight = -17.75 x V x N/W

Where

V= Volume in ml of standard sodium hydroxide solution used.

N= normality of standard sodium hydroxide solution and

W= weight in gm of sample taken for the test.

(Reference- IS Specification for superphosphate (revised)

IS 294- 1962)

5. Determination of potassium.

Determination of potassium in all kinds of fertilizers is given in this section. Two alternative methods have been described. Any of these two methods may be used depending upon the availability of reagent and suitability of the method.

(i)       Prechloric acid method.

(This method depends on the insolubility of potassium perchlorate and the solubility of sodium perchlorate in alcohol and is applicable in presence of alkali metals chlorides and nitrates. Sulphates and ammonium salts must be absent on account of the low solubility of sodium sulphate of ammonium perchlorate in alcohol. Phosphates must be removed. Methods are given for the elimination of the effect of interfering substances)

(a)      Reagents.

(1)     Concentrated hydrochloric acid.

 

(2)     Barium chloride solution- Dissolve 100gm of barium chloride in water filter the solution and dilute to 1 litre.

 

(3)     Dilute hydrochloric acid-- Dilute 240 ml of concentrated hydrochloric acid with water to one litre.

 

(4)     Calcium oxide 0-- finely ground.

 

(5)     Ammonium hydroxide solution- sp. gr. 0.88.

 

(6)     Ammonium carborate solution- saturated aqueous solution.

 

(7)     Ammonium oxalate solution saturated aqueous solution.

 

(8)     20 percent perchloric acid solution.

 

(9)     Alcohol industrial methylated spirit 95-96 percent V/V.

 

(10)   Wash solution- Add potassium perchlorate to alcohol and shake until saturated solution is obtained, Keep the solution over solid potassium perchlorate and filter immediately before use.

(b)      Potassium salts free from sulphates and other inferfering substances.

(1)     Dissolve in water a portion of the sample weighed to the nearest mg. equivalent to potassium content to 1.5 to 2.0 mg. of potash.

 

(2)     Cool the solution to 200C dilute to 500 ml in a volumetric flask mix well and filter through a dry filter.

 

(3)     Determine the potash in 50ml of solution by precipitating with perchloric acid as described under procedure.

(c)      Potassium salts with sulphates or other interfering substances.

(The following method is given for eliminating the interference caused by presence of sulphate. If salts contain phosphates, iron, manganese or substances other than sulphate that interfere with the determination of potash the method described for mixed fertilizer should be used.)

(1)     Weigh to the nearest mg a portion of the sample equivalent in potassium content to 1.5 to 2.0 mg of potash into a 500ml beaker. Add about 300ml of water and 20ml concentrated hydrochloric acid and heat the solution to boiling.

 

(2)     To the boiling solution cautiously add, drop by drop barium chloride solution in an amount slightly in excess of that previously determined as necessary to ensure the complete precipitation of sulphate.

 

(3)     Cool the liquid to 200C transfer to a 500 ml volumetric flask, dilute to 500 ml. mix and filter through a dry filter.

 

(4)     Take 50ml of the filtrate and evaporate to dryness in a basin. moisten the residue with concentrated hydrochloric acid.

 

(5)     Again evaporate to dryness, dissolve the residue with 5-10 ml dilute hydrochloric acid and filter, if necessary.

(6)     Determine the potash in solution by the method described under procedure.

(d)      Potassium in mixed fertilizers.

(1)     Weigh to the nearest centigram about 10gm of the sample and if organic matter is present , gently incinerate at temperature not exceeding 5000C.

 

(2)     Transfer the weighed portion of the sample or the incinerated residue to a 500ml breaker with a little water add 10ml concentrated hydrochloric acid and then warm for ten minutes.

 

(3)     Dilute with water to about 300ml and bring gradually to boiling point.

 

(4)     Add 10gm of calcium oxide made into a paste with water.

 

(5)     Bring contents again gently to the boiling point and keep so heated for about half an hour with frequent stirring .

 

(6)     Cool to 200C transfer to a 500ml volumetric flask dilute to 500ml and after thoroughly shaking filter through a dry filter paper.

 

(7)     Transfer 250ml of the filtrate to another 500ml volumetric flask, make just acid with hydrochloric acid and heat to boiling point.

 

(8)     To the boiling solution cautiously add drop by drop, barium chloride solution until there is no further precipitation of barium sulphate.

 

(9)     Render the contents of the flask alkaline with ammonium hydroxide solution and precipitate the calcium and any excess of barium by adding ammonium carbonate solution until no further visible precipitation occurs followed by the addition of about 1ml of ammonium oxalate solution.

 

(10)   Cool to 200C dilute with water to 500ml and after thoroughly shaking filter through a dry filter paper.

 

(11)   Measure 100ml of the filtrate and evaporate to dryness in a basin. Expel the ammonium salts from the residue by gently heating the basin over a low flame, being careful to keep the temperature below that of faint redness.

 

(12)   Cool the residue, moisten with concentrated hydrochloric acid and again evaporate to dryness.

 

(13)   Take up the residue with water and filter if necessary.

 

(14)   Determine the potash in the solution by precipitation with perchloric acid as described under procedure.

(e)      Procedure.

(1)     Transfer the solution obtained as described above into a basin and add about 7ml of perchloric acid solution.

 

(2)     Place the basin on a hot plate or sand bath and evaporate the contents until the transparent fumes are copiously evolved.

 

(3)     Cool and dissolve the precipitate in a little hot water.

 

(4)     Add about 1ml of perchloric acid solution and again concentrates to the fuming stage.

 

(5)     Thoroughly cool the residue in the basin and stir in 20ml. or alcohol.

 

(6)     Allow the precipitate to cool and settle, then pour the clear liquid through a dry filter paper, drain the precipitate in the basin and stir in 20ml or alcohol.

 

(7)     Allow precipitate to cool and settle then pour the clear liquid through a dry filter paper, drain the precipitate in thebasin as completely as possible.

 

(8)     Redissolve the precipitate on the paper and that remaining in the basin with hot water.

 

(9)     Add 2ml of perchloric acid solution to the combined solution and evaporate the whole down to the fuming stage.

 

(10)   Cool the residue in the basin and throughly stir the contents with 20ml. of alcohol.

 

(11)   Allow the precipitate to cool and settle and pour the clear liquid through a weighed gooch or sintered glass crucible, draining the precipitate as completely as possible from the liquid before adding 5mnl of wash solution.

 

(12)   Wash the precipitate by decantation with several similar small portions of the wash solution, pouring the washing through the crucible.

 

(13)   Transfer the precipitate to the crucible and wash it well with the wash solution until free from acid.

 

(14)   Dry the precipitate at 1000c and weight.

 

(15)   Regard the precipitate as potassium perchlorate (KClO4) and calculate its equivalent as potash (K2O) by multiplying its weight by 0.34.

(Reference- Statutory Instruments 1960 No. 1165 Agriculture the Fertilizer and Feeding Stuffs Regulation 1960).

(ii)      Sodium tetraphenyl boron method-This method is applicable to both mixed and straight potassium fertilizers.

(a)      Reagents.

(1)     Sodium hydroxide solution-20 percent. Dissolve 20gm NaOH in 100ml distilled water.

 

(2)     Formaldehyde solution-37 percent.

 

(3)     Sodium tetraphenyl boron (STPB) solution- approximately 1.2 percent. Dissolve .012gm sodium tetraphenyl boron in approximately 800 ml water. Add 20-25 ml Al (OH3 )stir for 5 minutes, and filter (Whatman No. 42 paper or equivalent) into 1 litre volumetric flask, Rinse beaker sparingly with water and add to filter. Collect entire filtrate add 2ml 20 percent NOH solution, dilute to volume with water and mix. Let it stand for 48 hours and standardize. Adjust to that 1ml STPB-1 percent K2O. Store at room temperature.

 

(4)     Quaternary ammonium chloride solution- approximately 0.625 percent. Dilute 50ml of 12.8 percent zephiran chloride to 1litre with water, mix and standardize. Cetyltrimethyl. If other concentration is used, adjust volume.

 

(5)     Clayton yellow- 0.04 percent. Dissolve 40mg in 100ml water.

(b)      Standardization of solutions.

(1)     Zephiran chloride-to 1.0ml STPB solution in 125 ml. Erlenmeyer flask add 20-25 ml water 1ml 20 percent NaOH 2.5 ml HCHO 1.5 ml 4 percent (NH4) 2 C2O4 and 6-8 drops of indicator (5) above.

 

(2)     Titrate to pink end point with zephiran chloride solution, using 10ml semimicro burette, Adjust zephiran chloride solution so that 2.0 ml = 1.0 ml STPB solution.

 

(3)     Sodium tetraphenyl boron solution- Dissolve 2.5 gm of KH2 PO in water in 250 ml volumetric flask, add 50ml 4 percent (NH4) 2C2O4solution, dilute to volume with water and mix.

(It is not necessary to brig to boil) Transfer 15ml aliquot (51.92 mg (K2 O43.10mg K) to 100ml volumetric flask add 2ml 20 percent NaOH, 5ml HCHO and 43 ml STPB reagent. Dilute volume with water, mix throughly, let stand 5-10 minutes and pass throughly dry filter. Transfer 50ml aliquot of filtrate to 125 ml. Erlenmeyer flask add 6-8 drops of indicator

(4)     above and titrate excess reagent with zephiran solution.

Calculate titration values as follows.

F= 34.61 (43 ml-ml zephiran) =% K2 O/ml STPB reagent. factor applies to all fertilizers if 2.5 gm sample is diluted to 250 ml and 15 ml aliquot is taken for analysis, If results are to be expressed as K rather than K2O, substitute 28.73 for 34.61 in calculating the value of F.

(c)      Preparation of solution.

(1)     Mixed fertilizer.

A.        Place 2.5 gm sample or factor weight. 2.430 gm in 250 ml volumetric flask.

 

B.        Add 125 ml water and 50ml saturated (NH4) 2C2O4 solution. Add 1ml of diglycol stearate solution if needed to prevent foaming.

 

C.        Boil for 30 minutes add slight excess of NH4OH and after cooling dilute to 250ml. Mix and pass through dry filter.

(2)     Potassium salts (Potassium chloride sulphate, potassium magnesium sulphate, and kainite)

A.        Dissolve 2.5 gm or factor weight 2.430 gm and dilute to x 250 ml without adding NH4OH and (NH4) 2C2O4

 

B.        When interfering substances such as NH3, Ca, Al, etc. are present proceed as in (1) above.

(d)      Procedure.

(1)     Transfer 15ml aliquot of sample solution to 100ml volumetric flask and add 2ml 20percent NaOH and 5ml HCHO.

 

(2)     Add 1ml standard STPB solution for each 1percent K2O expected in sample plus additional 8ml excess to ensure complete precipitation.

 

(3)     Dilute to volume with water mix thoroughly, let it stand for 5-10 minutes and pass it through dry filter (Whatman 12 or equivalent).

 

(4)     Transfer 50ml filtrate to 125 ml Erlenmeyer flask,. add 6-8 drops of indicator (5) above and titrate excess reagent with standard zephiran solution.

Percent K2O in the sample = (ml STPB added-ml zephiran)X F where F= percent-

K2O/ml STPB reagent. (Reference- Methods of Analysis, AOAC, 1965)-

6. Method of analysis of anhydrous ammonia

(i)       Estimation of water and ammonia.

(a)      Scope

This method is for the determination of water at 200C (or room temperature) (and usually ammonia by difference) of any essentially anhydrous ammonia liquid product. Normally, the water will be low (less than 0.5 percent) or sample of synthetic ammonia.

(b)      Apparatus.

(1)     Ammonia sampling tubes.

 

(2)     Fume hood with exhaust dust.

 

(3)     Sample tube holder rack in hood fabricated as convenient to hold number of tubes desired.

 

(4)     Gloves, protective, elbow length.

(c)      Reagents

Charcoal, reagent, 14-20 mesh.

(d)      Procedure.

(1)     Remove the sample tubes from the sample carrier and place in the provided sample tube holders in the fume hood.

 

(2)     Allow the ammonia sample to boil and to evaporate (approximately 30 minutes) spontaneously in the fume hood. Because of the low temperature of the boiling ammonia atmospheric moisture freezes on the sample container. Exercise care to see that none of this ice contaminates the sample.

 

(3)     When the boiling of the sample ceases, remove the tube from the holder. Wipe the outer surface of the tube dry and read and record the volume of liquid residue in the tube.

 

(4)     From the volume recorded, calculate the weight percent water in the sample. Ignore the small piece of charcoal, if used.

Calculation: Percent water = A x F x 0.890 x 0.684 / V x 0.682 x 100

Where A = Volume of residue in tube (ml)

V = volume of sample taken (ml)

F = Evaporation factor, taken from table 1 corresponding to noted sample pressure when sample was obtained.

0.890=density of residue (gm/ml)

0.684=wight fraction of water in residue.

0.682=density of sample (gm/ml)

Precaution: The evaporation in the fume hood should be conducted with the window lowered to protect personnel from possible spray. Whenever it is necessary to handle the sample tubes, protective gloves should be worn.

Note: Determination of residue on evaporation will not usually be necessary for normal ammonia sample. If sample is clear and water residue is clear and colourless, the residue may be considered to be nil. However, should it become necessary to determine the dissolved solids and suspended solids in anhydrous ammonia, proceed, as follows:

(e)      Sampling

Thoroughly clean and dry the sample tubes, weigh (W1) each selected tube to the nearest milligram with a similar tube as counterpoise. Obtain the sample as desired earlier.

(f)       Apparatus.

(1)     Analytical balance.

 

(2)     Ammonia sampling tubes.

 

(3)     Rubber tubing 1/4" OD length desired.

 

(4)     Reagents

(g)      Air dry, carbondioxide –free

(h)     Procedure

(1)     Start test following elimination of the water content of the sample as given earlier.

 

(2)     Connect one end of a rubber hose to a source of dry, carbon dioxide free air, Insert the other end of the hose into the sample tube and gently force air through the sample tube until all liquid has been evaporated and no ammonia gas remains in the tube.

 

(3)     Wipe a counterpoise and the sample tube containing the residue to substantially the same extent to remove moisture which may have condensed on their outer surfaces.

 

(4)     Weigh the sample tube and residue to nearest milligram.

 

(5)     Calculate the weight percent residue of the sample.

Calculation: percent residue = (W2-W1) x f x 100 / V x 0.682

Where W1 =weight (gm) 0f tube (before sampling).

W2=weight (gm) of tube and residue.

V =Volume of sample taken (ml).

F =Evaporation factor, taken from Table 1 corresponding to noted sample pressure when sample was obtained.

0.682 =density of sample (gm/ml).

(i)       Precaution.

A check of completeness of evaporation may be made by visual inspection and by carefully smelling the air in the tube making sure that no carbon dioxide or moisture from the sample tube.

(j)       percent ammonia content (by difference)

In general, the ammonia content of the sample will be percent ammonia =100 (percent water percent residue, if determined).

(i)      Precaution

The evaporation in the fume hood should be conducted with teh window lowered to protected personnel from possible spray. Whenever it is necessary to handle the sample tubes protective gloves should be worn.

(ii)    Determination of oil content.

(a)      Apparatus.

(1)     500 ml conical flask calibrated to hold 300ml (about 200gms)of sample and with a bunk fitted with glass through which the exit gas. can be led away to a safe place. Ensure the glass tube and exit line are free from constructions.

(2)     Platinum dish 75 mm in diameter.

(b)      Reagent

The reagent use shall be of a recognised analytical reagent quality like petroleum spirit with a boiling range of 400 to 600C.

(c)      Procedure

(1)     Quickly running the sample (as per the sample procedure) upto the calibration mark, insert the bunk.

 

(2)     Immerse the flask in a continuous stream of cold water and allow the ammonia to evaporate slowly.

 

(3)     When the evaporation is complete, remove the bunk and gently blow out the last traces of ammonia with a small jet of filtered air free from carbon dioxide.

 

(4)     Dry the outside of the flask.

 

(5)     Place the flask in an oven at 105+50C for 15 minutes to remove the moisture blowing out the last traces with a gentle stream of filtered air at the end of this period allow to cool.

 

(6)     Add to the flask approximately 100ml of the petroleum spirit and swirl to dissolve the oil.

 

(7)     Filter the solution through a small filter paper (a Whatman No. 31 paper is suitable)direct into the platinum dish previously traced to the nearest 0.1 mg.

 

(8)     Repeat the operation with two more successive 10ml portions of petroleum spirit, filtering through the same paper as before into the same dish.

 

(9)     Evaporate the combined extracts to dryness on a water bath in a fume cup board, taking care to avoid naked lights and finally dry in an oven at 105+50C for 30 minutes.

 

(10)   Allow the dish to cool thoroughly in desicator and weigh again to the nearest 0.1 mg.

 

(11)   At the same time, carry out a blank determination on the petroleum spirit and filter paper.

 

(12)   Make an appropriate correction in the calculation

Calculation: Oil content, parts per million by weight = (W1 W2)-W3 / 0.68 V2 x 106F / 0.68 V2

Where W1= Weight in grams of platinum dish and residue.

W2 = Weight in grams of dish alone.

W3= Weight in grams of oil in blank determination

V2 = Volume in ml of sample taken.

F = Evaporation factor taken from table 1 corresponding to noted sample pressure when sample was obtained.

Table 1- Evaporation factor for different vessels or line pressures

Note : When a sample of liquid ammonia is transferred to an open flask/tube from a container n which the pressure is higher than the atmospheric that environment. some of the liquid ammonia will evaporate and since the ammonia so lost as vapour contains non-volatile constituents present in the original product, the concentration will increase in the liquid sample taken. This may be significant factor the known thermo dynamic properties of ammonia an appropriate correction. This correction is usually known in this context as the evaporation factor of flask factor and is simply that fraction by weight of the original liquid ammonia which remains as liquid in the sample. Multiplication of the determined quantity of a non-volatile constituents (oil, water dissolved or suspended solids, etc) by the evaporation factor given a result which will be closer to the true figure. The Table above presents the evaporation factor for different vessel or line pressure. When a sample is transferred (example by gravity from a container of a cylinder or the sampler at the same pressure, there should be no loss by evaporation and in this case it is not necessary to use evaporation factor.

7. Method of analysis of zinc sulphate (Both Heptahydrate and Monohydrate)*

(i)       Quality of reagents

Pure chemicals and distilled water shall be used in tests.

Note: Pure chemicals shall mean chemicals that do not contain impurities which affect the results of analysis.

(ii)      determination of matter insoluble in water.

(a)      Reagents

Dilute sulphuric acid - 10 percent

(b)      Procedure

Dissolve 25.0 gm of the material in 125 ml of water and add 1ml of dilute sulphuric acid. Heat the solution to boiling, filter through a weighted and prepared Gooch crucible or sintered glass crucibel (G No.4) and wash the residue throughly with hot water. Dry the crucibel at 1100+50C to constant mass.

Calculation: Matter insoluble in water percent by mass weight=4A

Where A= weight in g of the residue.

(iii)     Determination of Zinc in Zinc Sulphate by modified EDTA titration method.

(a)      Reagents

(1)     E.D.T.A. Solution

Dissolve 3.72 g of Di-sodium Ethylene Diamine Tetracetate dihydrate in distilled water and make up the volume to 1litre

(2)     Standard Zinc metal solution:

Weigh about 1.0g of zinc metal and record the weight accurately. Express this as W, Add HCL (1:1) @ 20ml per g of zinc metal keep it for few hours and allow it to dissolve completely. Make up the volume of the solution to exactly 1000ml.

(3)     Ammonium Hydroxide (20%) (m/m)

 

(4)     Ammonium Chloride -AR grade salt

 

(5)     Sodium Cyanide -AR/GR grade salt.

 

(6)     Eriochrome Black (T) indicator mixture Mix thoroughly 1g of Eriochrome Black (T) indicator with 100g of AR grade sodium chloride.

 

(7)     Formaldehyde -Acetic Acid solution (4%)Dissolve 100ml of Formaldehyde (37-40%) in about 100ml of distilled water. Add 40ml glacial Acetic acid and make volume to 1litre with distilled water.

 

(8)     Hydroxylamine HydrochlorideAR Grade solid salt.

(b)      Procedure.

(1)     Standardization of EDTA solution.

(A)     Take 10ml of Zinc metal solution (Standard)

 

(B)     Add about 0.1 g of ammonium chloride and 30ml of ammonium hydroxide solution (20%)

 

(C)     Dilute it by adding about 30ml distilled water.

 

(D)     Add a pinch of eriochrome black (T) indicator mixture.

 

(E)     Titrate in with EDTA solution to obtain clear blue end point Note the volume of EDTA used as V1 ml.

(2)     Estimation of Zinc in samples.

(A)     Weigh accurately 1.0 g of a given zinc sulphate sample and dissolve it in 100ml of distilled water in a volumetric flask

 

(B)     Take 10ml of aliquot in beaker. Add 0.1 g of hydroxylamine hydrochloride and 0.1 g of ammonium chloride

 

(C)     Cautiously add small quantity of sodium cyanide. White precipitate will appear, Continue adding sodium cyanide till transparent precipitate disappears while swirling the beaker with hand. Add about 0.5 excess of sodium cyanide.

 

(D)     Dilute it by adding about 30ml of ammonium hydroxide (20%) and add about 30ml of distilled water.

 

(E)     Add a pinch of eriochrome black (T) indicator mixture. It will give red colour.

 

(F)      Titrate with EDTA solution till there is a sharp change to violet colour. Note the volume of EDTA used as V2 (ml)

 

(G)     Add 20ml of Formaldehyde -acid solution into above titrated solution and mix well. Red colour will reappear.

 

(H)     Titrate it with EDTA solution to get blue end point without red tinge. Note the volume of EDTA used in second titration as V3ml.

Calculation: Zinc % = 10 / V1 X V3 x W

W = Weigh in g of piece of Zinc metal taken for preparation of standard zinc solution

V1 = Volume of EDTA solution (in ml) used for 10ml of Zinc metal

V3 = Volume of EDTA solution (in ml)used for second titration

(iv)    Colorimetric method for determining of copper.

(a)      Reagent-

Outline of the method Sodium diethyldithiocarbamate reacts with slightly acidic or ammonical solution of coper in low concentration to produce a brown colloidal suspension of the cupric diethtyldithiocarbamante. The suspension can be extracted with an organic solvent and the colour extracted determined spectrophotometrically.

(b)      Apparatus

Photometer Any suitable photoelectric colorimeter.

(c)      Regents.

1.        Ammonium citrate solution 40percent (m/v)

 

2.        Sodium diethyldithiocarbamate 0.1 percent (m/v)

 

3.        Standard copper solution- Clean the surface of a copper wire with sand paper. Dissolve 100 mg of pur copper in dilute nitric acid. Heat the solution nearly to dryness to drive off the acid. Add about 10 ml of water and heat again nearly to dryness. Take upthe residue in water, add 25 ml of 1 N sulphuric acid and dillute to 1000 ml. One mililitre iof this solution contains 0.1 mg of copper (as Cu)

Alternatively dissolve 3.928g cupric sulphate (CuSO25H2O) in sufficient water containing 1 or 2 ml of concentrated sulphuric acid and dilute to 1000 ml. One ml of the solution contains 1.0 mg of copper (as cu)

(d)      Preparation of sample.

(1)     Weigh 5g sample accurately, dissolve in distilled water and add 1ml of sulphuric acid. Filter the solution and make up to 250 ml with water in a volumetric flask. Take 50 ml or the above solution in a beaker, heat, pass hydrogen sulphide gas or add sodium sulphide solution and ensure complete precipitation. Filter hot and keep the filtrate for subsequent analysis.

 

(2)     Boil the residue with diluter nitric acid and filter , if necessary To the filtered solution add sulphuric acid, evaporate, dilute and filter. Keep the residue for determination of lead.

(e)      Procedure for determination of copper.determine copper in the filtrate from (d) (2) above by diethyldithiocarbamate method as detailed below:-

Transfer an aliquot containing not more than 0.65 mg of copper to a 100ml. separating funnel. Add 2ml of ammonium citrate solution and adjust the pH to 8.5 with ammonium hydroxide. The presence of ammonium ions helps to dionize iron, if present, and to prevent rapid fading of developed colour. Add 10ml of sodium diethyldithiocarbamate solution and develop the colour. Extract the coloured complex with 5-19ml of carbon tetrachloride. Separate the carbon tetrachloride layer from aqueous layer and centrifuge for 5 minutes to separate the water droplets. Transfer the carbon tetrachloride solution to a photometeric cell and measure its absorbance at the wave length of maximum absorption 440 ms relative to reagent blank. Calculate the corrected absorbance by subtracting the reading obtained for the solution containing no copper.

Transfer to a series of 100 ml separating funnels aliquot of standard copper solution corresponding to 0,0.1,0.2,0.5,1.0,2.0 and 2.5 mg of copper and proceed exactly as prescribed above. Plot a graph of corrected, absorbance of solution against their copper contents.

Note: If bismunt is suspected it has to be separated or otherwise accounted for.

Calculation: Calculate the corrected absorbance by subtracting the value obtained for the black from that obtained for the test solution and read from the calibration curve the corresponding mass of copper.

Copper (as Cu), cent by mass = M1 / M2 x 100

Where M1 = mass in g of copper as determined in the given aliquot of the test solution, and M2 = mass in g of the material present in the aliquot of the test solution.

(v)      Determination of lead by colorometric method using dithizone.

(a)      Apparatus

Nessler cylinders - 50ml capacity.

(b)      Reagents.

(1)     standard lead solution- Dissolve 0.40 g of lead nitrate (pb(NO3)2)in water containing 2 or 3ml of concentrated nitric acid and make up the volume to 1000ml with water. Transfer 10ml of this solution to a volumetric flask add 20or 3 ml of concentrated nitric acid and dilute with water to 1000 ml. One milliliter of this solution contains 2.5 mg of lead (as pb.) The diluted solution shall freshly prepared.

 

(2)     Dilute ammonium hydroxide- 1N, approximately.

 

(3)     Reagent A- Dissolve 25g of triammonium citrate or 22 g of citric acid and 4 g of hydroxylamine hydrochloride in about 200ml of water. Add dilute ammonium hydroxide to bring the pH to 8.5 Dilute the solution to 500ml. Purify this solution by extracting with 15ml portions of 0.01 percent dithizone solution until the final colour of the dithizone extract is green. Wash the aqueous remainder portion three times with 25ml portions of chloroform and finally with 25ml portion of carbon tetrachloride.

 

(4)     Dithizone (diphenyl thiocarbazone or phenylazothiomoformic acid ) solution- Dissolve 0.001 g of dithizone in 100ml of carbon tetrachloride, shaking intermittently for 1 hour. Allow to stand overnight and shake once again before using. This shall be kept in a cool and dark place. This gives a 0.01 percent solution. Filter if necessary. Dilute 10ml of this solution to 100ml with carbon tetrachloride in a 100ml volumetric flask. This shall be prepared fresh before determination. This gives a solution of 0.001 percent

Note -1: carbon tetrachloride used should be further purified. One Liter of carbon tetrachloride is extracted with two portions of 25ml dilute ammonium hydroxide and then kept over 100g of activated carbon. Before use, it is decanted and distilled at about

Note -2: Sometimes dithizone solid and its 0.01 percent solution deteriorate on storage. The 0.01 percent solution should, therefore be tested before further dilution, by shaking 2ml of the solution should, therefore be tested before further dilution by shakeing 2ml of the solution with 5ml of 1 percent ammonium hydroxide. If the organic layer is only faintly yellow under these conditions, the solution may be used. If it is deeply coloured it shall be discarded and fresh solution may be used. If it is deeply coloured it shall be discarded and fresh solution be prepared. The solution as well as the reagent should be stored in a refrigerator and exposure to sunlight should be avoided during analytical work. To increase the stability of 0.01 percent solution, it should be covered with a thin aqueouslayer saturated with sulphur dioxide.

(5)     Thymol blue indicator solution- 1 percent (m/v) solution-in rectified spirit.

(c)      Procedure

(1)     Take several aliquots of standard lead solution into a series of separating funnels, add 5ml of the water and 10ml of the reagent A. Then add 2 drops thymol blue indicator and bring the pH of the solution to 8.5 by addition of dilute ammonium hydroxide. Add 5ml of the dithizone solution and shake well for about 10 seconds. Drain the organic layers into stoppered Nessler cylinders.

 

(2)     Dissolve the residue obtained in iv (d)(2) above, in dilute nitric acid and dilute with water. Take a suitable aliquot of the solution and transfer to a separating funnel. Develop the colour as prescribed above. Drain the organic layer into a stoppered Nessler cylinder, add 10ml of dilute ammonium hydroxide and shake for about 10 seconds. Compare the colour developed with those of the standard solution. Note the volume of the standard with which the colour of the test solution matches.

Note: If the colour of the test solution is intermediate between two standard solutions. then the experiment is repeated by taking more number of standard solutions in that range and exact colour matching is arrived at.

Calculation: Heavy metal (as pb) percent by mass = 100 x Y x f /M

where V= Volume in ml of standard lead solution matching with the test solution

f= mass in g of heavy metals (as Pb) equivalent to 1ml of standard lead solution and

M= mass in g of the material in the aliquot taken for the test.

(vi)    Determination of magnesium in the sample material.

(a)      Reagents.

(1)     Eriochrome black T indicators- Dissolve 0.1 g of eriochrome black T in 25ml of methyl alcohol.

 

(2)     Ammonium hydroxide -ammonium chloride buffer solution- Mix 350 ml of ammonium hydroxide (20percent w/w) with 54 g of ammonium chloride, Dilute with water and make up the volume to 1000 ml (the pH of the solution should not be more than 10)

 

(3)     Standard magnesium solution- 0.01 M weigh 2.4640 g of magnesium sulphate (MgSO4.7H2O) and dissolve it in water. Make up the volume to one litre.

 

(4)     Ethylenediamine tetra-acetate (EDTA) solution- Dissolve 3.72 g of disodium ethylenediamine tetra-acetate dihydrate in water and make up the volume to one litre.

(b)      Procedure

Standardization of EDTA solution- Take 10ml of standard magnesium solution in a conical flask. Add 20ml of water, one millilitre of eriochrome black T indicator and 25ml of ammonium hydroxide ammonium chloride buffer solution. Heat at 40 to 50 C and then titrate with EDTA solution, maintaining the temperature between 40 and 50 C until the colour changes form wine red to distinct blue.

Molarity of EDTA Solution = 10M1 / V1

Where M1= Molarity of standard magnesium solution and

V1= Volume in ml of EDTA solution used for titration

(c)      Determination of magnesium in the sample material

Take the filterate from (iv) (d) (1) (after removal of copper) add a few drops of concentrated nitric acid. boil and cool and then add solid ammonium chloride (about 2 grams) boil and cool and ammonium hydroxide till the strong smell of ammonia comes and filter the precipitate through sintered crucible take this filterate and add dilute sulphuric acid till the solution is acidic (test with methyl red) heat the solution to boil and add excess of di-ammonium-hydrogen phosphate with continuous stirring. Add 10 percent ammonia solution with continuous stirring till the solution is just alkaline (test with methyl red) while precipitate of zinc ammonium phosphate will be formed (the optimum pH of r precipitation is 6-7 allow it to stand for 3-4 hours. Filter through whatman filter paper no. 40.collect the filterate in a volumetric flask. Make up the volume (say 100ml) Take a suitable aliquot (say 10ml) for the determination of magnesium. Add 20ml of water, one ml of eriochrome black-T indicator and 20ml of ammonia hydorxide ammonia chloride buffer solution. Heat to 40C to 50C and titrate with standard EDTA solution maintaining the temperature between 40C and 50C until the colour changes from wine red to distinct blue.

1 ml of 0.01 M-EDTA = 0.2432 mg of 'Mg

Mg = X x 0.2432 / 5

Where X = volume of 0.1 M-EDTA use for titration.

The calculation factor 5 is derived presuming that 5g of material is taken for test and the filterate obtained is 100ml out of which 100ml is titrate.

(vii)   Determination of pH

Dissolve 5gm of the material in freshly boiled and cooled water.

Dilute to 100 ml and mix Determination the pH value of the solution a pH meter.

(viii)  Determination of iron in the sample material (Spectro-photometric Method)

(This method is applicable for Iron contents upto 1mg. in the final aliquot)

(a)      Outline of the method - In test solution iron is determined absorption metrically as Ferrous Iron forms red complex with Ortho-phenanthroline.

 

(b)      Appratus- Photo- elecric-- colorimete.

 

(c)      Reagents

(1)     Bromophenol blue indicator solution 0.4 percent solution in 95 percent ethanol.

 

(2)     Sodium citrate solution 25 percent.

 

(3)     Hydroquinone solution- 1 percent in an Acetic acid buffer of pH 4.5 obtained by mixing 65 ml of 0.1 M acetic acid with 35ml of 0.1 M Sodium Acetate solution.

 

(4)     Ortho-phenanthroline solution - 0.25 percent in 25 percent ethanol.

 

(5)     Dilute Hydrochloric acid- 1.3 (v/v)

 

(6)     Standard Iron solution - Dissolve 0.7002 gm. of Ammonium Ferrous Sulphate (AR) in distilled water containing 2ml of perchloric acid and dilute to 100ml with water. One ml of this solution contains 1mg of Iron.

(d)      Preparation of sample solution

Boil 1 gm. sample in 20ml of Hydrochloric Acid (1:1) for 20 minutes and filter through Whatman No. 40 filter paper in 100ml. volumetric flask. Follow with repeated extraction with boiling dilute Hydrochloric acid (1:5) decanting the solution each time through the same filter paper. Dilute the filterate to 100ml.

(e)      Procedure.

(1)     Take 5ml of the sample solution add bromophenol blue indicator solution and titrate with Sodium Citrate solution until yellow colour changes to blue.

 

(2)     Take another 5ml of sample solution in a 25 ml. volumetric flask. Add 1ml of Hydroquinone solution, 3ml of Ortho-phenanthroline solution and an amount of Sodium Citrate solution equivalent to the above titration in step (1) Dilute with distilled water to 25ml. Allow the solution to stand for one hour.

 

(3)     Measure the absorbance of test solution at 510 nm using 1cm. cell and also blank with water.

 

(4)     Place 4,8,12,16 and 20ml of standard Iron solution in a series of 100ml.

 

(5)     Using 5ml. aliquot proceed as for sample solution.

 

(6)     Measure the absorbance of the solution and plot a graph relating to absorbance to number or mgs. of Iron

Calculation: Percent Fe = 2X / W

Where X = concentration (in mg.) of Iron in final sample solution

aliquot as determination from the graph.

W= Weight in gm. of material taken for the preparation of sample

solution"

8. Alternate method of analysis of zinc sulphate (both Heptahydrate) and monohydrate)

(i)       Quality of reagents.

1.        Unless specified otherwise pure chemicals and glass distilled or demineralise water shall be use in test.

Note: Pure chemicals means chemicals that do not contain impurities which affect the results of analysis.

Demineralised water means the water obtained after passing distilled water through a cation and a anion exchange resins or a combined cationation exchange resin.

(ii)      Determination of zinc.

(a)      Reagents.

(1)     Standard zinc solution- Weigh 0.4398 g of zinc sulphate (ZnSO4.7H2O) A.R. grade on a clear watch glass and transfer it to one litre flask through the funnel giving several washings to watch glass and funnel with glass distilled or demineralised water. Add one ml of 10percent sulphuric acid (A.R. grade) and make the volume upto the mark. Stopper the flask and shake the solution well. This is 100 ppm zinc solution herein after called Standard A. This solution should be stored in a clean bottle for further use. Dilute 10ml of 100ppm solution of zinc (Standard A) to 100ml to get 10ppm standard zinc solution designated as Standard B.

 

(2)     Glass distilled or mineralised water of pH 2.5 + 0.5 Dilute 1 ml of 10 percent sulphuric acid to one litre with glass distilled or mineralised water and adjust the pH to 2.5 with a pH meter using H2SO4 or NaOH. This solution is called acidified water and 5 to 10 litres of this solution should be prepared at a time.

 

(3)     Preparation of working standards- Pipette the following volume of Standard B in 50ml numbered volumetric flask and make the volume with acidified water (See Table on page. 93) Stopper the flasks and shake them well. Prepare the standard in duplicate. The same acidified water should be used for preparing the solution of unknown fertilizer samples. Fresh standards should be prepared every time when a fresh lot of acidified water is prepared.

(b)      Procedure.

(1)     Preparation of zinc sulphate fertilizer sample- Weigh 0.25 g of the material on a clean watch glass and transfer it to one litre volumetric flask through the funnel giving repeated washings with glass distilled water and dissolve the material by shaking well. There make the volume upto mark with glass distilled water and shake well.

 

(2)     Take 5ml of the prepared solution in 250ml volumetric flask and make the volume with acidified water. Shake the solution well and filter through Whatman No. 42 filter paper in dry clean flasks. The flasks should be rinsed with a 10 to 15 ml of the filterate and then continue filtration.

 

(3)     Flaming the solutions-- Flame the standards and the filtered samples on atomic absorption spectrophotometer at a wavelength of 213.8 mu (Zn line of the instrument)

Calculations: Prepare a standard curve of know concentrations of zinc solution by plotting the absorbance values on Y-axis against their respective zinc concentration on X-axis Calculate the percentage zinc in zinc fertilizer by multiplying zinc concentration value calculation from standard curve by 20 Example.

Weigh of the fertilizers sample ..................= 0.25 g

Volume made.......................................= 1000ml

Further dilution .................................= 50times

Reading of the samples form atomic absorption.....= Y

Corresponding concentration value of zinc from standard curve against Y absorbance...............= X ppm

Percentage zinc in the fertilizer.................= 20(X)

(c)      Precautions.

(1)     Weighing must be done on a electric balance.

 

(2)     All the glass apparatus to be used should be of corning make and washed with dilute hydrochloric acid (1:4) and washed thoroughly. with distilled and then with demineralise water.

 

(3)     The pipette should be rinsed with the same solution to be measured.

 

(4)     The outside or the pipette should be wiped with filter paper after taking out form the solution to be measured.

 

(5)     After using the pipette, place them on a clean dry filter paper in order to prevent contamination.

 

(6)     To start filtration only a few drops should be added first in order to wet the filter paper and then continue further filtration.

(iii)     Determination of magnesium.

(a)      Reagents.

(1)     Strontium chloride- Dissolve 7.5 g of strontium chloride (SrCl26H2O) in one litre of glass distilled water.

 

(2)     Standard magnesium solution- Weigh 0.507 g of magnesium sulphate (MgSO4.7H2O) on a clean watch glass and transfer it to one litre flask through the funnel giving several washings to watch glass and the funnel with glass distilled or demineralise water. This is 50ppm Mg solution Dilute 10ml of 50 ppm solution of Mg to 100ml to get 5 ppm standard Mg solution.

1.        Preparation of working standards- Pipette the following volume of 5 ppm standard Mg solution in 50ml numbered volumetric flasks. Add 10ml of strontium chloride solution to each flask and make up the volume to 50 ml. Stopper the flask and shake them well prepare fresh standards every for night

(b)      Procedure.

(1)     Pipette 20ml of the solution which was prepared for the determination of zinc by dissolving 0.25 g of the fertilizer sample in one litre flask (Step a-2.2.1) Add 10ml of strontium chloride Make up the volume to 50ml.

(2)     Flame the standards and the samples on atomic absorption spectrophotometer at a wave length of 285.5 mu (Mg line of the instrument)

Calculations: Prepare a standard curve of known concentrations of Mg solutions by plotting the absorbance value on Y-axis against their respective concentration values on X-axis. Percentage magnesium in the zinc fertilizer will correspond to the concentration vales calculated from the standard curve.

Example:

Weight of the fertilizer .............................= 0.25 g

Volume made...........................................= 1000ml.

Further dilution......................................= 2.5 times

Reading of the sample from atomic absorption

spectrophotometer.....................................= Y

Corresponding concentration of Mg from standard

curve against Y absorbance............................= X ppm

Percentage magnesium in the fertilizer...............= X

(iv)    Determination of copper.

(a)      Reagents.

(1)     Standard copper solution- Weigh 0.196 g of copper sulphate (CuSO4.5H2O) on a clean watch glass and transfer it to one litre flask through the funnel giving several washings to watch glass and the funnel with glass distilled water. Add one ml of 10 percent sulphuric acid and make up the volume upto the mark. Stopper the flask and shake the solution well. This is 50 ppm Cu Solution and should be stored in a clean bottle for further use. Dilute 10ml of 50 ppm solution of copper to 100 ml to get 5 ppm standard copper solution.

(2)     Glass distilled or mineralized acidified water of pH 2.5 + 0.5 (same as given in B (ii) (a)(2).

Preparation of working standards- Pipette the following volume of 5 ppm standard copper solution in 50ml numbered volumetric flasks and make the volume with acidified water.

Stopper the flask and shake them well. prepare fresh standard every fortnight.

(b)      Procedure.

(1)     The solution which was prepared for the determination of zinc by dissolving 0.25 g of the fertilizer sample in one litre flask step B(ii) (b)(1) should be used for the determination of copper

(2)     Flame the standards and the samples on an atomic absorption spectro photometer at a wavelength of 324.8 mu (Cu line of  the instrument)

Calculations: Prepare a standard curve of known concentrations of copper

solutions by plotting the absorbance values on Y-axis against their

respective concentration values on X-axis calculate the percentage

copper in the zinc fertilizer by multiplying the copper in the zinc

fertilizer by multiplying the copper concentration value calculated

from the standard curve by 0.4.

Example :-

Weight of the fertilizer sample .........................=0.25 g

Volume made..............................................=1000ml.

Reading of the sample from atomic absorption spectro photometer.............................................=Y

Corresponding concentration of copper from standard

curve against Y absorbance...............................=X ppm

Percentage copper in the fertilizer......................=0.4 x

(v)      Determination of lead.

(a)      Reagents.

(1)     Standard lead solution- Weigh 0.1599 g of lead nitrate (Pb(NO3)2) on a clean watch glass and transfer it to one litre flask through the funnel giving distilled or demineralised water. Add 10ml of concentrated distilled nitric acid and make the volume upto the mark. Stopper the flask and shake the solution well. This is 100ppm lead solution and should be stored in a clean bottle for further use. Dilute 10 ml of 100 ppm solution of lead to 100ml with 1 percent nitric acid solution to get 10 ppm standard lead solution.

 

(2)     1 percent nitric acid solution- Dilute 10ml of concentrated distilled nitric acid to one litre with glass distilled water.

 

(3)     20 percent zinc sulphate solution- Weigh 20g of zinc sulphate (ZnSO4.7H2O) and dilute to 100ml with 1 percent nitric acid solution.

Preparation of working standards- Pipette the following volume of 10 ppm standard lead solution in 50 ml numbered volumetric flasks. Add 5ml of 20 percent zinc sulphate solution to each flask and make the volume with 1 percent nitric acid solution.

Stopper the flasks and shake them well. 

(b)      Procedure.

(1)     Preparation of zinc sulphate fertilizer samples- Weigh 1 g of the material on a clean watch glass and transfer to 50 ml volumetric flask through the funnel giving washings with 1 percent nitric acid solution. Dissolve the material and make the volume with percent nitric acid solution. Samples should be prepared in duplicate.

 

(2)     Flaming the solution-- Flame the standards and the samples on atomic absorption spectrophotometer a a wavelength of 217 m (Lead line of the instrument)

 

(3)     Calculations- Prepare a standard curve of known concentrations of lead solution by plotting the absorbance values on Y - axis against their respective lead concentration on X -axis. Calculate the percentage lead in zinc fertilizer by multiplying lead concentration value calculated from standard curve by 0.005.

(vi)    Determination of pH

(a)      Procedure

Dissolve 5gm of material in freshly boiled water. Dilute to 100ml and mix. Determine the pH value of the solution with pH meter.

(vii)   Determination of matter insoluble in water.

(a)      Procedure

Dissolve 25.0 g of the material in 125 ml of water. Filter through a weighed and prepared Gooch crucible or sintered glass crucible (G.NO.4) and wash the residue thoroughly with water. Dry the crucible at 110+8 to constant mass.

Calculations: Matter insoluble n water percent by weight = 4A Where A= Weight in g of the residue

(viii)  Determination of Iron (Atomic Absorption Spectrophotometric method)

(a)      Reagents

(1)     Standard Iron solution (1000 ppm)- Weigh accurately 1gm. pure Iron wire and put it in approximately 30 ml of 6 N HCL in a beaker and boil. Transfer it to one litre volumetric flask through the funnel giving several washings to the beaker and funnel with glass distilled water. Make the volume upto the mark. Stopper the flask and shake the solution well. This is 1000 ppm Iron solution.

 

(2)     Glass distilled or demineralised water of pH 2.5 + 0.5.

 

(3)     Preparation of working standards- Pipette 10ml. Iron stock solution in 100ml. volumetric flask and dilute to volume. This is 100ppm Iron solution. Pipette the following volumes of 100 ppm Iron solution in 50ml volumetric flask and make the volume with acidified water.

Stopper the flask and shake the solution well

(b)      Procedure.

(1)     Preparation of fertilizer sample solution - weight exactly 1gm of the material on a clean watch glass and transfer it to a one litre volumetric flask through the funnel giving repeated washings with acidified water and dissolve the material by shaking well. Make the volume upto the mark with acidified water and shake well and filter through Whatman No. 42 filter paper in dry clean flask. The flask should be rinsed with a 10-15 ml. of filtrate and then continue filtration.

(2)     Flamming the solution - Flame the standards and the filtered sample on atomic Absorption Spectrophotometer at a wavelength of 248.3 nm using clean air acetylene flame.

Calculations: Prepare a standard cure of known concentrations of iron solution by plotting the absorbance value on Y - axis against the respective Iron concentration on X - axis. Determine the concentration of Iron in the sample solution from the graph.

Total Iron (as Fe) percent = X

Note : In case a sample has been analyzed by both the methods. Viz. indicated under the heading '7' and '8' the result obtained by the method indicated under the heading '8' shall prevail.

9. Method of analysis of manganese sulphate agricultural grade

(i)       Quality of Reagents Unless specified otherwise, pure chemicals and glass distilled or demineralized water shall be used in tests.

Note: 'Pure chemicals' means chemicals that do not contain impurities which affect the result of analysis. 'Demineralized water' means the water obtained after passing distilled water through a cation and a anion exchange resins or a combined cation-anion exchange resins.

(ii)      Determination of manganese.

(a)      Reagents.

(1)     Standard manganese solution: Weigh 3.0763 g of manganese sulphate (MnSO4H2O A. R. grade) on a clear watch glass and transfer it to one litre flask through the funnel giving several washings to watch glass and funnel with acidified water and make the volume up to the mark. This solution will be 1000 ppm Mn. A secondary dilution of 5 ml to 100ml with acidified water gives a 50 ppm working standard.

 

(2)     Glass distilled or demineralised water of pH 2.5+0.2 Dilute 1 ml of 10 percent sulphuric acid to one litre with glass distilled or demineralised water and adjust the pH to 2.5 with a pH meter using 10% H2SO4 or NaOH. This solution is called acidified.

 

(3)     Preparation of working standards: Pipette the following volume of working standard solution in 50 ml numbered volumetric flasks and make the volume with acidified water.

Stopper the flask and shake them well. Prepare the standard in duplicate. The same acidified water should be used for preparing the solution of unknown fertilizer samples. Fresh standards should be prepared every time when a fresh lot of acidified water is prepared.

(b)      Procedure.

(1)     Preparation of manganese sulphate fertilizer samples: Weigh exactly 0.4 g of the material on the clean watch glass and transfer it to a one litre volumetric flask through the funnel giving repeated washings with acidified water and dissolve the material by shaking well. Make the volume up to the mark with acidified water and shake well.

 

(2)     Take 5ml of the prepared solution in 250 ml volumetric flask and make the volume with acidified water. Shake the solution well and filter through Whatman No. 42 filter paper in dry clean flasks. The flasks should be rinsed with a 10 to 15 ml of the filterate and then continue filtration.

 

(3)     Flaming the solutions: Flame the standards and the filtered samples on atomic absorption spectrophotometer at a wavelength of 279.5m (Mn line of the instrument).

Calculation: Prepare a standard curve of known concentration of manganese solution by plotting the absorbance value on Y- axis against their respective manganese concentrations on X -axis Calculate the percentage manganese in manganese fertilizer by multiplying manganese concentration value calculated from the standard curve by 12.5.

(c)      Precaution.

(1)     Weighing must be done accurately with a precision balance.

 

(2)     All the glass apparatus to be used should be corning/pyrex make and washed with dilute hydrochloric acid (1:4) and washed thoroughly wish distilled and then with demineralised water.

 

(3)     The pipette should be rinsed with the same solution to be measured.

 

(4)     The outside of the pipette should be wiped with filter paper after pipetting the solution to be measured.

 

(5)     After using the pipette. place them on a clear dry filter paper in order to prevent contamination.

 

(6)     To start filtration only a few drops should be added first in order to wet the filter paper and then continue further filteration.

10. Alternative method of analysis of manganese sulphate, agricultural grade.

(i)       Quality of reagents

Unless specified otherwise. Pure chemicals and glass distilled or demineralised water shall be used in tests.

Note: Pure Chemicals' mean chemicals that do not contain impurities which affect the results of analysis.

'Demineralised water' means the water obtained after passing distilled water through a cation and anion exchange resins or a combined cation- anion exchange resin.

(ii)      Determination of manganese.

(a)      Reagents

(1)     Hydrogen peroxide (H2O2)- 30 percent.

 

(2)     Nitric acid (HNO3)- concentrated.

 

(3)     Orthophosphoric acid (H3PO4.from steel industry)- 85 percent.

 

(4)     Potassium periodate (KLO4).

 

(5)     Glass distilled or mineralised water of pH 2.5+0.5- Dilute 1 ml of 10percent H2SO4 to one litre with glass distilled or demineralised water and adjust the pH to 2.5 with a pH meter using 10% H2SO4 or NaOH.

 

(6)     Standard manganese solution- Weigh 3.0763 g of manganese sulphate (Mn SO4.H2O- A.R. grade) on a clear watch glass and transfer it to one litre flask through the funnel giving several washins to the watch glass and the funnel with acidified water and make the volume up to the mark. This solution will be 1000 ppm Mn. A secondary dilution of 5 ml to 100 ml with acidified water gives a 50 ppm working standard.

 

(7)     Preparation of working standard- Pipette 0.0, 0.5, 1.0,1.5, 2.0, 2.5, 3.0, 3.5, 4.0, 4.5 and 5.0 ml of standard solution of manganese in a series of 11 different 100 ml beakers. Evaporate the solutions to dryness at low temperature on a hot plate or steam bath. Add 5 ml of HNO3 and 2ml of 30%H2O2 Cover the beakers with watch glass and digest the contents on a steam bath or hot plate for 30 minutes. Remove the glass cover and evaporate the contents to dryness. Cool the beakers add 2ml of HNO3 5ml of phosphoric acid and heat till boiling. Again cool and mix the contents with 10ml of demineralised water. Add 0.3 g of KIO4 and heat the solutions on water bath until pink colour appears. Add about 20ml water and heat for about 40 minutes or until there is no more increase in colour intensity. Cool the beakers to room temperature. transfer the solutions to 50ml volumetric flasks. Make the volume with deionised water and shake throughly. The concentration of manganese ion will be as follows.

Measure the light transmittance at 540 m (green filter). Make the standard curve by plotting percent transmittance against the concentration of manganese.

(b)      Procedure

(1)     Analysis of manganese sulphate fertilizer sample- weigh exactly 0.500 g of the material on a clean watch glass and transfer it to a one litre volumetric flask through the funnel giving repeated washings with acidified water and dissolve the material by shaking well. Make the volume up to the mark with acidified water and shake well. Pipette one ml solution in a 100ml pyrex/corning beaker and proceed further as described above for preparation of standard curve and make the volume to 50ml. The standard and the test samples should be prepared and processed for estimation at the same time.

Calculation: The percentage of manganese in the manganese sulphate fertilizer sample is calculated by multiplying manganese concentration value calculated from standard curve by 10.

11. Method of analysis of Borax (Sodium Tetraborate decahydrate fertilizer)

(i)       Quality of reagents

Unless specified otherwise, pure chemicals and glass distilled water shall be used in tests.

Note: Pure chemicals means chemicals that do not contain impurities which affect the results of analysis.

(ii)      Determination of Boron.

(A)     Atomic Absorption Spectrophotometer Method.

(a)      Reagents

Standard Boron Solution- Weigh 44.095 g of sodium tetraborate decahydrate (Na2B4O710H2O)- AR grade on clean watch glass and transfer it to one litre volumetric flask through the funnel giving several washings to watch glass and funnel with glass distilled water. Make the volume upto the mark. Stopper the flask and shake the solution well. This is 5000 ppm boron solution herein after called standard A. This solution should be stored in clean bottle for further use.

Preparation of working standards- Pipette the following volume of standard A in 50ml numbered volumetric flasks and make the volume with water.

(b)      Procedure.

(1)     Preparation of sample solution:

Weigh 2.500 g of the material on a clean watch glass & transfer it quantitatively in a 250 ml volumetric flask through the funnel giving repeated washing with water. Make up the volume, stopper the flask & shake well.

(2)     Flamming the solution- Flame the standards & the sample solution on atomic absorption spectrophotometer at a wavelength of 249.8 mn using nitrous oxide acetylene flame.

Calculations: Prepare a standard curve of known concentrations of boron solutions by plotting the absorbance value on Y-axis Calculate the percentage boron in the given sample by multiplying boron concentration value obtained from standard curve by 0.01.

Example

Reading of sample from atomic absorption = Y

Corresponding concentration value of boron from standard curve

against Y absorbance = X ppm

Percentage of boron in the sample = 0.01X

(B)     Titrametric method

(a)      Outline of the method: Borax is determined by first converting it to boric acid with hydrochloric acid and then titrating against Sodium hydroxide solution after complexing boric acid with mannitol or sorbitol.

 

(b)      Reagents:

(1)     Standard hydrochloric acid- 0.5N

 

(2)     Standard sodium hydroxide-1.0N

 

(3)     Methyl red indicator- Dissolve 0.1 g of the material in 60 ml of rectified spirit and dilute with water to 100ml.

 

(4)     Phenolphthalein indicator-

Dissolve 1 g of the material in 100ml of rectified spirit.

(5)     Mannitol or sorbitol.

(c)      Procedure:

(1)     Dissolve 2.0 g of the material. accurately weighed in 60 ml of water & titrate with hydrochloric acid. using methyl red solution as indicator.

(2)     Boil & cool the solution.

(3)     Add 20 g of mannitol or sorbitol and titrate with sodium hydroxide, using phenolphthalein solution as indicator.

Calculation: Boron content, percent by weight =1.0819 V.N. /W

V= Volume in ml of standard sodium hydroxide used.

N= Normality of sodium hydroxide and

W= Weight in g of the material taken for the test

(Ref- ISI- 1109-- 1980)

(iii)     Determination of pH

Same as method No. 8 (vii) (a)

(iv)    Determination of pH

Dissolve 3.8 g of the material in water and make it to 100ml. Measure the pH value of the solution with the help of suitable pH meter, using glass electrodes.

(v)      Determination of lead:

Same as method No. 8 (v) substitute Zinc sulphate by borax

12. Method of analysis of Copper Sulphate Fertilizer (CuSO4.5H2O)

(i)       Quantity of Reagents:

Unless specified otherwise pure chemicals and glass distilled or demineralise water shall be used in tests.

Note: Pure chemicals means chemicals which do not contain impurities which affect the results of analysis.

Demineralised water, means the water obtained after passing distilled water through a cation and anion exchange resin or a combined cation anion exchange resin.

(ii)      Determination of Copper:

(A)     Atomic Absorption Spectrophotometer method:

(a)      Reagents: As specified in 8 (iv) (a)(1)(2) and (3)

 

(b)      Procedure:

(1)     Weigh 0.25 g of the material on a clean watch glass an transfer it to one litre volumetric flask through the funnel giving repeated washing with glass distilled water. Add one ml of 10 percent sulphuric acid and make up the volume.

 

(2)     Take 5ml of the prepared solution in 500ml volumetric flask and make up the volume. Shake the solution well and filter through Whatman. No. 42 filter paper in dry clean flask. The flask should be rinsed with a 10 to 15 ml of the filterate and then continue filtration.

 

(3)     Flamming the solutions: Flame the standards and the filtered samples on an stomic absorption spectrophotometer at a wavelength of 324.8 nm using air acetylene flame.

Calculation : Prepare a standard curve of known concentrations of Copper solution by plotting the absorbance values on Y-axis against their respective concentration values on X -axis

Percent, copper in sample =- 10X / W

Where W= Weight in g of the material taken for test.

X= Conc. of copper (in ppm) as

determined from the graph.

(B)     By lodometric Titration method

(a)      Outline of the method

copper is determined with the addition of potassium iodide and titrating the liberated iodine against standard sodium thio-sulphate solution.

(b)      REAGENT:

(1)     Sodium Carbonate.

 

(2)     Potassium Acid--AR—Crystals

 

(3)     Acetic Acid-----AR GRADE

 

(4)     Standard Sodium thiosulphate solution -O.IN

 

(5)     Starch indicator solution-Triturate 5 g of starch and 0.01 g of mercuric iodide with 30 ml of cold water and boiling water .Boil for three minutes. Allow to cool and decent off the supernatant clear liquid.

 

(6)     Potassium thiocyanate crystals.

(c)      Procedure:

(1)     Dissolve about 1 g of the test sample (accurately weighed) in 50 ml of water.

 

(2)     Add a pinch of sodium carbonate till a slight turbidity appears. Then add 5 ml of acetic acid. 3 g of potassium iodide and titrate the liberated iodine with sodium thiosulphate solution, using starch as an indicator until only a faint blue colour remains.

 

(3)     Add about 2 g of potassium thiocynate shake and continue the titration until the blue colour disappears.

Calculations: Copper percent by mass =-6.35 V.N. / M

Where V= Volume in ml of standard sodium thiosulphate solution.

N= Normality of standard thiosulphate solution and

M= mass in g of the sample taken for the test.

(Ref: IS-261 (1982).

(iii)     Determination of Lead (Pb)

same as method No. 8(v)

Substitute Zinc Sulphate by copper sulphate.

(iv)    Determination of Soluble Iron and Aluminum compounds (expressed as Fe)

(a)      Outline k of the method iron and aluminum are determined gravimetrically by precipitation with ammonium hydroxide.

(b)      Reagents:

1.        Concentrated nitric acid-- AR grade.

 

2.        Ammonium Chloride-- AR grade

 

3.        Dilute Ammonium Hydroxide- approximately 15 percent NH3 (m/v)

 

4.        Dilute Hydrochloric acid-33 percent (m/v)

(c)      Procedure:

(1)     Take 10g of the test sample and add 25 ml of water 2ml of nitric acid and 5 g of ammonium chloride.

 

(2)     Make the solution alkaline by adding ammonium hydroxide solution.

 

(3)     Keep it on a water bath until the precipitate has flocculated, keeping the solution alkaline by the addition of more ammonium hydroxide if necessary.

 

(4)     Filter and wash the residue with dilute ammonium hydroxide.

 

(5)     Dissolve the residue in hot dilute hydrochloric acid.

 

(6)     Make the solution again alkaline by adding ammonium hydroxide and allow the precipitate to settle.

 

(7)     Filter and wash the residue with water.

 

(8)     Dry the residue ignite and weigh till a constant mass is obtained.

Calculation: Solution iron and aluminum compounds

70M1

(as Fe) percent by mass = 70 M1 /M2

Where M1 = Mass in g of the residue obtained and

M2= Mass in g of the sample taken for the test

(Ref: IS: 261-1982)

(v)      Determination of matter insoluble in water Reagents:

(a)      Reagents:

(1)     Concentrated sulphuric acid- AR Grade.

(b)      Procedure:

Weigh accurately about 10 g of the test sample and dissolve in 100ml of water. Add 3 ml of sulphate acid and stir thoroughly at room temperature. Filter through a tared filter paper or tared Gooch or Sintered galas crucible (G. No. 4) Wash the residue with water till it is free from acid. Dry the filter paper or crucible in an oven maintained at a temperature of 105 to 110 C till constant mass is obtained.

Calculation: Insoluble matter, percent by mass = M1 x 100 /M2

Where M1 = Mass in g of the residue obtained for the test

M 2= Mass in g of the material taken for the test.

(vi)    Determination of pH.

(a)      Procedure:

Dissolve 5 g of the test sample in water and make up the volume to 100ml. Determine the pH with glass electrodes using a suitable pH meter.

13. Method of Analysis of Ferrous Sulphate (heptahydrate) FeSO47H2O)

(i)       Quality of Reagents

Unless specified otherwise, pure chemicals & glass distilled or demineralised water shall be used in tests.

Note: Pure Chemicals means chemicals that do not contain impurities which affect the results of analysis. Demineralised water means the water obtained after passing distilled water through a cation & an anion exchange resin or a combined cation-anion exchange resin.

(ii)      Determination of Ferrous Iron.

(a)      Outline of the method-Ferrous iron content is determined by titration with standard potassium permanganate solution.

(b)      Reagents:

1.        Dilute Sulphate acid- 4N approximately

 

2.        Standard Potassium permanganate solution- 0.1 N

 

3.        Orthophosphoric acid.

(c)      Procedure.

1.        Weigh accurately about 5 g of the prepared sample and dissolve it in water.

 

2.        Add 1 to 2 ml of dilute sulphuric acid and make up the solution to 250 ml in a volumetric flask.

 

3.        Pipette out exactly 50 ml of the solution in a flask .

 

4.        Add 10 ml of dilute sulphuric acid and 2 ml of Ortho-phosphoric acid and titrate with standard potassium permanganate solution.

Calculation: Ferrous iron percent by weight = 27.92 V.N./W

Where V= Volume of standard potassium permanganate used

N= Normality of standard potassium permanganate solution.

W= Weight in g of the material taken for the test.

(Ref: IS 262 - 1982)

(iii)     Determination of total iron:

(A)     Titrimetric method using potassium dichromate.

(a)      Outline of the method:

Total iron is determined by reducing ferric iron with stannous chloride and then titrating the total ferrous iron with standard potassium dichromate solution.

(b)      Reagents:

(1)     Concentrated hydrochloric acid.

 

(2)     Stannous chloride solution- Dissolve 6.0 g of stannous chloride crystals (SnCl2.2H2O) in 60 ml of concentrated hydrochloric acid and dilute with water to 100ml. Keep this solution in stopped bottle.

 

(3)     Mercuric chloride solution-saturated

 

(4)     Concentrated sulphuric acid.

 

(5)     Diphenylamine indicator- Dissolve 0.1 g of diphenylamine in 100 ml of concentrated sulphuric acid.

 

(6)     Standard potassium dichromate solution-1.0N

(c)      Procedure :

(1)     Weigh accurately about 5 g of the prepared sample and dissolve it in water.

 

(2)     Add 1 to 2 ml of dilute sulphuric acid and make up the volume to 250 ml in a volumetric flask.

 

(3)     Take 50 ml aliquot of this solution and add 10 ml of concentrated hydrochloric acid and heat to boiling.

 

(4)     Reduce the iron by adding stannous chloride solution until the yellow colour of the ferric chloride disappears. Do not add more than 2 to 3 drops of stannous chloride in excess.

 

(5)     Cool the solution, add rapidly murcuric chloride solution and stir so that a transparent precipitate of mercurous chloride forms slowly, indicting that a slight excess of stannous chloride is present.

 

(6)     Allow to stand for 5 to 10 minutes, dilute to 150 to 200 ml and add 5 ml of phosphoric acid and 5 drops of diphenylamine indicator. Titrate with standard potassium dichromate solution until the colour of the solution changes to a deep blue which does not fade on stirring.

Calculation : Total iron, percent by weight = 27.92 V.N. /W

Where V = Volume in ml of potassium dichromate used in titration.

N = Normality of standard potassium dichromate

solution and

W = Weight in g of the material present in the

aliquot

(Ref. IS: 262-1967)

(B)     Atomic Absorption Spectrophotometer Method :

(a)      Regents :

(1)     Standard Iron solution - ( 1000 ppm ) - weigh accurately 1 g pure iron wire and put it in approximately 30 ml. 6 N HCL, in a beaker and boil. Transfer it to one litre volumetric flask through the funnel giving several washings to the beaker & funnel with glass distilled water. Make the volume up to the mark. Stopper the flask and shake the solution well. This is 1000 ppm iron solution.

 

(2)     Glass distilled or mineralised water of pH 2.5 +0.5.

 

(3)     Preparation of working standards - pipette 10 ml iron stock solution in 100 ml volumetric flask and dilute to volume. This is 100 ppm iron solution.Pipette the following volumes of 100 ppm iron solution in 50 ml numbered volumetric flask and make the volume with acidified water.

Stopper the flask and shake the solution well.

(b)      Procedure :

(1)     Preparation of ferrous sulphate fertilizer sample: Weight exactly 1.000 g of the material on a clean watch glass and transfer it to a one litre volumetric flask through the funnel giving repeated washings with acidified water and dissolve the material by shaking well. Make the volume up to the mark with acidified water and shake well.

 

(2)     Take 5 ml of the prepared solution in 100 ml volumetric flask and make up the volume with acidified water. Shake the solution well and filter through Whatman No.42 filter paper in dry clean flasks. The flasks should be rinsed with a 10 to 15 ml of the filtrate and then continue filtration.

 

(3)     Flamming the solutions - Flame the standards and the filtered sample on atomic absorption spectrophotometer at a Wavelenght of 248.3 nm using clean air-acetylene flame.

Calculation : Prepare a standard Curve of known concentrations of iron solutions by plotting the absorbance value on Y axis against their respective iron concentrations on X axis. Determine the concentration of iron in the sample solution from the graph.

Total iron % = 2 X/W

Where X = Concentration of Fe ( in ppm ) obtained from the standard curve.

W = Weight in g of the material taken for the test.

(iv)    Determination of Ferric iron -

Substract the value of Ferrous iron percent from total iron percent to obtain the Ferric iron percent in the sample.

(Ref. IS : 262-1967)

(v)      Determination of pH -Dissolve 5.0 g of the sample in 100 ml of freshly boiled and cooled water and determine the pH by means of pH meter using glass electrode.

(vi)    Determination of matter insoluble in water -

Same as method No.8 (vii)

(vii)   Determination of Lead -

Same as method No.8 (v), Substitute Zinc sulphate by ferrous sulphate.

14. Method of analysis of ammonium molybdate(NH4)6 Mo7O24.4H2O

(i)       Quality of Reagents -

Unless specified otherwise, pure chemicals and glass distilled or demineralised water shall be used in tests :

Note: ' Pure Chemical' means chemicals that do not contain impurities which affect the results of analysis. 'Demineralised Water' means the water obtained after passing distilled water through a cation and anion exchange resins or a combined cation-anion exchange resin.

(ii)      Determination of Molybdenum :

(A)     Atomic Absorption spectrophotometer method :

(a)      Reagents:

(1)     Potassium Sulphate - Dissolve 25 g of AR Potassium sulphate in 1 litre of distilled water.

(2)     Standard molybdenum solution - weigh 1.5 g of molybdenum trioxide (MoO3) and transfer it to one litre volumetric flask through the funnel giving several washing to beaker and funnel with glass distilled water. Make up the volume upto the mark. This is 1000 ppm standard molybdenum solution.

1.        Preparation of working standards - Pipette the following volume of 1000 ppm standard Mo solution in 100 ml numbered volumetric flasks. Add 20 ml of potassium sulphate solution to each flask and make up the volume to 100 ml. Stopper the flask and shake them well.

(b)      Procedure.

1.        Preparation of Ammonium Molybdate fertilizer sample: Weigh exactly 0.1 g of the material on the clean watch glass and transfer it to a 100 ml volumetric flask through funnel giving repeated washings and dissolve the material by shaking well. Make the volume upto the mark.

2.        Take 10 ml of the prepared solution in a 100 ml volumetric flask, add 20 ml of potassium sulphate solution and make the volume upto the mark.

3.        Flamming the solution : Flame the standards and the filtered samples on an atomic absorption spectrophotometer at a wavelength of 313.3 nm using nitrousoxide-acetylene flame.

Calculation : Prepare a standard curve of known concentration of molybdenum solution by plotting the absorbance value on Y-axis against their respective molybdenum concentration on X-axis.

Percent of Mo = X /10 W

Where X = Concentration of molybdenum (ppm)as obtained from the calibration curve.

W = Weight in g of the material taken for the test.

(B)     Colorimetric Method for Determination of Molybdenum.

(a)      Outline of the Method

Molybdenum (vi) in acid solution when treated with stannous chloride (best in the presence of a little ferrous ion) is onverted largely into molybdenum (v). This forms a complex with thiocyanate ion, probably largely Mo(SCN)5, which is red in colour. The latter may be extracted with solvents possessing donor oxygen atoms (3-Methylbutanol is preferred). The colour depends upon the acid concentration (optimum concentration 1 M) and the concentration of thiocyanate ion (<1.0 percent, but colour intensity is constant in the range 2-10 percent): it is little influenced by excess of stannous chloride. The molybdenum complex has maximum absorption at 465 nm.

(b)      Apparatus

(1)     Photometer - Any suitable photoelectric colorimeter.

(c)      Reagents

(1)     Standard molybdenum solution - (0.001 percent molybdenum)- weigh 0.184 of A.R. Ammonium molybdate (NH4)6.Mo7O24.4H2O on a clean watch glass and transfer it to one litre volumetric flask through the funnel giving several washings to watch glass and funnel with glass distilled water. Make the volume upto the mark. Pipette out 10 ml of this solution into 100 ml volumetric flask and make the volume up to the mark. This gives 0.001 percent Mo solution.

(2)     Ferrous Ammonium Sulphate - Dissolve 10 g of AR ferrous ammonium sulphate salt in 100 ml of very dilute H2SO4.

(3)     Stannous chloride solution - Dissolve 10 g of AR stannous chloride dihydrate in 100 ml of 1M - hydrochloride acid.

(4)     Potassium thiocyanate solution - Dissolve 10 g of AR potassium thiocyanate salt in 100 ml of distilled water.

(5)     Iso-amyl alcohol.

(d)      Preparation of Sample Weigh 0.1 g of sample on a clean watch glass and transfer it to one litre volumetric flask, through the funnel giving several washings to watch glass and funnel with glass distilled water. Make the volume up to the mark. Pipette out 5 ml of this solution into a 100 ml of volumetric flask and make up the volume up to the mark.

(e)      Procedure.

(1)     Place 1.0, 2.0, 3.0, 4.0 and 5.0 ml of the 0.001 percent molybdenum solution (containing 0.01 mg. 0.02 mg, 0.03 mg 0.04 mg and 0.05 mg molybdenum) severally in 50 ml capacity separating funnels and diluting each with an equal volume of water.

 

(2)     Add to each funnel 2.0 ml of conc. HCL, 1.0 ml of ammonium ferrous sulphate and 3.0 ml of the potassium thiocyanate solution.

 

(3)     Shake gently and then introduce 3.0 ml of the stannous chloride solution.

 

(4)     Add water to bring the total volume in each separating funnel to 25 ml and mix.

 

(5)     Pipette 10 ml of redistilled 3-methylbutanol (iso-amyl alcohol) into each funnel and shake individually for 30 seconds.

 

(6)     Allow the phases to separate and carefully run out the lower aqueous layer.

 

(7)     Remove the glass stopper and pour the alcoholic extract through small plug of purified glass wool in a small funnel and collect the organic extract in a 1.0 cm absorption cell.

 

(8)     Measure the absorbance at 465 nm in a spectrophotometer against a 3-methylbutanol blank.

 

(9)     Plot absorbance against concentration of standard molybdenum solutions and draw the calibration curve.

 

(10)   Take 10 ml of the sample solution and determine the absorbance of it by subjecting it to the same treatment as the standard solutions, using calibration curve, determine the corresponding concentration of molybdenum in the sample solution.

Calculation: % Mo = 2000.W /. Y.W.

Where X = Concentration of molybdenum (in mg ) of

the test solution.

Y = Volume of sample solution taken for the

test.

W = Wt in g of the material taken for the

preparation of the sample solution.

(Ref. : Vogal's Text Book of Quantitative analysis).

(iii)     Determination of matter insoluble in water

(a)      Procedure

Dissolve 25.0 g of the material in 125 ml of water. Filter through a weighed and prepared Gooch crucible or sintered glass crucible (G.No.4) and wash the residue thoroughly with water. Dry the crucible at 110 degree + 8 degree to constant mass.

(b)      Calculation :

Matter insoluble in water percent by weight = 4A

Where A = Weight in g of the residue.

(iv)    Determination of lead

Same as per method No.8(v). Substitute zinc sulphate by ammonium molybdate.

15. Method of Analysis of Chelated Zinc (As Zn-EDTA)

(i)       Reagents.

(a)      EDTA Solution - (0.05M) Dissolve 18.612 g of disodium

ethylene diamine tetra acetate dihydrate (EDTA) in

distilled water & make up the volume to 1 litre.

(b)      Standard Zinc solution (1000 ppm) - Weigh accurately

1.0 g of zinc metal in a beaker. Add 20 ml HCL (1:1).

Keep it for few hours and allow it to dissolve

completely. Transfer the solution to 1 litre

volumetric flask. Make the volume upto the mark.

(c)      Concentrated Ammonia solution (sp.gr.0.88)

(d)      Ammonium Nitrate - AR grade salt.

(e)      Buffer solution (pH-10) - Dissolve 8.0 g AR grade

ammonium nitrate in 65 ml of water and add 35 ml of

concentrated ammonia solution (sp.gr.-0.88)

(f)       Eriochrome black (T) indicator mixture - mix

thoroughly 1 gm of eriochrome Black (T) indicator with

100 gm of AR grade potassium nitrate.

(g)      Hydroxylamine hydrochloride - AR grade.

(h)     Potassium cyanide - AR grade (to be used with extreme

care) 15% aq. solution.

(i)       Manganese sulphate solution - Dissolve 11.15 g of AR

grade manganese sulphate in 1 litre of distilled water.

(j)       Sodium Fluoride AR grade.

(ii)      Preparation of Sample solution.

Weigh accurately 1.0 g of the sample and transfer it to 100 ml volumetric flask. Make up the volume with distilled water. Keep it overnight.

(iii)     Procedure

(a)      Standardization of EDTA solution

(1)     Take 10 ml of zinc solution (standard)

 

(2)     Dilute it by adding 30 ml distilled water.

 

(3)     Add 10 ml of buffer solution and 30-40 mg of indicator mixture.

 

(4)     Titrate with EDTA solution till clear blue end point is obtained. Note the volume of EDTA used s V1 ml.

(b)      Standardisation of Manganese sulphate solution.

(1)     Take 25 ml of manganese sulphate solution.

 

(2)     Dilute it by adding 100 ml distilled water.

 

(3)     Add 0.25 g of dydroxylamine hydrochloride and 10 ml of buffer solution.

 

(4)     Add 30-40 mg of indicator mixture.

 

(5)     Titrate with EDTA solution till clear blue end point is obtained. Note the volume of EDTA used as V2 ml.

(c)      Determination of EDTA content of Zn-EDTA fertilizer

(1)     Take 10 ml of sample of distilled water.

 

(2)     Dilute it by adding 100 ml of distilled water.

 

(3)     Add 0.25 g of hydroxylamine hydrochloride.

 

(4)     Add 10 ml of buffer solution and 30-40 mg of indicator mixture.

 

(5)     Warm to 40 deg.C. and titrate with standard EDTA solution (preferably stirring magnetically) to clear blue end point.

Note the volume of EDTA used as V3 ml.

(6)     After the end point, add 2.5 g of solution fluoride and stir for one minute.

(7)     Titrate the solution with standard mangenese sulphate solution, slowly, till a permanent red colour is obtained. Note the volume of manganese sulphate added as V4 ml.

(8)     Stir for 1 minute.

(9)     Titrate the excess of manganese ions with EDTA solution until the colour changes to pure blue.

Note the volume of EDTA used as V5 ml.

(10)   After the second end point (step 9) add 4-5 ml of 15% aqueous potassium cyanide solution.

(11)   Titrate it with manganese sulphate solution till colour changes sharply from blue to red.

Note:- The volume of manganese sulphate solution added as V6 ml.

Calculation: Molarity of EDTA solution (M1) =

Molarity of standard zinc solution x volume of

standard zinc solution taken.

Volume of standard manganese sulphate solution taken

Nos of millimoles of EDTA used in titrating Zn + other metals (A) = M1V3

No of millimoles of EDTA liberatedby sodium fluoride (B) = M2V4 - M1V5

Hence Nos of millimoles of EDTA used for titratingzinc (C) = A - B

But nos of millimoles of EDTA liberated by KCN (D) = M2V6

Hence no of millimoles of EDTA contained by Zn-EDTA sample = D - C

EDTA percent = 24.31 x B

Percent of free zinc = 65.38 x C

Percent of Zinc chelated with EDTA = 65.38 (D - C)

(Ref. Vogal's Text Book of Quantitive Inorganic Analysis).

16. Method of Analysis of Chelated Iron (As Fe-EDTA)

(i)       Quantity of reagents

Unless specified otherwise, pure chemicals and glass distilled or demineralised water shall be used in tests.

Note:- 'Pure Chemicals' means chemicals that do not contain impurities which affect the result of analysis. 'Demineralized Water' means the water obtained after passing distilled water through a cation and an anion exchange resins or a combined cation-anion exchange resin.

(ii)      Determination of chelated iron

(a)      Reagents.

(1)     Sodium hydroxide solution - 0.5N, Dissolve 20 g NaOH in water and dilute to 1 litre.

 

(2)     Disodium EDTA solution = 0.66%. Dissolve 0.73 g of Na2H2 EDTA 2H2O in water and dilute to 100 ml.

 

(3)     Iron standard solution -

(A)     Stock solution - (1000 ppm) Dissolve 1.000 g pure Fe wire in approximately 30 ml 6 N HCL withboiling. Dilute to 1 litre in a volumetric flask with distilled water.

 

(B)     Intermediate solution - (100 ppm). Pipette 10 ml iron stock solution and 10 ml Na2H2 EDTA solution in 100 ml volumetric flask and dilute to volume.

 

(C)     Working solution - Pipette the following volumes of 100 ppm intermediate solution in 50 ml numbered volumetric flask and make the volume with 0.5 N HCl.

(b)      Apparatus

Atomic Absorption Spectrophotometer with air/acetylene flame.

(c)      Procedure

(1)     Preparation of sample solution :

(A)     Weigh sample containing approximately 40 mg Fe into 200 ml tall form beaker.

 

(B)     Wet with 2-3 drops of alcohol and dissolve in 100 ml of water.

 

(C)     Add 4 drops of 30% H2O2, mix and adjust pH of solution to 8.5 with 0.5 N NaOH. If pH drifts above 8.8, discard solution and repeat analysis.

 

(D)     Transfer solution to 200 ml volumetric flask, dilute to volume with water and mix.

 

(E)     Filter solution through quantitative paper.

 

(F)      Pipette 10 ml filtrate into 200 ml volumetric flask and dilute to volume with 0.5 N HCl.

(2)     Flaming the Solution

Flame the standard and the sample solution on atomic absorption spectrophotometer at a wavelength of 248.3 nm using air acetylene flame. In same manner determine Fe blank on all reagents used.

Calculation:- Prepare a standard curve of known concentration of Fe solution by plotting the absorbance value on Y axis against their respective Fe concentrations on X axis.

Chelated Iron % = ( ppm Fe in sample---- ppm Fe in blank) x 0.4 / g sample

( Ref. Method of Analysis AOAC, 1984)

(iii)     Determination of pH

As per method No. 8(vi) (a)

17. Determination of Sodium in Potassium Chloride and Potassium Sulphate by Atomic Absorption Spectro-photometric method.

(i)       Quantity of Reagents - Unless Specified otherwise, pure chemicals and glass distilled or demineralised water shall be used in tests.

(ii)      Reagents.

(1)     Ammonium Oxalate Solution - Dissolve 40 g of Ammonium Oxalate in 1 litre of distilled water.

 

(2)     Standard Sodium Solution - (1000 ppm) - Weigh accurately 2.5421 g of dried NaCl on a clean watch glass and transfer it to one litre volumetric flask. Make up the volume upto the mark. Stopper the flask and shake the solution well. This is 1000 ppm sodium solution.

 

(3)     Preparation of working standard - Pipette the following volumes of 1000 ppm standard sodium solution in 100 ml volumetric flask and make up the volume with glass distilled water.

Stopper the flask and shake the solution well

(iii)     Procedure.

(1)     Preparation of sample solution - weigh exactly 2.5 grams sample on a clean watch glass and transfer it to 250 ml volumetric flask through the funnel giving repeated washings with glass distilled water (about 125 ml. of water should be used). Add 50 ml of Ammonium Oxalate solution. Boil for 30 minutes, cool, dilute to volume, mix and pass through dry filter paper (Whatman No.1 of equivalent).

(2)     Flaming the solution - Flame the standard and the filtered sample on Atomic Absorption Spectro-photometer at a wavelength of 330.3 nm using clean air acetylene flame.

Calculations : Prepare a standard curve of known concentrations of Sodium solution by plotting the absorbance value on Y-axis against their respective sodium concentration on X-axis. Determine the concentration of sodium in the sample solution from the graph. Sodium (Na) as Sodium Chloride % = 0.0254 X, where X is the concentration of Sodium in ppm obtained from the standard curve. (Ref. : AOAC, 1984)

18 Determination of Total Chlorides in Potassium Sulphate by Silver Nitrate Volumetric Method.

(i)       Reagents.

(1)     Standard Silver Nitrate (AgNO3) solution - 0.1 N

(2)     Potassium Chromate (K2CrO4) Indicator solution - 5 percent.

(ii)      Procedure

(1)     Weigh accurately about 10 gms of the prepared sample and transfer into 500 ml beaker.

 

(2)     Add about 250 ml of water and warm gently for about 20 minutes.

 

(3)     Cool and dilute the solution to 500 ml in a volumetric flask

 

(4)     Allow to stand to let any insoluble matter settle.

 

(5)     Transfer with a pipette 100 ml of the clear solution into a conical flask.

 

(6)     Titrate with standard AgNO3 solution (0.1 N) using 1 ml of Potassium Chromate Indicator solution.

Calculation : Total Chlorides ( as Cl ), percent by

Weight ( on dry basis ) = 17.73 N V / W

Where, N = Normality of standard AgNo3 solution.

19. Methods of Analysis of Magnesium Sulphate

(i)       Quality of Reagents.

Unless specified otherwise, pure chemicals and glass distilled or demineralised water shall be used in testa.

(ii)      Determination of Magnesium.

(A)     Atomic Absorption Spectrophotometer method

(a)      Reagents.

(1)     Hydrochloric Acid 0.5 N.

 

(2)     Magnesium Standard Solution : Dissolve 1.013 g Magnesium Sulphate (MgSO47H2O) in 0.5 N hydrochloric acid solution and dilute to 100 ml with this acid in a volumetric flask. This is 1000 ppm magnesium stock solution.

 

(3)     Strontium Chloride Solution : Dissolve 15 g strontium chloride (SrCl26H2O) in 0.5 N hydrochloric acid and dilute to 100 ml with the same solvent.

(b)      Preparation of working standards.

(1)     Pipette 8.1 ml of 1000 ppm magnesium stock solution to 100 ml capacity volumetric flask and make up the volume with 0.5 N hydrochloric acid. This is 10 ppm Magnesium Solution.

(2)     Pipette the following volume of 10 ppm magnesium solution in 100 ml numbered volumetric flask. Add 10 ml of strontium chloride solution to each flask and make up the volume to 100 ml with 0.5 N hydrochloric acid.

(c)      Procedure.

(1)     Preparation of sample solution.

(A)     Weight 1 g of the sample and place in a 500 ml volumetric flask. Add about 300 ml water and boil for 30 minutes. Allow to cool, dilute to the mark with water, mix and filter.

 

(B)     Pipette 5 ml of the filtrate (A) into a 100 ml volumetric flask, make up to the mark with water and mix.

 

(C)     Transfer by pipette 5 ml of the diluted filtrate (B) into 100 ml volumetric flask and make up to the mark with 0.5 N HCl.

(2)     Blank solution : Prepare a blank solution from which only the sample has been omitted.

(3)     Flaming of solution : Flame the standard and sample solutions on Atomic Absorption Spectrophotometer at wavelength of 205.2 nm using Air Acetylene flame.

Calculations: Plot the calibration curve using the mean absorbances on Y-axis and the corresponding concentrations of Magnesium (ppm) on X-axis. Determine the concentration of Magnesium in the sample by reference to the calibration curve.

Magnesium percent = 20X

Where X = concentration of Magnesium (in ppm) obtained from the standard curve.

(B)     Titrametric method (EDTA Titrations)

(Applicable to the samples which do not contain phosphate as impurity)

(a)      Reagents

(1)     Buffer solution (pH-10.0) - Dissolve 67.5 g ammonium chloride in 200 ml of distilled water, add 570 ml ammonia solution and dilute to 1 litre.

 

(2)     Potassium hydroxide - Potassium cyanide solution - Dissolve 280 g potassium hydroxide and 66 g potassium cyanide in 1 litre of distilled water.

 

(3)     Potassium cyanide solution (2%) - Dissolve 2 g potassium cyanide in 100 ml of distilled water.

 

(4)     Eriochrome black T indicator solution - Dissolve 0.2 g of indicator in 50 ml of methyl alcohol containing 2 g of hydroxylamine hydrochloride.

 

(5)     Calcium standard solution (1 mg/ml) - Dissolve 2.4973 g calcium carbonate, primary standard grade, previously dried for 2 hours at 2850. in HCl (1+10). Dilute to 1 litre with distilled water.

 

(6)     Calcein indicator mixture - Grind together 1 g calcein indicator (2',7'-bis(bis(Carboxymethyl,) amino)methyl-) fluorescein, sodium derivative sodium salt), 10 g charcoal 100 g potassium chloride.

 

(7)     Disodium dihydrogen ethylene diamine tetra acetic acid standard solution (0.4% - Dissolve 4 g Na2H2-EDTA in 1 litre of distilled water.

 

(8)     Triethanolamine (1 + 1)

 

(9)     Potassium ferrocyanide solution (4%) - Dissolve 4 g potassium ferrocyanide in 100 ml of distilled water.

(b)      Standardization of Calcium Solution :

(1)     Pipette 10 ml calcium standard solution into 250 ml erlenamayer flask.

 

(2)     Add 100 ml of distilled water, 10 ml KOH-KCN solution, 2 drops of triethanolamine solution, 5 drops of potassium ferrocyanide solution and 15+1 mg of calcein indicator.

 

(3)     Immediately place the flask on a magnetic stirrer in front of daylight fluorescent light with transparent background.

 

(4)     While stirring, titrate with EDTA solution to disappearence of all fluorescent green and until solution remains pink. Titrate more than 3 aliquots. From average, calculate calcium titer value.

Calcium Titer (mg/ml) = Volume of calcium standard  (ml) / Volume of EDTA solution used (ml)

From calcium titer, calculate magnesium titer value as follows :

Magnesium titer = Calcium titer x 0.6064

(c)      Preparation of sample solution

(1)     Weight 1 g magnesium sulphate fertilizer sample into 250 ml volumetric flask.

 

(2)     Add 200 ml of distilled water and boil for 30 minutes.

 

(3)     Cool dilute to volume with water and mix.

(d)      Procedure.

(1)     Titration for Ca + Mg

(A)     Pipette 25 ml of aliquot in 250 ml erlenmayer flask.

 

(B)     Dilute with 100 ml of distilled water.

 

(C)     Add 5 ml of buffer solution (pH 10), 2ml potassium cyanide solution, 2 drops of triethapolamine solution, 5 drops of potassium ferrocyanide solution and 8 drops of eriochrome black T indicator solution.

 

(D)     Titrate immediately with EDTA solution, stirring and lighting as in standardisation. Colour changes are wine, red, purple, dark blue, to clear blue end point, becoming green if over titrated.

Note:- The volume of EDTA used as V1 ml.

(2)     Titration for Calcium.

(A)     Pipette 25 ml of aliquot in 250 ml erlenmayer flask.

 

(B)     Dilute with 100 ml of water.

 

(C)     Add 10 ml KOH-KCN solution, 2 drops of triethanolamine solution, 5 drops of potassium ferrocyanide solution and 15+ mg. of calcein indicator.

 

(D)     Titrate immediately with EDTA solution in Standardisation.

Note:- The volume of EDTA used as V2 ml.

Calculation:- Magnesium percent = (V1-V2) x MKg Titer EDTA

(Reference : AOAC, 14th edition, 1984)

20. Determination of Particle size in different Fertilizers

(i)       Apparatus :

(A)     Indian Standard of 20 cms. diameter and 5 cms in height with lid and bottom pan of required sizes.

 

(B)     Sieve shaker or vibrator with automatic timer and variable cycle control.

 

(C)     Balance, top leading with suitable capacity and sensitivity of 0.1 gm.

 

(D)     Weighing pan round suitable for holding sample and approximately 23 cms in diameter.

 

(E)     Brush either soft, fine wire or stiff.

(ii)      Procedure :

(A)     Take the sieve of required sizes and stack them in progressive order. The biggest sieve size should be on the top and the smallest in the bottom. Place the empty pan at the bottom.

 

(B)     Put 200 gms of ungrinded sample on the top sieve and place lid on the top of the stack.

 

(C)     Position and secure sieve stack in shaking apparatus.

 

(D)     Start shaking action for 5 minutes. If automatic timer is used, set timer for 5 minutes. If vibrator is used, also set vibrator control at 3000 cycle per minute.

Note:- If mechanical sieve shaker is not available, use hand sieving. Conduct sieving by appropriate lateral and vertical motions accompanied by jarring action. Continue until no appreciable change is noted in sieve fractions.

(E)     After completion of shaking time, transfer material from each sieve to weighing pan with brush and weight to +/- 0.1 gm.

(F)      Record weight from each sieve (sum of weights from each sieve should agree closely with original sample weight)

Calculations:- Percent weight on sieve = Weight on sieve (gm) /Total weight of sample (gm)

21. Method Of Analysis of Calcium nitrate

(i)       Determination of total nitrogen

By the as specified in 3 (viii)

(ii)      Determination of Ammonical Nitrogen

By the method as specified in 3 (vii)

(iii)     Determination of nitrate

By the method as specified in 3(viii) & vii)

(iv)    Determination of water insoluble matter

By the method of specified in 8(vii)

(v)      Determination of water soluble calcium.

A.        Titrimetric method (EDTA) Titrations.

(a)      Reagents.

(i)       Buffer solution (pH-12.0) - Dissolve 225 gm KOH (AR) in 250 ml water. Add 15 ml triethanolamite and make volume to one litre after cooling the solution.

 

(ii)      Pattan and Reeder's indicator 0.2 gm indicator in 100ml methanol.

 

(iii)     calcium standard solution (mg/ml). - Dissolve 2.4973g calcium carbonate, primary standard grade, previously dried for 2 hours at 2850 c, in Hcl (1 + 10). Dilute to 1 litre with distilled water.

 

(iv)    Disodium dihydrogent ethylene diamine tetra acetic standard solution (0.01 m) - Dissolve 3.7224 gm Na₂H₂-EDTA(AR) previously dried at 105 to 110° c for 1 hr in distilled water and make volume to one litre.

(b)      standardisation of calcium Solution

(i)       Pipette 10m1 calcium standard solution into 250 ml erleninayer flask.

 

(ii)      Add 10-15 ml distilled water and 20 ml Duffer solution [153][in case of Potassium Magnesium Calcium Sulphate add 50 ml distilled water and 20 ml buffer solution].

 

(iii)     Add few drops of indicator's solution. A red rose colour will appear.

 

(iv)    Titrate with EDTA till a blue colour is obtained. Note the volume of EDTA used as V₁ ml Calcium Titer (mg/m1) = Volume of Calcium standard solution (m1)/Volume of EDTA solution use (m1) (v1)

(c)      preparation of sample solution..

(i) weigh 2.5 g calcium nitrate fertiliser sample into 250 Volumetric Flask

(ii) make up the volume with distilled water. shake well.

[154][(iii) In case of Potassium Magnesium Calcium Sulphate "weighed 2.5 gm of fresh sample in 250 ml volumetric flask and add 5 ml concentrated HCl, make up the volume and shake well;]

(d)      Procedure.

(i)       pipette 5 ml of aliquot in 250 ml erlenmayer flask.

 

(ii)      Add 10-15 ml distilled water & 20 ml Buffer solution.

 

(iii)     Add few drops of indicator's solution. A red rose colour will appear.

 

(iv)    Titrate with EDTA till a blue colour is obtained. 

Note the volume of EDTA used as v2 ml

calculation

Calcium per cent = V2 x Calcium Titer x 2

B.        Atomic Absorption spectrophotometric method-

(1)     Reagent:

Unless specified otherwise pure chemicals and Glass distilled or demineralised water shall be used in test.

(a)      Hydrochloric Acid r= 3 N

(b)      preparation of stock solution:-

(i)       Calcium stock solution - Dissolve 2.498 gram CaCO₃ in a minimum amount of 3 N Hcl . Dilute to 1 litre (1000 ppm Ca). Dilute 10 ml to 100 ml. This is 100 ppm stock solution.

(ii)      Lanthanum stock solution:- 50 g La/L.

Dissolve 58.65 gram La₂O₃ in 250 ml Hcl, adding acid slowly. Dilute to 1 litre.

(c)      Preparation of working standard: 

Add 0, 5, 10, 15 and 20 ml of ca stock solution in a 100 ml volumetric flask. Add 20 ml La stock solution and make up the volume to 100 ml with distilled water, This will correspond to 0, 5, 10, 15, and 20 Mg Ca/m1 containing 1% La.

(2)     procedures:

weigh 1.00 gram well grind sample in a 100 ml volumeric flask. Add 25 ml water and shake to dissolve. Then add 20 Lanthanum solution in the flask and make volume to 100 ml with Distilled water. shake well and allow to settle. Filter, if required, before it is aspirated.

(3)     Flaming of the solution:- Flame the standard and sample solution on AAS at wave length of 422.7 nm using Air - Acetylene flame.

(4)     Calculation ;- plot the calibration curve using the mean absorbance on Y axis and the corresponding concentration of ca (ug/m1) at 'X'' axis. Determine the concentration of calcium in the sample by reference to the calibration curve:

% Ca = Concentration (ug/ml) x 10-2

22. Analysis of Micronutrient Fertilisers Mixtures by Atomic Absorption Spectro photometric Method-

(a)      Reagents :

(1)     Acidified water : Dissolve 10 ml of 10% Sulphuric Acid in 10 litre of double distilled water and adjust the pH to 2.5 ( ±0.5) with help of a pH meter using H₂SO₄ or NaOH.

 

(2)     Strontium Chloride Solution : Dissolve 7.5 g of Strontium Chloride (SrC12.6H20) in one litre of distilled water.

 

(3)     Potassium Sulphate Solution : Dissolve 25 gm of AR Potassium Sulphate in one litre of distilled water.

(b)      Procedure:

(i)       Preparation of standard stock solution :

Dissolve the specific quantity of standard material for specific element with the help of suitable solvent as indicated below and make up the volume 1000 ml with distilled water. Further dilute it to suitable flaming range with acidified water in case of Fe, Cu, Mn and Zn. In case of Mg, add 20 ml of Strontium Chloride and in case of Mo, add 20 ml of Potassium Sulphate before make up the volume up to the mark, in 100 ml volumetric flask with acidified water.

(ii)      Preparation of sample solution -

Weigh 1 gm micronutrient fertilizer mixture (Solid or liquid) transfer to 100 ml volumetric flask with the help of acidified water and make up the volume up to the mark. Shake well and keep it stand for at least 4-6 ;hours. Dilute it further to suitable standard working range with acidified water in case of Fe, Cu Mn and Zn. In case of Mg, add 20 ml of Strontium Chloride and in case of Mo, add 20 nil of Potassium Sulphate before making up the volume up to the mark, in 100 ml volumetric flask with acidified water.

(iii)     Flaming of Solutions :

Flame the standard solution of specific element at concentration mode. Then flame the sample solution to observe the concentration (in ppm). of specified element.

Calculation : % Concentration = X x Dilution Factor x 10-4

(X = Concentration in ppm observed by instrument)

23. Determination of Boron in Micronutrient Fertiliser Mixture-Volumetric Method-

(a)      Reagents-

(1)     Mannitol

 

(2)     Bismuth Nitrate Solution : Dissolve 22 gm of Bismuth Nittate [(BiNO3)3 5 H2O] in 8 ml of conch Nitric Acid Warm slightly and dilute to 100 ml with distilled water.

 

(3)     Nitric Acid :- Concentrated AR Grade.

 

(4)     Dilute Nitric Acid :- (1:20)

 

(5)     Sodium Hydroxide Solution :- 109% M/V

 

(6)     Sodium Hydroxide Solution - 0.02 M

 

(7)     Bromothymol Blue Indicator Solutions.

(b)      Procedure :

(1)     Weigh accurately 2.5 gm of prepared sample in to 250 ml beaker.

 

(2)     Add 2 ml of conc. Nitric Acid and 50 ml of water and warm gently and dilute to 100 ml with water.

 

(3)     Warm the solution (but do not boil).

 

(4)     Slowly add 5 ml of Bismuth Nitrate Solution for each 1% of P205 percent in the sample, from a burette with continuous stiffing and maintaining. the liquid hot during addition.

 

(5)     Cool and transfer the contents in to 250 ml volumetric flask and dilute up to the mark with distilled water.

 

(6)     Allow precipitate to settle and dilute up to the mark with distilled Water.

 

(7)     Filter through a dry filter paper (No. 40) rejecting the first few drops in to a beaker.

 

(8)     Pipette 100 ml of the filtrate in 250 ml beaker, add a few drops of indicator solution.

 

(9)     Add few drops of 10% NaOH solution with thorough stirring until the indicator turns blue.

 

(10)   Filter through a dry filter paper (No. 40) into 250 ml beaker and carefully wash the residue several times with cold water. The total volume should be 150 to 200 ml.

 

(11)   Adjust the pH to about 5 by adding diluted HNO₃ . Warm to about 90°C (do. not boil), and stir vigorously to avoid CO2. Cool the solution.

 

(12)   Place in the "solution, the electrodes of pH meter and adjust the pH to exactly 6.3 using NaOH solution.

 

(13)   Add 10 gm of mannitol and again adjust pH to exactly 6.3 with 0.02 N NaOH solution.

 

(14)   Continue adding mannitol in 10 gm portion till pH remains constant at 6.3. Note the total volume of 0.02 N NaOH used for the addition of Mannitol (Step 13).

 

(15)   Carry out a blank determination on fertilizers mixture to which Borate is not added.

(c)      Calculation :

% B = (A-B) x 0.05405/W

Where : A = Volume of 0.02 N NaOH solution used in the sample. 

B = Volume of 0.02 N NaOH solution used in the blank.

Note : In case phosphate is not present in the sample, proceed as follows:-

(i)       Take 2.5 gm of the sample in 250 ml volumetric flask and make up the volume with distilled water.

proceed as given from step (8) onwards.

24. Determination of total sulphur

(The total sulphur includes sum of sulphur present in Sulphate and elemental form).

(A)     Determination of Sulphate Sulphur

Method of determination of sulphur present in the sulphate form in various fertilizers for nitrate free and nitrate containing samples is given below:

Classification of procedures-

Procedure (a) : For nitrate free samples such as ammonium sulphate, potassium sulphate, zinc sulphate , copper sulphate, ferrous sulphate, manganese sulphate , N.P. and NPK complexes and mixtures, 

Procedure (b): Super phosphate

Procedure (c) : For nitrate containing fertilizers such as ammonium phosphate sulphate nitrate 20 :20 :0

(i)       Quality of Reagents-

Unless specified otherwise, pure chemicals, glass, distilled or demineralised water shall he used in tests.

Note :- (1) " pure chemicals" means chemicals which do not contain impurities which affect the results of analysis.

(2) " demineralised water" means water obtained by water passing through a cation and anion exchange resins er a combined cation-anion exchange resins.

(ii)      Reagents-

(1)     Hydrochloric acid-concentrated

 

(2)     Dilute hydrochloric acid - Dilute 250 ml. of concentrated hydrochloric acid to 1000 ml, of water.

 

(3)     Barium chloride solution - 2 percent . Dissolve 20 g of barium chloride in 1000 ml of water.

 

(4)     Silver nitrate solution - 5 percent . Dissolve 5 g silver nitrate in 100 ml water.

(iii)     Procedure (a)-

(1)     Weigh about 2.5 g of sample and transfer to 250 ml capacity volumetric flask with the help of dilute hydrochloric acid.

 

(2)     Make up the volume with dilute hydrochloric acid.

 

(3)     Apply stopper, shake well and filter through Whatman Filter paper No.40 or equivalent part in a dry beaker if the solution is not clear and transparent.

 

(4)     Take 25 ml of the filtered aliquot in a beaker of 250 ml capacity. Add 100 ml of water and heat to boil. While stirring add in a slow stream.1 ml of hot barium Chloride solution for each one percent. Sulphur expected in sample plus additional 10 ml in excess to ensure complete precipitation of sulphur as barium sulphate. Boil for a minute.

 

(5)     Digest the precipitate on a hot plate or water bath for 2 hours at low temperature such that the solution does not boil. Ensure the supernatent liquid to be clear and transparent. Cool to room temperature. Filter into a 30 ml capacity G 4 grade - sintered Gooch crucible previously dried at. 250° C cooled and weighed. - Wash the precipitate 10-12 times with hot water to ensure the precipitate to make it free from barium chloride. The filtrate may be tested with silver nitrate solution to confirm that the precipitate is free from chloride.

 

(6)     Dry the crucible and its content to 250 C for two hours in a furnace by raising the temperature of the furnace slowly from room temperature: After drying, cool to room temperature in a desiccator to a constant weight taken.

Calculations: Sulphate Sulphur (as S) per cent by weight - 137.4 x M

Where M = weight of precipitate

W weight of the sample taken.

Procedure (b): Weigh about 2.5 g of sample and transfer to a beaker of 250 ml capacity. Add 25 ml of concentrated hydrochloric acid and 25 ml of water. Heat to boil the solution gently. Boil for 5 minutes and cool. Add 75 ml of water and transfer quantitatively into a volumetric flask of capacity 250 ml with dilute hydrochloric acid solution and make up the volume. Apply stopper, shake well and filter about 50 ml or prepared solution through Whatman filter paper No.40 or equivalent and proceed as at step (2) of Procedure (a) onward.

Procedure (c): (1) Weigh about 2.5 g of sample and transfer to a beaker of 250 ml capacity. Add 10 ml of concentrated hydrochloric acid and grind the sample with the help of a glass rod. Evaporate to dryness on a hot plate Soak the mass again with few drops of concentrated hydrochloric acid and evaporate to dryness.

(2) Add 100 ml of dilute hydrochloric acid, heat to boil and cool to room temperature. Transfer the content to a 250 ml volumetric flask. Filter a portion of the solution through a Whatman No.40 filter paper or equivalent and proceed as at step (2) of Procedure (a) onwards. 

Note: Based on AOAC 1995.

(B)     Determination of elemental Sulphur

(a)      Reagents.

(1)     Hydrochloric Acid- concentrated(4 N)

 

(2)     Sulphur powder (AR Grade)

 

(3)     Acetone saturated with sulphur- Add 2-3 g of sulphur powder in 250 ml of acetone in stoppered bottle. Shake well and allow it to stand for 1 hour. Filter through whatman filter paper No.42 & collect , filtrate in a stoppered glass bottle.

 

(4)     Carbon di sulphide (AR Grade)

(b)      Procedure.

Take 1 g of prepared sample in a beaker. Add 50 ml of 4 N 1-ICI boil for 5 minutes. Cool and filter through a sintered glass crucible (G 4). Wash thoroughly with distilled water. Wash the residue 5-6 times with 10 ml portion of Acetone saturated with sulphur. Dry at 100°C for 1 hour. Cool in a desiccator and take weight of the crucible. Let the weight be W.

After taking the weight of the crucible (WO wash the crucible 8-10 times with 10 ml portion of carbon disulphide thoroughly under slow suction. Dry the crucible at 100° C for 1 hour. Cool in a desicator and weigh. Let this weight be W2.

Calculation:- Elemental sulphur as (S) % by weight = (W₁- W₂) X 100/W

Where "W" is the weight of the sample taken

(C)     Total sulphur(as 5) per cent by weight = Sulphate sulphur (as per procedure 24)+ elemental Sulphur (as per procedure 24 A).

26. Method of analysis of Zincated Oxide (suspension) :-

[155][(i) Determination of total zinc

Scope: Total extraction of Zinc (Zn), Arsenic (As), Lead (Pb) and Cadmium (Cd) from Zinc Oxide Suspension Concentrate.

Principle: Zinc and heavy metal impurities are extracted from the sample with boiling Aqua Regia.

(a)      Sample preparation:

The details of the procedure for drawl of samples of fertilizers have been provided in Schedule II Part A, Serial No. 9 (Method for sampling of liquid fertilizers (other than anhydrous ammonia), however importance of proper shaking and mixing of contents before withdrawal of sample and before drawing aliquot for analysis is particularly emphasized. Since in suspension formulation insoluble materials might settle down over time, thorough mixing of contents would ensure representative composition along the entire depth of the container.

(b)      Reagents:

All the reagents should be of analytical grade to ensure negligible concentration of the elements to be determined.

(1)     Glass double distilled water (free from micronutrients)

(2)     Hydrochloric acid 37% HCI ((HCI) = 12 mol/l, p = 1.18 g/ml)

(3)     Nitric acid 65% HNO₃   {c(HNO3) = 14.3 mol/l, p = 1.4 g/ml}

(c)      Appartatus:

Apparatus for thermal heating digestion-with reaction vessel and reflux condenser.

The vessel should be at least 5 times the volume of the aqua regia used.

In case reaction vessel with reflux condenser is not available, Erlenmeyer flask or high beakers covered with watch glass can be used for the purpose.

Ash free filter paper is required if filtration is necessary.

(d)      Procedure:

(1)     Weight one gram (1 ± 0.001 g) of the sample and transfer quantitatively to the reaction vessel.

 

(2)     Moisten the sample with about 0.5 to 1.0 ml distilled water

 

(3)     Mix the contents well and 21 ml of HCL) followed by 7 ml of HNO3 (reagent both drop wise to reduce foaming.

 

(4)     Connect the condenser to the reaction vessel and let the mixture stand at laboratory room temperature until effervescence ceases.

 

(5)     Turn on the heating device and slowly raise the temperature of the reaction mixture to reflux condition. Maintain for 2 hours.

 

(6)     Ensure that the condensation zone is lower than half of the height of the condenser.

 

(7)     After 2 hours of reflux, allow to cool and rinse the condenser with 10 ml of distilled water.

 

(8)     Transfer the contents quantitatively into a 500 ml volumetric flask and dilute to the mark with water. The test solution corresponds to a 500 times dilution of the sample.

 

(9)     Test solution can be filtered, if necessary (should not be required for Zinc Oxide Suspension concentrate). If filtered, discard the first 20 ml (approx) portion for analysis.

(10)   Prepare a blank test solution following the same procedure as the sample. This is to be used for background correction of analysis, in case of any possible contamination through reagents.

 

(11)   Measurement can be carried out immediately, or can be stored in tightly closed plastic vessels for up to 15 day.

Note:-Addition of one drop of octanol to the reaction vessel can be used as an antifoaming agent.

(e)      Determination of Zinc in the extracted material:

Process for analysis of Zinc shall be as per the procedure specified at Method no. 7 (iii) (b) (2) step (B) onwards or method No. 8 (ii) (b) step (2) onward.

Note:-Calculation need to be adjusted accordingly, in view of extent of dilution of original sample.]

(ii) Determination of lead

By the method as specified in 8 (v) [156][specified in 8(v) after extraction thorugh aqua regia as specified in sub-item (d) of item (i)]

(iii) Determination of specific gravity

By the method as specified in 21

[157][(iv) For determination of Arsenic

By the method specified as 8 (ix) after extraction thorugh aqua regia as specified in sub-item (d) of item (i).

(v) For determination through Cadmium

By the method specified as 8 (x) after extraction thorugh aqua regia as specified in sub-item (d) of item (i).]

27. Determination of Boron in Colemanite :-

(a)      Reagents:-

(1)     Mannitol

 

(2)     Bismuth nitrate solution: Dissolve 22g of bismuth nitrate {(BiNO3)3.5H20} in 8 ml of conc. Nitric acid. Warm slightly and dilute to 100 ml with distilled water.

 

(3)     Nitric acid - Concentrated AR grade.

 

(4)     Dilute nitric acid - (1:20).

 

(5)     Sodium hydroxide solution - 10% MN.

 

(6)     Sodium hydroxide solution - 0.5M.

 

(7)     Bromothymol blue indicator solutions.

(b)      Procedure:-

(i)       Weigh accurately 2.5g of sample into 250 ml of beaker.

 

(ii)      Add 5m1 of concentrated Nitric acid and 50 ml of water, warm gently and dilute to 100 ml cool and transfer the contents into 250 ml volumetric flask and dilute to the mark with distilled water.

 

(iii)     Filter through a dry filter paper Whatman No.40 rejecting the first few drops into a beaker.

 

(iv)    Pipette 100 ml of the filtrate into 250 ml beaker, add a few drops of indicator solution.

 

(v)      Add few drops of 10% NaOH solution with thorough stirring until the indicator turns blue.

 

(vi)    Filter through a dry filter paper into 250 ml beaker and carefully wash the residue several times with cold water. The total volume should be 150¬200 ml.

 

(vii)   Adjust the pH to about 5 by adding dilute nitric acid. Warm to about 90° C (do not boil) and stir vigorously to avoid carbon dioxide. Cool the solution.

 

(viii)  Adjust the pH to exactly 6.3 using NaOH solution.

 

(ix)    Add 10g of mannitol and again adjust pH to exactly 6.3 with 0.5 NaOH solution.

 

(x)      Continue adding mannitol in 10g portion till pH remains constant at 6.3. Note the total volume 0.5 NaOH use for the first addition of mannitol.

 

(xi)    Carry out a blank determination to which borate is not added.

(c)      Calculation:

Percentage boron = (A-B) x 1.3512/W

Where A is the volume of 0.5 N NaOH solution used in the sample

B is the volume of 0.5 N NaOH solution used in the blank.

28. Method of Analysis of Customized and Fortified Fertilizers:-

(i)       Determination of nitrogen by method 3 (iv) or 3 (v).

 

(ii)      Determination of ammoniacal nitrogen by method 3 (vii).

 

(iii)     Determination of neutral ammonium citrate soluble phosphate by method 4 (v).

 

(iv)    Determination of water soluble phosphate by method 4 (iii).

 

(v)      Determination of water soluble potash by method 5 (i).

 

(vi)    Determination of sulphur by method 24.

 

(vii)   Determination of micronutrients in Customized or Fortified Fertilisers.

(a)      Sample Preparation:-

1.        Weigh accurately 2.5g sample into a 250 ml beaker. Add 50 ml of 1+1 HCI and cover with a glass.

 

2.        Heat to boiling and continue to boil until volume is reduced to about 25 ml.

 

3.        Dilute to about 100 ml with water and bring to boil.

 

4.        Cool, transfer to a 500 ml volumetric flask and dilute to volume with water.

 

5.        Mix thoroughly and allow to stand until a clear solution is obtained or filter a portion through a dry whatman No.40 filter paper.

 

6.        Transfer 25 ml aliquot to 250 ml volumetric flask, dilute to volume and mix thoroughly.

 

7.        Dilute it further to suitable standard working range with acidified water.

 

8.        Prepare a blank solution in the same manner, omitting the sample.

(b)      Preparation of Standard Stock Solution, working standards and Determination:

As given in Method 22 A

(c)      Determination of Boron-Method 23

29.Determination of Plant Available Silicon (Si(OH)4)

CaCl2 extraction of Silicon fertilizer amendment

Analysis with UV

(a)      Reagents: Do not store any reagent in glass containers, and do not expose to glassware any longer than absolutely necessary while making up reagents. e.g. dissolve reagent/prepare solution in plastic beaker with slightly less than the final volume of solvent, and use volumetric glassware only for a short interval at the very end to make up to volume.

1.        Extractant 0.01 M CaCl2: Dissolve 7.35 g CaCl2.2H2O in de-ionised water, and make up to 5L.

 

2.        Tartaric Acid: Dissolve 100 g of tartaric acid and make up to 500 ml with deionized water. Store in polyethylene bottle. Make up fresh solution when appreciable sediment forms. Store in refrigerator.

 

3.        ANSA reducing agent: Dissolve 25 g of sodium bisulphite (NaHSO3) in 200 ml water, and combine with a solution containing 2 g of anhydrous sodium sulfite (Na2SO3) and 0.4 g of 1-amino-2-napthol-4- sulfonic acid in 25 ml of water. Dilute the combined solution to 250 ml and store in a polyethylene bottle in fridge. Discard if solution darkens in colour.

 

4.        Ammonium paramolybdate tetrahydrate: Dissolve 54 g ammonium molybdate (see note 2) in about 800 ml deionised water in a plastic beaker. Adjust pH to 7 with 5 N NaOH or 0.5 M H₂SO₄ depending on whether the pH needs to be raised or lowered. Make up to 1 L, and store in polyethylene bottle in refrigerator.

 

5.        0.5M Sulfuric Acid: 56 ml of conc. sulfuric acid (from plastic bottle) in 2 L deionised water.

 

6.        5NNaOH: 20 g of NaOH pellets in 100 ml of deionised water (Make and store in plastic container.

(b)      Standards:

A minimum of 5 calibration standards must be prepared; covering the core range from 0 to 5.0 mg/L. Higher standards may be included. Suggested standards are: Si Primary standard - 1000 mg/L Si. Commercial Si standard solution is used.

Si Secondary standard - 50 mg/L Si: Dilute 50 ml primary standard to 1 L with deionised water. Store in tightly stoppered polyethylene bottle.

Working standards: Prepare 0, 0.5, 1, 2, 3, 4, 5, and 6 mg/L Si standards equivalent to 0, 5, 10, 20, 30, 40, 50, 60mg/kg in the Silicon Fertiliser. Add 0, 0.5, 1 ,2 ,3 ,4, 5,and 6ml of secondary standard to separate 50 ml volumetric flasks and make up to volume with 0.01 M CaCl2.

0.01 M CaCl2 is the 0 standard.

Method: 1. Dry approximately 2-3 grams of Silicon fertiliser in a 1050C oven overnight. Grind the sample if not already in powder form.

2. Weigh 0.4 g of dried Silicon fertiliser into a 70 ml container, and add 40 ml 0.01 M CaCl2. Lid, and shake in an end over end shaker overnight (16 hours). Centrifuge sample extract at 2000 rpm for 10 minutes. The extract should be clear.

3. Transfer 1 ml of filtrate into a 20 ml capacity test tube (See note 4)

4. Add 2.5ml of 0.5M sulfuric acid

5. Add 2.5ml ammonium molybdate solution

6. Shake well on a vortex stirrer and wait 5minutes.

7. Add1.25ml tartaric acid solution

8. Add 0.25ml ANSA reducing solution. Mix well.

9. Prepare a sample blank for each sample in a similar way, but using water instead of the ammonium molybdate solution. Also prepare a reagent blank, using 0.01M CaCl2 instead of sample and water instead of the ammonium molybdate solution. The reagent blank is used to zero the spectrophotometer prior to calibration.

10. Prepare a standard curve from the working standards by using the samealiquot for the standards as is used for the samples and treat the same way. (See note 5.)

11. The spectrophotometer should be set to 820 nm wavelength. After 30 minutes, transfer reagent blank to spectrophotometer cell, place in machine and zero absorbance. Remove, transfer sample to cell, place in machine and record absorbance reading (ie. colour intensity due to amount of soluble silica Si in sample). Wash cell before next sample with a small amount of the next sample blank.

12. Read the concentration of silica Si in the soil sample, mg/kg Si, directly from a regression equation prepared from the standard curve.

[158][Note:- 1. Discard ANSA solution if it does not completely dissolve, or yields a dark solution immediately. Try again after changing source of de-ionised water.

2. Molybdate compounds are considered as environmental hazard. Waste containing those elements has to be collected and disposed of according to regional requirements.

3. Avoid use of glass whenever possible. All standards and reagents should be kept in polyethylene or other plastic bottles, particularly NaOH to avoid any possibility of it being stored in glass. (NaOH is able to actively dissolve silica in glass)

4. Do not start filling glass test tubes in advances with any of the reagents or sample, at the glass can leach silicon.

5. As the same amount of each reagent is used for both standard solutions and samples, a small amount of Si contamination can be tolerated. The calibration line will allow for minor background contamination. However, if the blue colour in the zero stand becomes too intense, the working range may be pushed beyond the linear range of the calibration line, and all contain solutions must be prepared again. Si Contamination may occur in one or more of the following solutions; de-ionised water (used to make up one or all of the solutions), 0.5 sulfluric acid, ammonium para molybdate, tartaric acid or ANSA. Another de-ionised water supply should be used, if available. If Si is still present, reagents and extractant may need to be prepared in distilled, no de-ionised water.]

[159][30. Method of analysis of Sodium Silicate

(i)       Determination of Silicon

(a)      Chemicals and Glasswares:

(1)     Conc. HCl

 

(2)     Conc. HNO3

 

(3)     Hot Plate

 

(4)     Platinum Crucible

 

(5)     Muffle Furnace (Temp. capacity by 10000C)

 

(6)     Desiccators and other routine laboratory glasswares

(b)      Procedure:

(1)     Take 1 gm of prepared sample in Teflon or corning beaker, add 2-3 ml HCl solution (1:1) and 2-3 ml HNO3 solution (1:1).

 

(2)     Digest the solution on a hot plate till it becomes semi-solid, cool it and again add 3-4 ml HNO3 solution. Dry it completely on hot plate.

 

(3)     Add 2-3 ml HCl solution (1:1) and boil it till yellow fumes cease. Filter it with Filter Paper No. 1, wash with 10 ml HCl solution (1:1) one time and 2-3 washing with hot water .

 

(4)     Transfer the filter paper alongwith residue in pre-weighed platinum crucible, dry for one and half hour in muffle furnace at 250oC temperature and finally ignite the residue at 950oC temperature for 30 minutes.

 

(5)     Cool the crucible in desiccator and re-weigh and calculate

Calculation: (i) Determination of sodium

By the method as specified in serial number 17

(ii) Determination of Specific gravity

By the method as specified in serial number 21]

[160][31. Method of analysis of nano Nitogen

(i)       Determination of Nitrogen-Total Kjeldahl Nitrogen.

(a)      Procedure:

(1)     Liquid Nano Fertilizer sample: Take aliquot quantity (10 ml) of sample in the Kjeldahl flask.

 

(2)     In case of solid Nano Fertilizer Sample: Take one gram of powdered nano-fertilizer sample is transferred to the Kjeldahl flask

 

(3)     Add 15 g K2SO4   or 12 g anhydrous Na2SO4, 0.4g anhydrous CuSO4, or 0.6g CuSO4.5H2O, and approximately 0.8g alundum granules.

 

(4)     Add 37 ml diluted Sulfuric acid with water H2SO4+H2O(1+1, v/v) or 20 ml concentrated Sulfuric acid, if adequate ventilation is available.

 

(5)     Add sufficient test portion mass, precisely 0.1000 to 2.800 g for fertilizers with 30 to 5% nitrogen, respectively. Rinse the inner wall with about 10ml water.

 

(6)     Transfer the flask to a preheated (400oC) Kjeldahl block digestor and digest test portions for 75 minutes.

 

(7)     Remove the flask from the heating block and upon cooling (the reaction mixed must be near room temperature). Wash the inner wall with 20-30 ml water and mix.

 

(8)     Prepare the distillate receiving flask (300ml Erlenmeyer flask) by adding 30ml of 0.25 N standardized Sulfuric acid to trap the expected total Nitrogen in the test portion.

 

(9)     Add 2-3 drops of Methyl purple indicator and install the receiver on the outlet tube of the distillation unit, being sure that the distillate outlet tube end is totally immersed in the standardized acid solution.

 

(10)   Install the digestion tube on the distillation unit. Initiate steam generation and slowly dispense about 80ml (30-35%) Sodium Hydroxide into the flask.

 

(11)   Continue steam distillation until about 250 ml or more of steam condensate has been collected in the receiving flask. This usually requires about 6-8 minutes.

 

(12)   If color changes to green, add more 0.25 N H2SO4   to bring the color back to purple and record the amount of acid added.

 

(13)   Titrate to a grey end point (pH5.7) with 0.25 N Standard NaOH. The color of the distillate depends upon the amount of total nitrogen in the test portion, which is a function of the amount of ammonia trapped in the receiver flask.

 

(14)   A green color indicates that the acid in the trap was neutralized by the Ammonia. At this point, add an additional known amount of standardized H2SO4   to get to the grey end point.

 

(15)   The net volume (in ml) of standardized acid would be equal to the total amount of acid initially added to the receiving flask plus the amount of the acid added, after distillation, to reach the grey end point. A blue or Purple colour indicates that there is still acid in the receiving flask, and back titration with NaOH is required.

 

(16)   The net volume standardized acid would be equal to the amount of acid in the receiving flask minus the amount of base added, after distillation, to reach to the grey end point.

(b)      Calculations:

Weight percent total nitrogen is calculated as follows:

(ii)      Physical Particle Size (as per Transmission Electron Microscope (TEM) Analysis)

(a)      Equipment and Apparatus:

(1)     Transmission Electron Microscope

 

(2)     Sample grid

 

(3)     Tweezers, Petri dish, Ethanol and Deionized water

(b)      Procedure:

(1)     TEM sample grids carbon coated film that is electron transparent supported by copper mesh or equivalent are suitable.

 

(2)     Glassware and apparatus used for sample preparation should be cleaned with filtered, demineralized water and stored dry.

 

(3)     The apparatus used for dispersion and deposition of particles consists of a small glass vial with a screw-on cap, a teflon pillar about 10 mm high that may be inserted into the vial, a petri dish, and a teflon block about 40 mm by 40 mm square.

 

(4)     Hold the grid with tweezers, dip rinse the grid thoroughly with ethanol. Wick the excess liquid off the grid using filter paper. Place the dried grid onto the clean Teflon block.

 

(5)     Place a 10 µL drop of the nanoparticle solution onto the grid.

 

(6)     Cover the grid with a petri dish lid and let stand at room temperature for getting the grid dry, typically from 5 to 30 minutes, depending on solvent type.

 

(7)     Transfer the grid on TEM sample holder. Record enough micrographs to image a minimum of 200 nanoparticles per sample per grid square from a minimum of 2 widely separated regions of the grid using a well-aligned and stable TEM, operated at a fixed magnification that allows a large number of nanoparticles to be visible within the micrograph field of view, while ensuring that each individual nanoparticle is recorded with a large number of image pixels.

(c)      Precautions:

(1)     Transmission Electron Microscope grids (especially thin film membranes) are very fragile and must be held by their edges with fine tweezers so as not to damage or crack the membrane.

 

(2)     Exposure of Transmission Electron Microscope grids to the ambient environment should be minimized to reduce the likelihood of dust contamination. Grids should be stored in suitable boxes in dust-free or desiccating cabinets.

 

(3)     A well-aligned Transmission Electron Microscope is essential to obtain accurate particle size results.

 

(4)     A minimum of 200 discrete particles should be measured from each of at least two widely separated regions of the sample (that is, different grid squares or membrane regions). Foreign debris in a given image (e.g., dust particles or residues from the rinsing and drying process) should be avoided.

 

(5)     Particle size results obtained from Transmission Electron Microscope measurements may not coincide with those obtained from other techniques (e.g., dynamic light scattering). This is due in part to differences in the weighted averages determined in each case (e.g., number for Transmission Electron Microscope versus intensity for dynamic light scattering), as well as differences in the physical property that is actually measured (e.g., projected area versus hydrodynamic diffusion area).

(iii)     Hydrodynamic particle size (as per Dynamic Light Scattering (DLS) Analysis

(a)      Equipment and Apparatus:

(1)     Dynamic Light Scattering Equipment

(2)     Sample Cuvettes of size

(3)     Deionized water

(b)      Procedure:

(1)     For liquid nano-fartilizer sample, 10 ml is sonicated for one minute and used for the analysis. In case for solid nano-fertilizer, fertilizer: distilled water (1:10 ratio) suspension is prepared, sonicated for one minute

 

(2)     Known standard samples (either one of the nano particles such as Ag, Au or TiO2) are used to set the machine

 

(3)     Load sample into the Cuvette

 

(4)     Pre-rinse filter with solvent (at least 1 ml, depending on filter size and dead volume of filter holder or cartridge).

 

(5)     After loading syringe with sample and inserting syringe filter, allow the first 4 drops to go to waste. Use the next 4 drops to pre-rinse the cuvette, and discard. The remainder can be used for the sample measurement.

 

(6)     Load sample into cuvette using minimum amount necessary to ensure liquid level is at least 2 mm above the entrance height of the laser beam for your particular instrument configuration.

 

(7)     Take care not to touch the cuvette windows with your bare hands while loading. Wipe outside of quartz or glass cuvette with lens paper if needed. Cap the cuvette to prevent dust contamination and solvent evaporation.

 

(8)     Inspect the cuvette to ensure that air bubbles are not clinging to the optical window area.

 

(9)     Load the sample into Dynamic Light Scattering machine.

 

(10)   Perform 3 to 10 independent measurements per sample.

(c)      Precautions:

(1)     To measure the size of solid phase nano nitrogen particles, 1 gram of nanoparticles sample should be suspended in 20 ml water followed by 1 minute ultra-sonication before the size measurement carried out by the Dynamic Light Scattering.

 

(2)     Measurement cuvettes should be cleaned with filtered demineralized water and stored dry.

 

(3)     The choice of pore size depends on the maximum dimension of the test particles and their tendency to adhere to the filter membrane.   µ   Suspended medium (such as solvent, dispersant, solution) should be filtered prior to sample preparation using a 0.1 or 0.2.

 

(4)     A typical starting sample concentration is 1 mg/ml.

 

(5)     Use cuvette with quartz or equivalent optical-quality windows.

 

(6)     Pre-rinse cuvette with filtered solvent at least 3 times.

(iv)    Zeta Potential Analysis

(a)      Equipment and Apparatus:

(1)     Dynamic Light Scattering (DLS).

 

(2)     Sample Cuvettes of zeta.

 

(3)     Deionized water.

(b)      Procedure:

(1)     For liquid nano-fertilizer sample, 10 ml is sonicated for one minute and used for the analysis and in case for solid nano-fertilizer, fertilizer: distilled water (1:10 ratio) suspension is prepared, sonicated for one minute.

 

(2)     Known standard samples (either one of the nano particles such as Ag, Au or TiO2) are used to set the machine.

 

(3)     Loading Sample into the Cuvette.

 

(4)     Pre-rinse filter with solvent (at least 1 ml, depending on filter size and dead volume of filter holder or cartridge).

 

(5)     After loading syringe with sample and inserting syringe filter, allow the first 4 drops to go waste. Use the next 4 drops to pre-rinse the cuvette, and discard. The remainder can be used for the sample measurement.

 

(6)     Load sample into cuvette using minimum amount necessary to ensure liquid level is at least 2 mm above the entrance height of the laser beam for your particular instrument configuration.

 

(7)     Take care not to touch the cuvette windows with your bare hands while loading. Wipe outside of quartz or glass cuvette with lens paper if needed.

 

(8)     Cap the cuvette to prevent dust contamination and solvent evaporation.

 

(9)     Inspect the cuvette to ensure that air bubbles are not clinging to the optical window area.

 

(10)   Load the sample into Dynamic Light Scattering machine.

 

(11)   Perform 3 to 10 independent measurements per sample.

(c)      Precautions:

(1)     Measurement cuvettes should be cleaned with filtered demineralized water and stored dry. The choice of pore size depends on the maximum dimension of the test particles and their tendency to adhere to the filter membrane. µ suspending medium (such as solvent, dispersant, solution) should be filtered prior to sample preparation using a 0.1 or 0.2

 

(2)     A typical starting sample concentration is 1 mg/ml.

 

(3)     Use cuvette with quartz or equivalent optical-quality windows.

 

(4)     Pre-rinse cuvette with filtered solvent at least 3 times.

(v)      Viscosity Measurement:

(a)      Equipment and Apparatus:

(1)     Demineralised water.

 

(2)     Viscometer.

 

(3)     Measuring cylinder.

 

(4)     Bottle Adapter.

(b)      Procedure:

(1)     Calibrate the viscometer with distilled water to set the machine as 1 cps.

 

(2)     Viscometer Assembly.

 

(3)     Attach vertical pole to the base using the wrench provided in the case.

 

(4)     Attach the viscometer to the vertical pole.

 

(5)     Connect power cable to the viscometer.

 

(6)     Turn on the viscometer and calibrate.

 

(7)     Starting up-Select and attach required spindle.

 

(8)     Raise the viscometer to the highest level using a screw on the vertical pole.

 

(9)     Place beaker with liquid under the spindle.

 

(10)   Lower the viscometer until the spindle is submerged to the spindle's mark.

 

(11)   Viscometer Operation:-This depend on the software of the instrument make. The analyst should follow the manufacturer's operating instructions for a particular instrument. Set the viscometer using distilled water to measure 1cps at room temperature.

(c)      Precautions:

(1)     Wait for 30-60 sec before reading.

 

(2)     Good results are in range 60%-80% of torque.

 

(3)     Results depend on beaker and volume of liquid so use the same beakers for comparison measurements. Viscosity of a Liquid nano-fertilizer N is measured directly.

 

(4)     For solid nano-fertilizer, fertilizer: water suspension should be in 1:10 ratio with distilled water.

(vi)    Measurement of pH

(a)      Apparatus:

pH meter, vacuum pump, beaker, pipette, glass rod, china dish, spatula etc.

(b)      Reagents:

Buffer solutions of pH 4.0, 7.0 and 9.2: One buffer tablet of the respective pH is dissolved in water and the volume is made to 100 ml.

(c)      Procedure:

(1)     Take 10 ml of liquid sample, homogenise it and take the pH measurement. For solid/powder samples (1 g dry sample/10 ml water) homogenisation or ultrasonic agitation of the sample for 1 minute followed by pH measurement should be taken after settling of the samples.

 

(2)     pH meter is set at room temperature and calibrated by immersing theelectrodes in different buffer solutions of pH 4.0, 7.0 and 9.2.

 

(3)     Take the beaker of homogenised samples and dip the electrodes into it and note the pH reading.

 

(4)     After each determination the electrodes must be washed with distilled water and wiped out by ordinary filter paper.

(d)      Precautions:

(1)     Proper homogenisation/sonication must be done.

 

(2)     The glass and reference electrode of pH meter should always remain dipped in water.

 

(3)     Buffer solutions should be prepared accurately and stored well in glass container.

 

(4)     It is desirable to prepare fresh buffer solutions after few days. Connect the pH meter to the stabilizer to avoid the fluctuations in pH readings. Adjust the temperature knob of pH meter at room temperature for correct pH determination]

[161][32. Method of analysis of Zinc Polyphosphate

(i)      Quality of reagents

Pure chemicals and distilled water shall be used in tests.

Note: Pure chemicals shall mean chemicals that do not contain impurities which affect the results of analysis.

Demineralised water means the water obtained after passing distilled water through a cation and an anion exchange resins or a combined cationation exchange resin. Glass distilled water means distilled water that is redistilled in a glass distillation apparatus.

(ii)    Determination of zinc:

(a)      Reagents

(1)     Standard zinc solution-Weigh accurately 1.0 g of zinc metal A.R. grade in a 250 mL beaker. Add 20 mL HCl (1: 1) to it and cover with a watch glass. Keep it for a few hours and allow it to dissolve completely. Transfer it to one litre flask through a funnel giving at least 10 washings of beaker and funnel with glass distilled water. Make up the volume using glass distilled water. Stopper the flask and shake the solution well. This is 1000 ppm zinc solution herein after called Standard A. This solution should be stored in a clean bottle for further use. Dilute 10 ml of 1000 ppm solution of zinc (Standard A) to 1 litre to get 10ppm standard zinc solution designated as Standard B.

 

(2)     Concentrated hydrochloric acid (HCl).

 

(3)     Glass distilled water of pH 2.5. Dilute 1 ml of concentrated hydrochloric acid to one litre with glass distilled water and adjust the pH to 2.5 with a pH meter using HCl or NaOH. This solution is called acidified water and 5 to 10 litres of this solution should be prepared at a time. Do not use sulphuric acid for preparing this acidified water.

 

(4)     Preparation of working standards-Pipette the following volume of Standard B in 50 ml numbered volumetric flask and make the volume with acidified water (See Table below). Stopper the flasks and shake them well. Prepare the standard in duplicate. The same acidified water should be used for preparing the solution of unknown fertilizer samples. Fresh standards should be prepared every time when a fresh lot of acidified water is prepared.

Flask No.

(b)      Procedure

(1)      Preparation of zinc polyphosphate fertilizer sample-Weigh 250 mg (0.25 g) fertilizer in a clean watch glass. Transfer into a 250 mL Erlenmeyer flask (conical flask) using a funnel. Wash the watch glass and funnel with 10 mL concentrated hydrochloric acid. Do not use sulphuric acid for dissolving the sample. Do not dilute with water. Place a funnel over the mouth of the Erlenmeyer flask and heat over a hot plate till fumes of acid appear. Allow the solution to cool to room temperature. Carefully add 100 mL water and swirl to mix. Then filter through Whatman 1 filter paper into a 1L volumetric flask. Wash the Erlenmeyer flask and filter paper repeatedly (at least ten times with 10 mL portions of water) and then dilute to volume. Prepare these solutions in duplicate.

(2)      Pipette 10 ml of the prepared solution in 500 ml volumetric flask and make the volume with acidified water (hydrochloric acid water).

(3)      Flaming the solutions--Flame the standards and the filtered samples on atomic absorption spectrophotometer at a wavelength of 213.8 mu (Zn line of the instrument).

(c)      Calculations

Prepare a standard curve of known concentrations of zinc solution by plotting the absorbance values on Y-axis against their respective zinc concentration on X-axis Calculate the percentage zinc in zinc fertilizer by multiplying zinc concentration value calculation from standard curve by 20.

Example

Weigh of the fertilizers sample .................. = 0.25 g

Volume made ............................................. = 1000 ml

Further dilution .......................................... = 50 times

Reading of the samples form atomic absorption...= Y

Corresponding concentration value of zinc from standard curve against Y absorbance ................................................ = X ppm

Percentage zinc in the fertilizer ................. = 20X

(d)      Precautions.

(1)     Weighing must be done on an electric or electronic balance.

 

(2)     All the glass apparatus to be used should be of corning or borosil make and washed with dilute hydrochloric acid (1:4), and subsequently washed thoroughly with distilled water and then with glass distilled water.

 

(3)     The pipette should be rinsed thrice with the same solution to be measured.

 

(4)     The outside or the pipette should be wiped with filter paper after taking out from the solution to be measured.

 

(5)     After using the pipettes, wash with distilled water and place them on a clean dry filter paper in order to prevent contamination.

 

(6)     To start filtration only a few drops should be added first in order to wet the filter paper and then continue further filtration.

 

(7)     Do not use sulphuric acid for dissolving the sample or for dilution of solution prior to analysis.

(iii)   Determination of magnesium

(a)      Reagents

(1)     Strontium chloride-Dissolve 7.5 g of strontium chloride (SrCl2.6H2O) in one litre of glass distilled water.

 

(2)     Standard magnesium solution-Weigh 0.507 g of magnesium sulphate (MgSO4.7H2O) on a clean watch glass and transfer it to one litre flask through the funnel giving several washings to watch glass and the funnel with glass distilled water. This is 50ppm Mg solution Dilute 10 ml of 50 ppm solution of Mg to 100 ml to get 5 ppm standard Mg solution.

 

(3)     Preparation of working standards-Pipette the following volume of 5 ppm standard Mg solution in 50 ml numbered volumetric flasks. Add 10 ml of strontium chloride solution to each flask and make up the volume to 50 ml. Stopper the flask and shake them well prepare fresh standards every for night.

(b)      Procedure.

(1)     Pipette 5 ml of the solution which was prepared for the determination of zinc by dissolving 0.25 g of the fertilizer sample in one litre flask [this section (ii) (b) (1)] Add 50 ml of strontium chloride Make up the volume to 250ml.

(2)     Flame the standards and the samples on atomic absorption spectrophotometer at a wave length of 285.5 mu (Mg line of the instrument)

(c)      Calculations

Prepare a standard curve of known concentrations of Mg solutions by plotting the absorbance value on Y-axis against their respective concentration values on X-axis. Percentage magnesium in the fertilizer will correspond to the magnesium concentration value calculated from the standard curve multiplied by 20.

Example: Weight of the fertilizer ............................. = 0.25 g

Volume made ........................................... = 1000 ml.

Further dilution ......................................... = 50 times

Reading of the sample from atomic absorption spectrophotometer ..................................... = Y

Corresponding concentration of Mg from standard curve against Y absorbance ................................ = X ppm

Percentage magnesium in the fertilizer ............... = 20X

(iv)   Determination of lead

(a)      Reagents.

(1)     Standard lead solution-Weigh 0.1599 g of lead nitrate [Pb(NO₃)₂] on a clean watch glass and transfer it to one litre flask through a funnel using glass distilled water. Add 10 ml of concentrated distilled nitric acid and make the volume upto the mark. Stopper the flask and shake the solution well. This is 100 ppm lead solution and should be stored in a clean bottle for further use. Dilute 10 ml of 100 ppm solution of lead to 100 ml with 1 percent nitric acid solution to get 10 ppm standard lead solution.

 

(2)     1 percent nitric acid solution-Dilute 10 ml of concentrated distilled nitric acid to one litre with glass distilled water.

 

(3)     10 percent nitric acid solution-Dilute 10 ml of concentrated distilled nitric acid to 100 ml with glass distilled water.

 

(4)     20 percent zinc sulphate solution-Weigh 20g of zinc sulphate (ZnSO₄.7H₂O) and dilute to 100 ml with 1 percent nitric acid solution.

 

(5)     Preparation of working standards-Pipette the following volume of 10 ppm standard lead solution in 50 ml numbered volumetric flasks. Add 5 ml of 20 percent zinc sulphate solution to each flask and make the volume with 1 percent nitric acid solution.

Stopper the flasks and shake them well.

(b)      Procedure.

(1)     Preparation of zinc polyphosphate fertilizer samples-Weigh 1 g of the material on a clean watch glass and transfer to 100 ml volumetric flask through the funnel using 10 ml of 10 percent nitric acid solution. Let it stand for a few hours till it dissolves. Add 10 mL of 20% zinc sulphate solution to the flask. Make the volume with glass distilled water. Samples should be prepared in duplicate.

(2)     Flaming the solution--Flame the standards and the samples on atomic absorption spectrophotometer at a wavelength of 217 m (Lead line of the instrument)

(c)      Calculations

Prepare a standard curve of known concentrations of lead solution by plotting the absorbance values on Y-axis against their respective lead concentration on X-axis. Calculate the percentage lead in zinc polyphosphate fertilizer by multiplying lead concentration value calculated from standard curve by 0.01.

Example: Weight of the fertilizer ............................. = 1.0 g

Volume made ........................................... = 100 ml.

Further dilution ......................................... = Nil

Reading of the sample from atomic absorption spectrophotometer ..................................... = Y

Corresponding concentration of Pb from standard curve against Y absorbance ................................ = X ppm

Percentage Pb in the fertilizer ............... = 0.01X

(v)     Determination of Arsenic (as As)

The principle and reagents in this case shall substantially be the same as given in Schedule IV, Part D, 12 relating to determination of As in organic fertilizers by Atom Absorption Spectrophotometer (AAS).

(a)      Reagents.

(1)     Standard sodium hydroxide solution--approximately 20 percent.

 

(2)     Standard arsenic trioxide solution-Dissolve 1.320 gm. of resublimed arsenic trioxide (AS₂ O₃) in 25 ml. sodium hydroxide solution and neutralize with dilute sulphuric acid. Dilute with freshly distilled water containing 10 ml of concentrated sulphuric acid per liter and make up the volume to 1 liter. This solution contains 1000 ppm As and is solution A.

 

(3)     Pipette 5 mL of solution A into a 1 L volumetric flask and dilute to volume. This solution contains 5 ppm As and is solution B.

 

(4)     Prepare standards having concentration of 0.05, 0.1 and 0.2 ppm by diluting 1.0, 2.0 and 4.0 ml, respectively of 5 ppm Arsenic solution (solution B) with double distilled water in volumetric flask and make up the volume to 100 ml.

(b)      Procedure.

(1)     Preparation of zinc polyphosphate fertilizer sample-Weigh 1.0 g of fertilizer in a clean watch glass. Transfer into a 250 mL Erlenmeyer flask (conical flask) using a funnel. Wash the watch glass and funnel with 10 mL concentrated hydrochloric acid. Place a funnel over the mouth of the Erlenmeyer flask and heat over a hot plate till fumes of acid appear. Allow the solution to cool to room temperature. Carefully add 100 mL water and swirl to mix. Neutralise the solution with 12 mL I N NaOH solution. Transfer to a 1 L volumetric flask and make up volume.

 

(2)     Estimate Arsenic using vapour generation assembly attached to Atomic Absorption Spectrophotometer as per the procedure given for the instrument. Use the solution of fertilizer directly without further dilution.

(c)      Calculations.

Prepare a standard curve of known concentrations of As solutions by plotting the absorbance value on Y-axis against their respective concentration values on X-axis. Percentage As in the fertilizer will correspond to the As concentration value calculated from the standard curve multiplied by 0.1.

Example: Weight of the fertilizer ............................. = 1.0 g

Volume made ........................................... = 1000 ml.

Further dilution ......................................... = Nil

Reading of the sample from atomic absorption spectrophotometer ..................................... = Y

Corresponding concentration of AS from standard curve against Y absorbance ................................ = X ppm

Percentage As in the fertilizer ............... = 0.1X

(vi)   Determination of cadmium

Same as provided in paragraph (x) under subheading 7.

(a)      Reagents and procedure same as in subheading 7 (x).

(b)      Procedure.

(1)     Preparation of zinc polyphosphate fertilizer sample-Weigh 1.0 g of fertilizer in a clean watch glass. Transfer into a 100 mL beaker with 10 mL 20 percent hydrochloric acid. Heat over a hot plate till dissolved. Allow the solution to cool to room temperature. Neutralise with 4% NaOH solution (1 N NaOH) to pH 2.5. Transfer to a 100 mL volumetric flask and make up volume.

(2)     Aspirate the standards as well as the sample solution for Cd on an atomic absorption spectrophotometer at a wavelength of 228.8 nm using air acetylene flame and note the absorbance for each solution.

(c)      Calculations.

Prepare a standard curve of known concentrations of Cd solutions by plotting the absorbance value on Y-axis against their respective concentration values on X-axis. Percentage As in the fertilizer will correspond to the Cd concentration value calculated from the standard curve multiplied by 0.01.

Example: Weight of the fertilizer ............................. = 1.0 g

Volume made ........................................... = 100 ml.

Further dilution ......................................... = Nil

Reading of the sample from atomic absorption spectrophotometer ..................................... = Y

Corresponding concentration of Cd from standard curve against Y absorbance ................................ = X ppm

Percentage Cd in the fertilizer ............... = 0.01X

(vii)  Determination of pH

(a)      Procedure

Weigh 5 g of fertilizer into a 100 mL beaker. Add 50 mL distilled water, stir and immediately record pH before the suspension sediments.

(viii)    Determination of water soluble zinc.

(a)      Reagents

As described in item (ii) (a) of this serial number relating to "Determination of Zinc".

(b)      Procedure.

(1)     Extraction of water soluble zinc

Weigh 250 mg zinc fertilizer into a 500 mL Erlenmeyer flask (conical flask). Add 100 mL of glass distilled water. Place a stopper at the mouth and shake the solution in a horizontal shaker for 15 min. Filter through a Whatman 1 filter paper into a 500 mL volumetric flask. Wash the Erlenmeyer flask and filter paper repeatedly (at least ten times with 10 mL portions of water). Remove the funnel and filter paper. Add 5 mL concentrated HCl directly to the solution in the volumetric flask and then make up volume. Prepare these solutions in duplicate.

(2)     Pipette 5 ml of the prepared solution in 50 ml volumetric flask and make the volume with acidified water (hydrochloric acid water).

(3)     Flaming the solutions--Flame the standards and the filtered samples on atomic absorption spectrophotometer at a wavelength of 213.8 mu (Zn line of the instrument).

(c)      Calculations

Prepare a standard curve of known concentrations of zinc solution by plotting the absorbance values on Y-axis against their respective zinc concentration on X-axis Calculate the percentage zinc in zinc fertilizer by multiplying zinc concentration value calculation from standard curve by 20.

Example. Weigh of the fertilizers sample .................. = 0.25 g

Volume made ............................................. = 500 ml

Further dilution .......................................... = 10 times

Reading of the samples form atomic absorption...= Y

Corresponding concentration value of zinc from standard curve against Y absorbance ................................................ = X ppm

Percentage water soluble zinc in the fertilizer ................. = 2X

(ix)   Determination of DTPA soluble zinc.

(a)      Reagents

(1)     Prepare a solution of 0.005 M DTPA (diethylenetriaminepentaacetic acid, [(HOOCCH2)2 NCH2CH2]2NCH2COOH; molecular weight 393.35) by weighing 1.97 g DTPA in a 1000 mL volumetric flask. Add 800 mL water and heat till it is completely dissolved. Cool to room temperature and then make up the volume to 1 litre.

(2)     Other reagents as described in item (ii) (a) of this serial number relating to "Determination of Zinc".

(b)      Procedure.

(1)     Extraction of DTPA soluble zinc-Weigh 250 mg zinc fertilizer into a 1 L Erlenmeyer flask (conical flask). Add 250 mL of the DTPA solution. Place a stopper at the mouth and shake the solution in a horizontal shaker for 60 min. Filter through a Whatman 1 filter paper into a 1 L volumetric flask. Wash the Erlenmeyer flask and filter paper repeatedly (at least ten times with 10 mL portions of water). Remove the funnel and filter paper. Add 5 mL concentrated HCl directly to the solution in the volumetric flask and then make up volume. Prepare these solutions in duplicate.

(2)     Pipette 10 mL of the DTPA extracted solution into a 500 mL volumetric flask and make up volume with acidified water (hydrochloric acid water).

(3)     Flaming the solutions--Flame the standards and the filtered samples on atomic absorption spectrophotometer at a wavelength of 213.8 mu (Zn line of the instrument).

(c)      Calculations

Prepare a standard curve of know concentrations of zinc solution by plotting the absorbance values on Y-axis against their respective zinc concentration on X-axis Calculate the percentage zinc in zinc fertilizer by multiplying zinc concentration value calculation from standard curve by 20.

Example. Weigh of the fertilizers sample .................. = 0.25 g

Volume made ............................................. = 1000 ml

Further dilution .......................................... = 50 times

Reading of the samples form atomic absorption...= Y

Corresponding concentration value of zinc from standard curve against Y absorbance ................................................ = X ppm

Percentage DTPA soluble zinc in the fertilizer ................. = 20X

(d)      Precautions.

(1)     Weighing must be done on a electric or electronic balance.

 

(2)     All the glass apparatus to be used should be of corning or borosil make and washed with dilute hydrochloric acid (1:4) and subsequently washed thoroughly with distilled water and then with glass distilled water.

 

(3)     The pipette should be rinsed thrice with the same solution to be measured.

 

(4)     The outside or the pipette should be wiped with filter paper after taking out form the solution to be measured.

 

(5)     After using the pipettes, place them on a clean dry filter paper in order to prevent contamination.

 

(6)     To start filtration only a few drops should be added first in order to wet the filter paper and then continue further filtration.

 

(7)     Do not use sulphuric acid for dilution of solution prior to analysis.]

[162][33. Method of analysis of potassium Thiosulphate and Calcium Thiosulphate (Liquid Fertilizers)

(i)       Determination of potassium by the method as specified in 5 (ii);

 

(ii)      Determination of Specific Gravity by the method as specified in 21 (ii);

 

(iii)     Determination of Calcium by the method as specified in 21 A (v);

 

(iv)    Determination of Arsenic by the method as specified in 8 (ix);

 

(v)      Determination of Lead by the method as specified in 8(v);

 

(vi)    Determination of Sulphur (as S) in potassium thiosulphate and calcium thiosulphate (Liquid Fertiliser).-

(a)      Apparatus.

(i)       Electric hot plate, water bath, muffle furnace, Oven;

 

(ii)      Electronic balance;

 

(iii)     Desiccators;

 

(iv)    Gooch crucible;

 

(v)      Vacuum pump for filtration;

 

(vi)    Electronic balance (0.001g capacity);

 

(vii)   Whatman No. 40 and 50 filter papers;

 

(viii)  Routine laboratory glassware, instruments;

(b)      Reagents.

(i)       Conc. Hydrochloric acid(37% HCL);

 

(ii)      Dilute hydrochloric acid-Take 250 ml of concentrated hydrochloric acid in one litre volumetric flask. Make the volume upto 1000 ml water. Shake and mix it well';

 

(iii)     Barium chloride solution: Dissolve 120 gm barium chloride in 1000 ml of water;

 

(iv)    silver nitrate (5 percent solution): Dissolve 5g of silver nitrate in 100 ml of distilled water;

 

(v)      Hydrogen per oxide 30 percent (fresh) solution: Dilute liquid hydrogen peroxide to bring final concentration 30 percent;

 

(vi)    Sodium hydroxide solution: Dissolve 40g sodium hydroxide salt in 100 ml distilled water;

 

(vii)   Methyl orange indicator: Dissolve 1g methyl orange indicator in 100 ml alcohol. Shake it and store in cool dry Place;

 

(viii)  Sodium Thiosulphate: AR Grade.

(c)      Procedure.

1.        Oxidation of liquid fertilizer test sample;

(a)      Weight 5.0g sample of potassium thiosulphate (or calcium thiosulphate) liquid fertilisers (up to 0.001 g) accurately in a dry, clean 500 ml graduated flask on an electronic balance. Denote "W" to this as weight of sample. Fill the flask to the mark of 500 ml by using double distilled water'.

 

(b)      Add exactly 50 ml (of the diluted sample from (a) to a 500 ml beaker and add approximately 100 ml of water. Add 2 ml of 40% NaOH solution to it. Add now slowly 2 ml of 30% hydrogen per oxide (H2O2) solution. Cover the beaker with watch glass carefully. Heat the solution on low heat on hot plate slowly for about 30 minutes. Cool it and then add slowly 2 ml of hydrogen peroxide 30% solution again. Heat the solution on hot plate slowly. If required add more 1 to 2 ml of hydrogen per oxide solution. Total hydrogen peroxide solution addition should not be more than 6 ml for complete oxidation. Cool the beaker; add 100 ml of water and then mix.

 

(c)      Add a few drops of methyl orange indicator to the solution. Add 2-5 ml of dilute hydrochloric acid and mix it until colour changes to red uniformly. Add a few more drops of acid and mix well with glass rod.

Then, keep the beaker on hot plate (below boiling temperature, <800C) to bring the solution to colorless within 10 minutes.

Note: lf necessary, add a few drops of 30% H2O2 to the beakers to bring the solution to colourless.

2.        Precipitation of sulphur for gravimetric determination of total sulphur,-

(a)      Add slowly 15 ml barium chloride to the oxidized sample to ensure complete precipitation of sulphur as barium sulphate;

 

(b)      Digest the precipitation on a hot plate or water bath for minimum 5 hours at such a temperature that the solution does not boil (around 80oC). Put a watch glass above the beaker to prevent complete evaporation of the solution. Ensure the supernatant liquid to be clear and transparent. Cool it to room temperature and keep it over night to settle precipitates;

 

(c)      Take 30 ml capacity G4 grade Sintered Gooch crucible. Dry it in furnace at 2500C; cool it and record weight of empty crucible(G1);

 

(d)      Pour the sample with precipitate into 30 ml capacity G4 grade Sintered Gooch Crucible previously weighed. Filter it. Wash the precipitate 10-12 times with hot water to ensure the precipitate to make it free from excess barium chloride. The filtrate may be tested with silver nitrate solution to confirm that the precipitate is free from chloride.

 

(e)      Dry the crucible having barium sulphate precipitate at 2500 C for two hours in a furnace by raising the temperature of the furnace slowly from room temperature to constant weight taken and note the weight(G2).

3.        Calculations:-

Total sulphur (as S) percent = 

Whereas

G1= weight of Gooch crucible (+ filter paper if used)

G2 = Weight of Gooch crucible + barium sulphate precipitate (+ filter paper if used)

W= Weight of sample

Factor 13.74= Per cent total sulphur (w/w) in barium sulphate = 32 × 100/233.39

34. Method of analysis of Phospho Gypsum

1.        Determination of calcium as calcium Sulphate Dihydrate in Phospho Gypsum

(i)       Standarisation of calcium solution-as per method specified in 21A (b)

(ii)      Procedure:-

(a)      Take 1 gram of sample in 250 ml dry beaker. Add 50 ml dilute Hydrochloric acid (1:1)

 

(b)      Boil for 5 minutes on slow heater and cool to room temperature. Add 50 ml distilled water.

 

(c)      Transfer the solution in 250 ml volumetric flask and make the volume to 250 ml with distilled water.

 

(d)      Take 25 ml aliquot in 250 ml washed conical flask and 20 ml distilled water and 20 ml buffer solution. Add few drops of indicator and tighted with EDTA solution till blue color is obtained. Note the volume of EDTA used as V2.

Note:- if the solution is not clear after digestion filter it and then take aliquot.

2.        Calculation:-

Calcium (as Calcium Sulphate Dihydrate) per cent.= V2 X Calcium titer X 3. 4 X 1.]

[163][35. Method of analysis of potash Fortified Silicon by Spectrophotometer

I.         Determination of Silicon as Si (OH)4.

A.        Reagents:

(1)     Silicon Standard Solution (1000 ppm):--

Take 7.5534 gm of Na 2SiO₃.5H₂O in 1000 ml of volumetric flask and dissolve in 100 ml distilled water and make the volume to 1000 ml with distilled water. From 1000 ml standard solution take 10 ml in 100 ml volumetric flask and dilute to the mark with distilled water. Prepare 1 ppm, 2 ppm, 3 ppm and 4 ppm working standard solution in 100 ml volumetric flask accordingly.

(2)     Tartaric Acid Solution:-

Dissolve 50 gram tartaric acid in water and dilute to 500 ml. Store in plastic bottle.

(3)     Ammonium Molybdate Solution:-

Dissolve 7.5 gm Ammonium Molybdate (NH₄)₆ M07 O24 4H2O) in 75 ml water, add 10ml H₂SO₄(1:1) and dilute to 100 ml with distilled water and Store in plastic bottle.

(4)     Reducing Solution:-

Dissolve 0.7 gm Na₂SO₃ in 10 ml water and add 0.15 gm 1-Amino-2-Naphthol-4-Sulphonic Acid. Stir until dissolved. Dissolve 9 gm NaHSO₃ in 90 ml distilled water, add to first solution and mix properly. Store in plastic bottle.

B.        Preparation of Sample Solution.

(1)     Grind requisite quantity of Sample and dry at 105-degree C for two hours.

 

(2)     Place 0.2-0.5 gm sample in 75 Nickel Crucible.

 

(3)     Mix 0.3 gm KNO3 with sample and add 1.5 gm NaOH pellets.

 

(4)     Cover the crucible with Nickel cover and heat to 5 minutes at dull redness over gas flame (do not fuse in furnace).

 

(5)     Remove the crucible from flame and swirl melt around sides.

 

(6)     Cool and add 50 ml distilled water and warm to disintegrate fused cake.

 

(7)     Transfer the material to 150 ml plastic beaker containing 15 ml 5N HClO4 (perchloric acid).

 

(8)     Scrub crucible and lid and wash any residue (with warm distilled water) into beaker.

 

(9)     Transfer it into 250 ml volumetric flask and dilute to volume.

 

(10)   Dilute this sample solution for spectrophotometric analysis accordingly.

C.        preparation of Standard Curve.

(1)     Prepare working standard solution of different strength in 100ml volumetric flask as the like 1 ppm, 2ppm, 3 ppm and 4 ppm and blank solution. Add 1 ml Ammonium Molybdate solution with swirling. Mix well and let it stand for 10 minutes then add 4 ml tartaric acid solution with swirling and mix well. Add 1 ml reducing solution with swirling. dilute to volume with distilled water. Mix well let it stand for thirty minutes.

(2)     Take the absorbance of standard Si solution against blank at 650 nm. Follow same procedure for sample solution and calculate the Si percentage in sample.

Calculation:-

(i)       % Si = X x DF x 10-4

X = Concentration of sample in ppm

(ii)      % of Silica as Si (OH)₄ =% Si x CF

Note:- All the plastic wares are to be used during the analysis.

II.       Determination of Potash

Determination of water Soluble K₂O by the method as specified in 5 (ii) under The said order.]

[164][36. Method of analysis Chelated Manganese as Mn-EDTA:-

A.        Reagents:

(i)       Glass distilled water or demineralized water of pH 2.5+/- 0.5:-Dilute l ml of 10% H2SO4 to one litre with glass distilled water or demineralized water and adjust the pH to 2.5 with a pH meter using 10% H2SO4 or NaOH.

(ii)      Di Sodium EDTA solution :- Dissolve 0.73 gm of di sodium EDTA di hydrate indistilled water and make volume to 100 ml.

B.        Preparation of standard Manganese metal stock solution [1000ppm]:

(i)       Dissolve 1.0 gm of Manganese metal in 50 ml of conc. Hydrochloric acid and make volume to 1000 ml with distilled water. This is 1000 ppm Manganese stock solution.

(ii)      Intermediate solution (100 ppm):- Pipette 10 ml of Manganese stock solution and 10 ml of Di sodium EDTA solution in 100 ml of volumetric ?ask and dilute to volume with distilled water.

(Note:- In case the metal stock solution is not exactly 100.0 ppm, the exact titer value of di sodium EDTA required to chelate the metal has to be added.)

(iii)     Working Standard Solution:- Pipette following volumes of 100 ppm intermediate solution in 100 ml Volumetric ?ask and make volume with acidi?ed water.

C.        Preparation of sample solution for Chelated Manganese:

(i)       Weigh 1.0 gm of sample and transfer into 100 ml volumetric ?ask and make volume with distilled water. Pipette out 1.0 ml of sample solution and dilute further to make second dilution of 100 m1 with distilled water, pipette 5 ml from second dilution and make volume to 50 ml with acidi?ed water to get the above flaming range from 1.0-4.0 ppm.

(ii)      Flaming the solutions:- Flame the standards and the sample of Chelated Manganese on atomic absorption spectrophotometer at a wavelength of 279.5nm (Mn line of instrument ) using air-acetylene flame.

(iii)     Prepare a blank solution from which only the sample has been omitted. Flame along with standards and sample.

D.       Calculations:- Prepare a standard curve of 1‹nown concentration of Manganese solutions by plotting the absorbance value on Y-axis against their respective concentrations on X-axis.

Part-I :- Determination of Total Manganese content in Chelated Manganese sample:- Total Mn content = Concentration of Mn in ppm obtained after flaming the solution X 10

Part-II :- Determination of Free Manganese content in Chelated sample:-

Reagents:- 0.02 M Disodium salt of EDTA- 0.7444 gm of Disodium Salt of EDTA in 100 ml of distilled water. Standardize with 0.02 M standard Zinc or Manganese Metal solution.

(i)       Hydroxylamine Hydrochloride - 0.1-0.2 gm;

(i)       Trietanolamine - 1-2 m1

(ii)      Buffer solution of pH - 10.0;and

(iii)     Indicator Eriochrome black T (EBT) powder.

Take 10 ml of aliquot from stock dilution of sample (1.0 g in 100 ml) Add to it 0.1 g Hydroxylamine HCl,  1to 2 ml of triethanolamine, 10 ml bu?er of pH 10.0, EBT indicator and titrate against 0.02 M disodium EDTA solution.

% Free Manganese=Titration value of EDTA x Atomic weight of Mn metal Molarity of EDTA x 1

% Chelated Manganese content = % Total Manganese - % Free Manganesecontent

37. Method of analysis of Chelated Calcium as Ca EDTA:-

A.        Reagents:-

(i)       Glass distilled water or demineralized water of pH 2.5+/- 0.5:-

Dilute l ml of 10% H2SO4 to one litre with glass distilled water or demineralized water and adjust the pH to 2.5 with a pH meter using 10% H2SO4 or NaOH.

(ii)      Di sodium EDTA solution:- Dissolve 0.73 gm of di sodium EDTA di hydrate indistilled water and make volume to 100 ml.

(iii)     Strontium Chloride (SrCl2 .6H2O )- 15.0 gm in 0.5N HCl and dilute to 100 ml.

B.        Preparation of Standard stock solution of Calcium 1000 ppm.-

(i)       Dissolve 2.498 gm CaCO3 in a minimum amount of 3 N HCl. Dilute to 1000 ml with distilled water. This is 1000 ppm calcium stock solution.

(ii)      Intermediate solution [100 ppm].- Pipette 10 ml of Calcium stock solution and 50 ml of Disodium EDTA solution in100 ml volumetric flask and dilute volume with distilled water.

(Note:- In case the metal stock solution is not exactly 100.0ppm, the exacttiter value of disodium EDTA required to chelate the metal has to be added.)

(iii)     Working Standard solution.- Pipette following volumes of 100 ppm intermediate solution in 100 ml Volumetric ?ask and make volume with acidi?ed water.

C.         Preparation of sample solution for Chelated Calcium.

(i)       Weigh 1.0 gm of sample and transfer into 100 ml volumetric ?ask and make volume with distilled water. Pipette out 5.0 ml of sample solution and dilute further to make second dilution of 100 ml with distilled water, pipette 10.0 ml from second dilution and make volume to 100 ml with acidi?ed water to get the above flaming range from 5.0-20.0 ppm.

(ii)      Flaming the solutions.

Flame the standards and the sample of Chelated Calcium on Atomic Absorbption Spectrophotometer at a wavelength of 422.7 nm (Ca line of instrument) using air-acetylene flame.

(iii)     Prepare a blank solution from which only the sample has been omitted. Flame along with standards and sample.

D.       Calculations.- Prepare a standard curve of known concentration of Calcium solutions by plotting the absorbance value on Y-axis against their respective concentrations on X- axis.

Part-I :- Determination of Total Calcium content in Chelated Calcium sample:-

Total Ca content = Concentration of Ca in ppm obtained after flaining the solution X 2

Part-II :- Determination of Free Calcium in Chelated sample:-

(i)       Reagents:- 0.02 M Disodium salt of EDTA- 0.7444 gm of Disodium Salt of EDTA in 100 ml of distilled water. Standardize with 0.02 M standard Zinc and Manganese Metal solution.

(ii)      Buffer solution of pH - 10.0

(iii)     Indicator Eriochrome black T (EBT) powder,

(iv)    Take 10 ml of aliquot from stock dilution of sample (1.0 g in 100 ml) Add to it 0.1 g

Hydroxylamine HCl, 1 to 2 ml of triethanolamine, 10 ml bu?er of pH 10.0, EBT indicator and titrate against 0.02 M disodium EDTA solution.

% Free Calcium = Titration value of EDTA x Atomic weight of Ca metal x Molarity of EDTA x 1

% Chelated Calcium content = % Total Calcium - % Free Calcium content

38. Method of analysis of Chelated Magnesium as Mg-EDTA:-

A.        Reagents.

(i)       Glass distilled water or demineralized water of pH 2.5+/- 0.5. -

Dilute 1ml of 10% H2SO4, to one litre with glass distilled water or demineralized water and adjust the pH to 2.5 with a pH meter using 1 0% H2 SO4 or NaOH.

(ii)      Di sodium EDTA solution:- Dissolve 0.73 gm of di sodium EDTA di hydrate indistilled water and make volume to 100 ml.

B.        Preparation of Standard stock solution of Magnesium 1000 ppm.

(i)       Dissolve 1.0 gm of magnesium metal in 30 ml of 1:1 HCl and dilute to 1000 ml involumetric flask with distilled water. This is 1000 ppm magnesium stock solution.

(ii)      Intermediate solution {100 ppm].

Pipette 10 ml of magnesium stock solution and 20 ml of Disodium EDTA solution in 100 ml volumetric flask and dilute volume with distilled water.

(Note:- In case the metal stock solution is not exactly I 00 ppm, the exact titer value of disodium EDTA required to chelate the metal has to be added.)

(iii)     Working Standard solution :- 

Pipette following volumes of 100 ppm intermediate solution in 100 ml Volumetric flask and make volume with acidified water.

C.        Preparation of sample solution for Chelated Magnesium:

(i)       Weigh 1.0 gm of sample and transfer into 100 ml volumetric ?ask and make volume with distilled water. Pipette out 2.0 ml of sample solution and dilute further to make second dilution of 100 ml with distilled water, pipette 1.0 ml from second dilution and make volume to 100 ml with acidi?ed water to get the above flaming range from 0.1-0.25 ppm.

(ii)      Flaming the solutions:- Flame the standards and the sample of Chelated Magnesium on atomic absorption spectrophotometer at a wavelength of 285.2 rim (Mg line of instrument) using air-acetylene.

(iii)     Prepare a blank solution from which only the sample has been omitted. Flame along with standards and sample.

D.       Calculations:

Prepare a standard curve of known concentration of Magnesium solutions by plotting the absorbance value on Y-axis against their respective concentrations on X-axis.

Part-I :- Determination of Total Magnesium content in Chelated Magnesium sample.-

Total Mg content = Concentration of Mg in ppm obtained after flaming the solution X 50

Part-II - Determination of Free magnesium in Chelated sample:-

(i)       Reagents:- 0.02 M Disodium salt of EDTA- 0.7444 gm of Disodium Salt of EDTA in 100 ml of distilled water. Standardize with 0.02 M standard Zinc and Manganese Metal solution.

(ii)      Buffer solution of pH - 10.0

(iii)     Indicator Eriochrome black T (EBT) powder

(iv)    Take 10 ml of aliquot from stock dilution of sample (1.0 g in 100 ml) Add to it 0.1 gram Hydroxylamine HCl, 1to 2 ml of triethanolamine, 10 ml bu?er of pH 10.0, EBT indicator and titrate against 0.02 M disodium EDTA solution.

% Free Magnesium=Titration value of EDTA x Atomic weight of Mg metal x Molarity of EDTA x 1

% Chelated Magnesium content = % Total Magnesium - % Free Magnesiumcontent

39. Determination of Chelated Copper as Cu-EDTA:-

A.        Reagents:-

(i)       Glass distilled water or demineralized water of pH 2.5+/- 0.5:-

Dilute l mI of 10% H2SO4 to one litre with glass distilled water or demineralized water and adjust the pH to 2.5 with a pH meter using 10% H2SO4 or NaOH.

(ii)      Di sodium EDTA solution:- Dissolve 0.73 gm of di sodium EDTA di hydrate in distilled water and make volume to 100 ml.

B.        Preparation of Standard stock solution of Copper 1000 ppm.

(i)       Dissolve 1.0 gm of Copper turnings in 30 ml of 1:1HNO3 and dilute to 1000 ml in volumetric flask with distilled water. This is 1000 ppm copper stock solution.

(ii)      Intermediate solution [100 ppm].-Pipette 10 ml of Copper stock solution and 10 ml of Disodium EDTA solution in100 ml volumetric flask and dilute volume with distilled water.

(Note:- In case the metal stock solution is not exactly 100.0 ppm, the exact titer value of disodium EDTA required to chelate the metal has to be added.)

(iii)     Working Standard solution :- Pipette following volumes of 100 ppm intermediate solution in 100 ml Volumetric flask and make volume with acidified water.

C.        Preparation of sample solution for Chelated Copper:

(i)       Weigh 1.0 gm of sample and transfer into 200 ml volumetric ?ask and make volume with distilled water. Pipette out 2.0 ml of sample solution and dilute further to make second dilution of 100 m l with distilled water, pipette 10.0 ml from second dilution and make volume to 100 ml with acidi?ed water to get between the above flaming range from 0.5-2.0 ppm.

(ii)      Flaming the solutions:- Flame the standards and the sample of Chelated Copper on atomic absorption spectrophotometer at a wavelength of 324.8 nm (Cu line of instrument ) using air-acetylene flame.

(iii)     Prepare a blank solution from which only the sample has been omitted. Flame along with standards and sample.

D.       Calculations:

Prepare a standard curve of known concentration of Copper solutions by plotting the absorbance value on Y-axis against their respective concentrations on X-axis.

Part-I :- Determination of Total Copper content in Chelated Copper sample:-

Total Cu content = Concentration of Cu in ppm obtained after ?aming the solution X10

Part-II :- Determination of Free Copper in Chelated sample:-

(i)       Reagents:- 0.02 M Disodium salt of EDTA- 0.7444 gm of Disodium Salt of EDTA in 100 ml of distilled water. Standardize with 0.02 M standard Zinc/Manganese Metal solution.

(ii)      Acetate buffer (pH= 2.8) - 4.0 gm of Sodium acetate trihydrate + glacial acetic acid 155 ml make volume to 1000 ml.

(iii)     Methanolic PAN Indicator:- 0.2 gm of PAN indicator in 10 ml of methanol.

Take 20 ml of aliquot from stock dilution of sample (1.0 g in 200 ml). Add 10 ml acetate bu?er of pH

2.8 and PAN indicator solution and titrate against 0.02 M disodium EDTA solution. End point is Magenta red to yellowish green.

% Free Copper=Titration value of EDTA x Atomic weight of Cu metal x Molarity of EDTA x 1

% Chelated Copper content = % Total Copper - % Free Copper content

40. Estimation of Zinc Content in Chelated Zinc as Zinc Glycine by AAS

E. Principle:-

The total Zinc in Zinc-Glycine is extracted by wet digestion (as Zinc) and estimated by using Atomic Absorption Spectrophotometer.

1.        Instruments / Equipments / Glasswares:-

(i)           Atomic Absorption Spectrophotometer;

(ii)         Hot Plate;

(iii)       Analytical Balance weight least count 0.1 mg; and

(iv)       Required Glasswares.

2.        Reagents and Chemicals:

(i)           Zinc Metal (pure);

(ii)         Nitric Acid (AR Grade conc.);

(iii)       Sulphuric Acid (AR Grade conc.);

(iv)       Perchloric Acid (AR Grade - 70%); and

(v)         Tri Acid Mixture (10 part of Nitric Acid + 01 part of Sulphuric Acid + 04 parts of Perchloric Acid).

3.        Procedure:

(a)      Preparation of Standard Solutions:

(i)       Preparation of 1000 ppm Standard Solution of Zinc - Weigh accurately 500 mg of Zinc metal and dissolve in 10 ml conc. Hydrochloric Acid and make the volume to the volume of 500 ml with distilled water; and

(ii)      Preparation of Working Standard Solution - Take 1 ml, 2ml, 5 ml, 8 ml, 10 ml aliquot of 100 ppm standard solution in di?erent 100 ml volumetric ?asks and add 2 ml nitric acid in each volumetric ?ask and dilute to volume using distilled water.

(iii)     These solutions will be of 1.0, 2.0, 5.0, 8.0 and 10.0 ppm respectively.

(b)      Preparation of Sample Solution.

(i)       Take 1.0 gm sample of Zinc Glycine weighed in 250 ml Erlenmeyer (Conical) flask;

(ii)      Add 10 ml of Tri acid mixture (10 part of Nitric acid : 1 part of Sulphuric acid : 4parts of Perchloric acid);

(iii)     Boil the solution at temperature between 150 to 200oC on hot plate till the solution is clear and reduce the volume till transparent fumes appears;

(iv)    Then remove the solution from hot plate, cool it and make up the volume to 250 ml with distilled water;

(v)      Take 5 ml aliquot in 250 ml volumetric ?ask and make the volume with distille dwater; and

(vi)    Run blank solution also to the same level.

(c)      Estimation of Zinc in the sample by AAS. -

Flame the standard solution followed by sample solution at 215.9 nm wavelength.

4.        Calculation:-

Zinc % by weight :-

(S-B) x V x D x 100 / W x 106

Where S = Average of concentration in sample reading in ppm V = Volume of solution

B = Blank reading in ppm D = Dilution

W = Weight of the sample in gm

Note:- Distilled water instead of Milli-Q-Water has been used during analysis of the sample.

41. Estimation of Calcium Content in Chelated Calcium as Calcium Glycine by Atomic Absorption Spectrophotometer.

Principle:-

The total Calcium in Calcium-Glycine is extracted by wet digestion (as Calcium) and estimated by using Atomic Absorption Spectrophotometer.

I.         Instruments / Equipments / Glasswares:

(i)       Atomic Absorption Spectrophotometer;

(ii)      Hot Plate;

(iii)     Analytical Balance weight least count 0.1 mg; and

(iv)    Required Glasswares.

II.       Reagents and Chemicals:

(i)       Calcium Carbonate (Assay 99.5%);

(ii)      Nitric Acid (AR Grade conc.);

(iii)     Hydrochloric Acid (Assay 35.8 - 36.5%);

(iv)    Perchloric Acid (AR Grade - 70%);

(v)      Lanthanum Oxide (Assay 99.0%);

(vi)    Acid Mixture (Nitric Acid 2 parts : Perchloric Acid 1 part) ; and

(vii)   Lanthanum Oxide Solution: 5.86%w/v (58.65 gm of lanthanum oxide, 250 ml Hydrochloric acid and make up the volume 1000 ml with Milli-Q water).

III.     Procedure:

A.        Preparation of Standard Solutions.

(i)       Preparation of 1000 ppm Standard Solution of Calcium - Weigh accurately 2.50 gm of Calcium Carbonate and dissolve in 1000 ml volumetric ?ask and make the volume to 1000 ml with distilled water; and

(ii)      Preparation of Working Standard Solution - Take 0.5 ml, 1.0 ml, 2.0 ml, 3.0 ml, 4.0 ml, 5 ml aliquot of 100 ppm standard solution in di?erent 100 mlvolumetric ?asks and add 10 ml of lanthanum oxide solution in each volumetric ?ask and dilute to volume using distilled water. These solutions will be of 0.5, 1.0,2.0, 3.0, 4.0, 5.0 ppm respectively.

B.        Preparation of Sample Solution.

(i)       Take 1.0 gm sample of Calcium Glycine weighed in 250 ml Conical flask;

(ii)      Add 10 ml of acid mixture;

(iii)     Boil the solution at temperature between 150 to 200°C on hot plate till the solution is clear & reduce the volume till transparent fumes appears;

(iv)    Then remove the solution from hot plate, cool it and add 5 ml Hydrochloric acid and make up the volume to 250 ml with distilled water;

(v)      Take 2 ml aliquot in 250 ml volumetric ?ask and add 25 ml lanthanum oxide solution and make the volume with distilled water; and

(vi)    Run blank solution also to the same level.

C.        ESTIMATION of Calcium in the sample by AAS. -

Flame the standard solution followed by sample solution at 422.67 nm wavelength.

Calculation:- Calcium % by weight :- (S-B) x V x D x 100 / W x 106

Where S = Average of concentration in sample reading in ppm V = Volume of solution

B = Blank reading in ppm D = Dilution

W = Weight of the sample in gm

Note:- Distilled water instead of Milli-Q-Water has been used during analysis of the sample.]

 

FORMS FOR REGISTRATION

EMBLEM

FORM 'A'

[See Clause 8]

FORM OF APPLICATION TO OBTAIN DEALER'S (INDUSTRIAL)*

CERTIFICATE OF REGISTRATION

To,

the Controller (If the application is for industrial dealer's certificate of

registration)

Place ......................... State of .............................

1.        Full name and address of the applicant :

(a)      Name of the concern, and postal address:

(b)      Place of business (Please give exact address):

(i)       for sale

(ii)      for storage

2.        Is it a proprietory/partnership/limited company/Hindu Undivided family concern?

Give the name(s) and address(es) of proprietor/partners/manager/Karta:

3.        In what capacity is this application filed.

(i)       Proprietor

 

(ii)      Partner

 

(iii)     Manager

 

(iv)    Karta

4.        Whether the application is for wholesale or retail or industrial dealership?

5.        Have you ever had a fertiliser dealership registration certificate in the past?

If so, give the following details :

(i)       Registration number

 

(ii)      Place for which granted

 

(iii)     Whether wholesale or retail or industrial dealership.

 

(iv)    Date of grant of registration certificate

 

(v)      Whether the registration certificate is still valid?

 

(vi)    If not, when expired?

 

(vii)   Reasons for non-renewal

 

(viii)  If suspended/cancelled and if so, when

 

(ix)    Quantity of fertilisers handled during last year

 

(x)      Names of products handled

 

(xi)    Name of source of supply of fertilisers.

6.        Was the applicant ever convicted under the Essential Commodities Act, 1955 or any Order issued thereunder including the Fertiliser (Control) Order, 1957 during the last three years preceding the date of application? If so give details.

7.        Give the details of the fertilisers to be handled

SI.No. Name of Fertiliser Source of supply

8.        Please attach certificate(s) of source from the supplier(s) indicated under column 3 of Sl.No.7.

9.        I have deposited the registration fee of Rs...vide Challan No....dated .... in treasury / Bank or enclose the Demand Draft No... datedfor Rs........... drawn on .............................. bank, in favour of..................... payable at........................................................ towards registration fee. (Please strike-out whichever is not applicable).

10.     Declaration :-

(a)      I/we declare that the information given above is true to the best of my/ our knowledge and belief and no part thereof is false.

 

(b)      I/we have carefully read the terms and conditions of the Certificate of Registration given in Form `B' appended to the Fertiliser (Control) Order, 1985 and agree to abide by them.

 

(c)      I/we declare that I/we do not possess a certificate of registration for industrial dealer and that I/we shall not sell fertilisers for industrial use. (Applicable in case a person intends to obtain a wholesale dealer or retail dealer certificate of registration, excepting a State Government, a manufacturer or importer or a pool handling agency).

 

(d)      I/we declare that I/we do not possess a certificate of registration for wholesale dealer or retail dealer and that I/we shall not sell fertilisers for agricultural use. (Applicable in case a person intends to obtain a industrial dealer certificate of registration, excepting a State Government, a manufacturer, importer or a pool handling agency).

Date Signature of the Applicant(s)

Place :

Note :

(1)     Where the business of selling fertilisers is intended to be carried on at more than one place, a separate application should be made for registration in respect of each such place.

 

(2)     Where a person intends to carry on the business of selling fertilisers both in retail and wholesale, separate applications for retail and wholesale business should be made.

 

(3)     Where a person represents or intends to represent more than one State Government, Commodity Board, Manufacturer/Importer or Wholesale dealer, separate certificate of source from each such source should be enclosed.

For use in Office of Controller

Date of receipt : Name and designation of

Officer receiving the Application

EMBLEM

FORM AI

MEMORANDUM OF INTIMATION

[See Clause 8(2)]

1.        Details of the application:

(a) Name of the applicant

(b) Name of the concern

(c) Postal address with telephone number

[165][(d) Mobile number]

2.        Place of business (Please given full address)

(i)       For Sale

(ii)      For Storage

3.        Whether the application is for -

4.        Details of fertiliser and their source in Form 'O'*

(i)       Yes No

(ii)      Yes No

(iii)     Yes No

[Please tick mark whichever is applicable]

5.        I have deposited the registration fee of Rs._______ vide Challan No.__________________ Dated______________________________ in the Bank/ Treasury_________________ or enclose Demand Draft No._____________________________ Dated_____________________________ for Rs._____________________ drawn on in favour of _____________________payable at ______________________________ towards registration fees.

6.        Whether the intimation is for an authorization letter or a renewal thereof. (Note : In case the intimation is for renewal of authorization letter, the acknowledgement in Form A2 should be submitted for necessary endorsement thereon.)

7.        Any other relevant information.

I have read the terms and conditions of eligibility for submission of Memorandum of Intimation and undertake that the same will be complied by me and in token of the same. I have signed the same is enclosed herewith.

Place:

Signature of applicant

Attach a separate sheet if the number exceeds three. Terms and Conditions of authorisation:

(1)     I shall comply with the provisions of the Fertiliser (Control) Order, 1985 and the notification issued thereunder for the time being in force.

 

(2)     I shall from time to time report to the Notified Authority and inform about change in the premises of sale depot and godowns attached to sale depot.

 

(3)     I shall also submit in time all the returns as may be prescribed by the State Government.

 

(4)     I shall not sell fertilisers for industrial use.

 

(5)     I shall file a separate Memorandum of Intimation for, where the storage point is located outside the area jurisdiction of the Notified Authority where the sale depot is located.

 

(6)     I shall file a separate Memorandum of Intimation for each place when the business of selling fertilisers is intended to be carried on at more than one place.

 

(7)     I shall file separate Memorandum of Intimation if I carry on the business of fertilisers both as retail and wholesale dealer.

 

(8)     I confirm that my previous certificate of Registration or Authorisation is not under Suspension or Cancellation or debarred from selling of fertilisers.

DECLARATION

I/we declare that the information given above is true to the best of my/our knowledge and belief and no part thereof is false or no material information has been concealed.

Signature of the Applicant(s)";

Date:

Place:

EMBLEM

FORM `A 2'

ACKNOWLEDGEMENT

[See Clause 8(3)]

1.        Received from M/s _________________ a complete Memorandum of Intimation alongwith Form O, fee of Rs. ________________by Demand Draft bearing number ___________________________ dated __________________ .

2.        this acknowledgement shall be deemed to be the letter of authorisation entitling the applicant to carry on the business as applied for, for a period of 3 years from the date of issue of this Memo of acknowledgement unless suspended or revoked by the competent authority.

Signature of Notified Authority

Dated :

Renewals

Received from M/S. __________________ a complete Memorandum of Intimation alongwith Form O, fee of Rs. _______________by Demand Draft bearing number ___________________________ dated ______________.

2. this acknowledgement shall be deemed to be the letter of authorisation entitling the applicant to carry on the business as applied for, for a period of

3 years from the date of issue of this Memo of acknowledgement unless suspended or revoked by the competent authority.

Dated : Signature of Notified Authority

EMBLEM

FORM 'B'

[See Clause 9]

Book No  Registration No.

Date of Issue

Valid upto

CERTIFICATE OF REGISTRATION TO CARRY ON thE BUSINESS OF SELLING FERTlLISERS AS A *INDUSTRIAL DEALER IN thE STATE OF

, is hereby granted certificate of registration to carry on the business of selling fertilisers in retail/ wholesale/ for industrial use at the place specified below in the State of ____________subject to the terms and conditions specified below and to the provisions of the Fertiliser (Control) Order,

1985.

DESCRIPTION OF thE PLACE AND TYPE OF BUSINESS

Name and style Location of Location Type of Source of by which the sale depot of godowns fertiliser supply business is attached to carried on sale depot

Date : Controller / Registering Authority

Seal : State of

Terms and conditions of certificate of registration:

(1)     this certificate of registration shall be displayed in a prominent and conspicuous place in a part of the business premises open to the public.

(2)     the holder of the certificate shall comply with the provisions of the Fertiliser (Control) Order 1985 and the notification issued thereunder for the time being in force.

(3)     the certificate of registration shall come into force immediately and be valid upto.

Unless previously cancelled or suspended

(4)     the holder of the certificate shall from time to time report to the Registering Authority any change in the premises of sale depot and godowns attached to sale depot.

(5)     the wholesale dealer/retail dealer shall submit a report to the Registering Authority, with a copy to the Block Development Officer or such other officer as the State Government may notify, in whose Jurisdiction the place of business is situated, by the 5th of every month, showing the opening stock, receipts, sales and closing stocks of fertilisers in the preceding month. He shall also submit in time such other returns as may be prescribed by the Registering Authority.

(6)     the Industrial dealer shall submit a report to the Central Government by the 15th of April for the preceding year, showing the opening stocks as on 1st of April of the reporting year, sourcewise receipts during the year, sale and closing stocks of fertilisers alongwith the sourcewise purchase/sale price.

(7)     the wholesale or the retail dealer, except where such a dealer is a State Government, a manufacturer, importer or a pool handling agency, shall not sell fertilisers for industrial use and, as the case may be, an industrial dealer for agricultural use.

Note : (a) the original is meant for the holder of the certificate which will be delivered against his proper and adequate acknowledgement. the original certificate of registration shall be torn off at the place perforated while all duplicates shall be kept intact bound in the registration book by the Registering Authority.

(b) Where the business of selling fertilisers is intended to be carried on at more than one place, a separate registration certificate should be obtained in respect of each such place.

(c) Where a person intends to carry on the business of selling fertilisers both in retail and wholesale and, as the case may be, a State Government, a manufacturer, importer or a pool handling agency, also for industrial use, separate registration certificate should be obtained for retail and wholesale business and for sale for industrial use.

EMBLEM

FORM 'C'

[See Clause 11]

APPLICATION FOR RENEWAL OF thE CERTIFICATE OFREGISTRATION TO CARRY ON thE BUSINESS OF SELLING

FERTlLISERS IN RETAIL/WHOLESALE / FOR INDUSTRIAL USE

To,

the Registering Authority/Controller (if the application is for Industrial dealer's certificate of Registration).

Place :

State :

1.        I/we hereby apply for renewal of the certificate of registration to carry on the business of selling fertilisers in retail/wholesale/ for industrial use under the name and style of ___________________________the Certificate of registration desired to be renewed was granted by Registering Authority for the____________________________(mention place and state) and allotted registration certificate No____________________ on the _______________Day of __________ 20________ .

2.        (i) I/we hereby declare that the situation of my/our premises where fertilisers are (a) stored and (b) sold is as stated below:

(ii) I/we hereby declare that the fertiliser(s) in which I/we am/are carrying on the business of selling and the name(s) of manufacturer(s) /importer(s), Commodity Board(s), State Govemment(s) and Wholesale Dealer(s) whom I/we represent are as stated below:

3.        I/we enclose a certificate of source from the manufacturer(s), importer(s), Commodity Board(s), State Government(s), Wholesale Dealer(s) whom I/we represent or intend to represent and from whom fertiliser(s) will be obtained by me/us.

4.        I have deposited the renewal fee of Rs. ___________vide challan No. ____________ dated ___________ in Treasury/Bank ______________ or I enclose the Demand Draft No. ______________dated ___________for Rs. ______________ drawn on _____________ Bank, in favour of __________ payable at _____________________ towards renewal fee (Please strike out whichever not applicable).

Full Name and address of the Signature of applicant(s)

applicant(s) (in block letters)

Date :

Place:

Certified that the certificate of registration bearing number ________________granted on_________ for the period from ___________________to ________________ to carry on the business of selling fertilisers in retail/wholesale/ for Industrial use at the premises situated at ________________is hereby renewed till the ___________ unless previously suspended or cancelled under the provisions of the Fertiliser (Control) Order 1985.

 

EMBLEM

FORM D

[See Clause 14(2), 14(2) (b) and 18(1)]

FORM OF APPLICATION TO OBTAIN A CERTIFICATE OF MANUFACTURE OF PHYSICAL/GRANULATED /SPECIAL MIXTURE OF FERTILISER OR ORGANIC

FERTILISER/BIOFERTILISER

To

The Registering Authority

Place___________________

State of_______________

(1)     Full name and address of the applicant:

 

(2)     Does applicant possess the qualification prescribed by the State Government under sub-clause(1) of clause 14 of the Fertiliser(Control) Order 1985.

 

(3)     Is the applicant a new comer? (say 'Yes' or 'No')

 

(4)     Situation of the applicant's premises where physical/granulated/special mixture of fertilisers/organic fertiliser/biofertiliser will be prepared.

 

(5)     Full particulars regarding specifications of the physical/granulated/special mixture of fertilisers/organic fertiliser/biofertiliser for which the certificate is required and the raw materials used in making the mixture.

 

(6)     Full particulars of any other certificate of manufacture, if any, issued by any other Registering Authority;

 

(7)     How long has the applicant been carrying on the business of preparing physical/granulated/special mixture of fertilisers/organic fertiliser/iofertiliser/mixture of micronutrient fertilisers?

 

(8)     Quantities of each physical /granulated/special mixture of fertilisers/ mixture of micronutrient fertilisers/ organic fertilisers/bio fertilisers (in tonnes) in my/our possession on the date of the application and held at different addresses noted against each;

 

(9)     (i) If the applicant has been carrying on the business of preparing physical/granulated/special mixtures of fertilisers/mixture of micronutrient fertilisers/organic fertiliser/biofertiliser, give all particulars of such mixtures handled, the period and the place (s) at which the mixing of fertilisers was done;

(ii) Also give the quantities of physical/granulated/special mixture of fertiliser/organic fertiliser/ biofertiliser handled during the past calendar year;

(10)   If the application is for renewal, indicate briefly why the original certificate could not be acted on within the period of its validity.

(11)   In case of special mixture of fertilisers

Name and address of the person requiring the special mixture of fertilisers;

Declaration

(a)      I have deposited the prescribed registration certificate fee/renewal fee.

 

(b)      I/we declare that the information given above is true and correct to the best of my/our knowledge and belief, and no part there is false.

 

(c)      I/we have carefully read the terms and conditions of the certificate of manufacture given in Form F appended to the Fertiliser (Control) Order, 1985 and agree to abide by them.

 

(d)      I/we declare that the physical/granulated /special mixture of fertilisers/organic fertiliser/bio fertiliser for which certificate of manufacture is applied for shall be prepared by me/us or by a person having such qualifications as may be prescribed by the State Government from time to time or by any other person under my/our direction, supervision and control or under the direction, supervision and control or person having the said qualification.

 

(e)      I/we declare that the requisite laboratory facility specified by the Controller, under this Order is possessed by me/us.

 

(f)       In case of special mixture of fertilisers:

I am enclosing an attested copy of the requisition made by the purchaser of the special mixture of fertilisers;

Name and address of applicant in block letters:

Date:

Place:

Signature of applicant(s)";

EMBLEM

FORM 'E'

[See Clause 14(2) (b)]

FORM OF APPLICATION TO OBTAIN A CERTIFICATE OF MANUFACTURE FOR SPECIAL MIXTURE OF FERTILISERS

To,

the Registering Authority

Place_______________ State ________________

(1)     Full name and address of the applicant:

 

(2)     Does the applicant possess qualifications prescribed by the State Government under sub-clause (1) of 14 of the Fertiliser (Control) Order, 1985.

 

(3)     Name and address of the person requiring the special mixture of fertilisers:

 

(4)     Particulars of certificate(s) of manufacture already obtained from the same Registering Authority:

 

(5)     Situation of the applicants premises where fertilisers are/will be mixed:

 

(6)     Full particulars regarding specifications of the special mixture of fertilisers required to be manufactured and the materials used in making the special mixture:

 

(7)     I am enclosing an attested copy of the requisition made by the purchaser of the special mixture of fertilisers:

 

(8)     I have deposited the prescribed registration certificate fee:

Declaration :

(a)      I/We declare that the information given above is true and correct to the best of my/our knowledge and belief, and no part thereof is false.

 

(b)      I/we have carefully read the terms and conditions of the certificate of manufacture given in Form "G' appended to the Fertiliser (Control) Order 1985 and agree to abide by them.

 

(c)      I/we declare that the special mixture for which a certificate of manufacture is applied for, shall be prepared by me/us or by a person having such qualifications as may be prescribed by the State Government from time to time or by any other person under my/our direction, supervision and control or under the direction, supervision and control of a person having the said qualifications.

 

(d)      I/we declare that the requisite laboratory facility specified by the Controller under this Order is possessed by me/us.

Name and Address of the applicant(s) Signature of the applicant(s)

in block letters:

Date:

Place:

EMBLEM

FORM F

[See clause 15(2) and 18(2)]

Book No. Certificate No.

Date of issue

Valid upto

CERTIFICATE OF MANUFACTURE IN RESPECT OF PHYSICAL/GRANULATED/SPECIAL

MIXTURE/ORGANIC FERTILISER/BIOFERTILISER

(Name of Manufacture) is hereby given the certificate for manufacture of physical/ granulated/special mixture of fertilizers/organic fertilizer/biofertiliser specified below subject to the terms and conditions of this certificate and to the provisions of the Fertiliser (Control) Order, 1985.

Terms and conditions of this certificate:

(1)     The holder of this certificate shall display the original thereof in a conspicuous place open to the public in a part of the principal's premises in which business of making the physical/ granulated /special mixture of fertilizers/organic fertilizer/biofertiliser is carried on and also a copy of such certificate in similar manner in every other premises in which that business is carried on. The required number of copies of the certificate shall be obtained on payment of the fee thereof.

 

(2)     The holder of this certificate shall not keep in the premises in which he carried on the business of making physical/ granulated/special mixture of fertilizers/organic fertilizer/biofertiliser in respect of which a certificate of registration has not been obtained under the Fertiliser (Control) Order, 1985.

 

(3)     The holder of the certificate shall comply with the provisions of the Fertiliser (Control) Order, 1985 and the notification order and direction, issued there under for the time being in force.

 

(4)     The holder of the certificate shall report forth with to the Registering authority any change in the premises specified in the certificate or any new premises in which he carried on the business of making physical /granulated/special mixture of fertilizers/organic fertilizer/biofertiliser and shall produce before the authority the original certificate and copies thereof so that necessary correction may be made therein by that authority.

 

(5)     The holder of this certificate shall ensure that the physical/granulated/special mixture of fertilizers/organic fertilizer/biofertiliser in respect of which a certificate of registration has been obtained in prepared by him or by a person having such qualifications as may be prescribed by the State Government, from time to time or by any other person under the direction, supervision land control of the holder or the person having the said qualifications.

 

(6)     The certificate and copies thereof, if any, will be machine numbered and delivered against the signature of the holder thereof or his agent on the carbon copy of the certificate which will be kept intact bound in the "Certificate Book" by each Registering Authority.

EMBLEM

[166][FORM-G

[See clause 20C(3)]

APPLICATION FOR INCLUSION OF BIOSTIMULANTS IN SCHEDULE VI

To,

The Controller of Fertiliser

-------------------------

------------------------

(i)       Name of manufacturer along with address of unit where it is located:

 

(ii)      Address of the Registered office of the company:

 

(iii)     Location and full address of storage/godown(s):

 

(iv)    Name and address of the applicant along with his designation, contact number and email ID:

 

(v)      PAN and Adhaar number of the authorized person:

 

(vi)    Name of biostimulant (indicate the category of biostimulant as specified in sub-clause (2) of clause 20C):

 

(vii)   Brand Name:

 

(viii)  In case of importer, following additional information shall be provided:

(a)      country of origin:

(b)      is biostimulant registered under country of origin (provide the copy):

(c)      whether the agronomic efficacy trials and toxicity trials are conducted in the country of origin:

(ix)    Technical details of product:

(x)      Labels and leaflet details:

(xi)    Quantity manufactured and sold during last three years (attach sale document):

Verification:-

I do hereby solemnly verify that to the best of my knowledge and belief the statement given above is correct and complete.

I clearly understand that the certificate of registration is liable to be canceled if any information or data, submitted with application is found incorrect or false at any stage.

Signature of the applicant

FORM-G-1

[See clause 20C(5)]

APPLICATION FOR PROVISIONAL REGISTRATION OF BIOSTIMULANTS

To,

The Controller of Fertiliser

-------------------------

------------------------

(i)       Name of manufacturer [167][or importer] along with address of unit where it is located:

 

(ii)      Address of the Registered office of the company:

 

(iii)     Location and full address of storage/godown(s):

 

(iv)    Name and address of the applicant along with his designation, contact number and email ID:

 

(v)      PAN and Adhaar number of the authorized person:

 

(vi)    Name of biostimulant (indicate the category of biostimulant as specified in sub-clause (2) of clause 20C):

 

(vii)   Brand Name:

 

(viii)  In case of importer, following additional information shall be provided:

(a)      country of origin:

 

(b)      is biostimulant registered under country of origin (provide the copy):

 

(c)      whether the agronomic efficacy trials and toxicity trials are conducted in the country of origin:

(ix)    Technical details of product:

(x)      Labels and leaflet details:

 

(xi)    Quantity manufactured and sold during last three years (attach sale document):

 

(xii)   Date and year when introduced in market:

 

(xiii)  State(s) in which product is sold:

Verification:-

I do hereby solemnly verify that to the best of my knowledge and belief the statement given above is correct and complete.

I clearly understand that the certificate of registration is liable to be canceled if any information or data, submitted with application is found incorrect or false at any stage.

Signature of the applicant

FORM-G-2

[See clause 20C(5)(b)]

(To be issued by the State Government(s))

This is to certify that M/s. is selling biostimulant (Name) brand name prior to the (date of publication of notification) and during last three years,-----metric ton/litre of biostimulant were sold in the state.

This is further certified that no complaint has so far been reported of ill effects or hazardous effects of the said biostimulant on humans as well as on animals or environment.

Director of Agriculture

FORM G-3

[See clause 20C(6)]

(To be issued by Controller)

Certificate of Provisional Registration

M/s. ....... (name) and (address) is hereby given the Certificate of Provisional Registration to manufacture [168][or importer] the biostimulant (Name) under sub-clause (6) of clause 20C of the Fertiliser (Inorganic, Organic or Mixed) (Control) Order, 1985, details of which are as under:--

1.        Name of the bio-stimulant:

 

2.        Brand Name of the bio-stimulant:

 

3.        Location of manufacturing unit:

 

4.        Place of storage:

 

5.        Certificate Registration Number:

The provisional registration shall be valid [169][upto 22nd day of February, [170][2025]].

The provisional registration shall be subject to the following terms and conditions:--

1.        The holder shall manufacture [171][or importer] only the biostimulant for which the registration is provided.

 

2.        The heavy metal content and Pesticide content shall not exceed the limit prescribed under the Order.

 

3.        The holder shall comply with the provisions of the said Order and notification issued thereunder.

 

4.        For selling of biostimulant, the authorization letter shall be obtained from the Notified Authority of the concerned State Government.

 

5.        Any information provided in Form G-1 if found incorrect, or on violation of any terms and conditions, the Controller of Fertiliser shall cancel the provisional registration.]

(Controller)

[172][FORM-G-4

[See clause 20D(3)]

APPLICATION FOR OBTAINING APPROVAL OF NANO FERTILISER UNDER THE FERTILISER

(INORGANIC, ORGANIC OR MIXED) (CONTROL) ORDER, 1985

To,

The Controller of Fertiliser

-------------------------

------------------------

1.        Name of manufacturer:

 

2.        Name of the nano fertiliser:

 

3.        Specifications:

 

4.        Details of Multi locational bio-efficacy trials:

(i)       Name of State Agricultural University/Institute of Indian Council of Agricultural Research:

 

(ii)      Crops:

 

(iii)     Details of locations:

5.        Details of Bio safety/Toxicology trials:

(i)       Whether trials have been conducted as per Department of Bio technology Guidelines on nano technology:

(ii)      Type of trial (as per Department of Bio technology guidelines on nano technology:

(iii)     Name of the NABL accredited laboratory where the trials are conducted:

List of documents attached:

(i)       Agronomic efficacy trials report:

(ii)      Bio-safety/Toxicology trials report:

Authorised Signature
On/or behalf of the ...........

EMBLEM

FORM H

[See Clause 23(1)(b)]

APPLICATION FOR GRANT OF PERMISSION TO SELL NON-STANDARD FERTILISERS

To,

The Notified Authority

State of ___________________________

(1)     Full name and address of the applicant:

(2)     The name of fertilisers in which the applicant has been authorized to carry on business:

(3)     Number and date of authorisation letter granted in favour of the applicant:

(4)     (i) Analysis Report by notified fertiliser control laboratory attached - Yes/No

(ii) The source from which the fertilisers were originally purchased and the period during which they have been held by the applicant.

I enclose a copy of the authorisation letter for dealing in fertilisers already granted to me and I have deposited the prescribed fee for permission to sell non-standard fertilisers.

I certify, that I will comply with the requirements of sub-clause (a) of clause 23 of the Fertiliser (Control) Order, 1985.

Signature of the applicant";

Name and address of applicant in block letters

Date : Place:

EMBLEM

FORM 'I'

[See Clause 23(1)(b)]

AUTHORISATION FOR THE SALE OF NON-STANDARD FERTILISERS

M/s. _______________________________________________is/are hereby permitted to sell the non-standard fertilisers described below subject to the terms and conditions noted hereunder.

Particulars of non-standard fertiliser

(1)     Name of the fertiliser:

(2)     Place of location of the non-standard fertiliser.

Terms and conditions:

(1)     The seller of the non-standard fertiliser described above shall comply with the provisions of sub-clause (a) of Clause 23 of the Fertiliser (Control) Order, 1985.

(2)     The non-standard fertilisers described above shall be sold at a price not exceeding Rs. per metric tonne.

[173][Form 'I-1'

[See clause 23 A]

APPLICATION TO GRANT CERTIFICATE FOR REPROCESSING OF DAMAGED FERTILIZER

To,

The Notified Authority

State of _______

1.        Full name and address of the applicant:

 

2.        The name of fertilizers which is damaged:

 

3.        Whether the material is indigenously manufactured or imported:

 

4.        Name of the Manufacturer/Importer:

 

5.        Name of the dealer with whom the material is stored or location of godown or warehouse where the material is stored:

 

6.        If the material is stored with dealer (wholesaler/retail dealer), provide the number and date of authorisation letter granted in favour of the dealer:

 

7.        Approximate quantity of damaged fertiliser and their number of bags:

 

8.        Address of the plant where the material is to be reprocessed:

 

9.        Whether the damaged material has been segregated:

 

10.     Whether the damaged material is conspicuously superscribed with the word 'Non-Standard' and also whether the "X' mark was marked on the bags of the material.

I enclose a copy of the authorization letter for the dealing in fertilizers already granted to me and I have deposited the prescribed fee for permission to reprocess the fertilizer damaged during storage.

I certify, that I have complied with the requirements of clause 23A of the Fertilizers (Control) Order, 1985 and no subsidy/assistance is availed on this material.

Signature of the applicant

Name and address of applicant in block letters

Form 'I-2'

[See clause 23 A]

CERTIFICATE FOR REPROCESSING OF FERTILISER DAMAGED DURING STORAGE

M/s. (Name of manufacturer/importer)________________ is/are hereby permitted to reprocess the fertiliser damaged during storage described below subject to the terms and conditions noted hereunder:-

1.        Name of the fertiliser:

 

2.        Name of the manufacturer/importer:

 

3.        Name and address of the dealer or godown or warehouse where the material is stored:

 

4.        Quantity of damaged fertiliser permitted to be reprocessed:

 

5.        Address/location of the plant where the material is to be reprocessed:

Terms and Conditions:

(1)     The material shall be moved within one week from the date permission is granted.

 

(2)     The company shall inform the Department of Fertiliser, Ministry of Chemical and Fertilisers/Government of India about reprocessing of fertiliser damaged during storage.

 

(3)     Before selling the same, the company shall ensure its quality/standards.

Date:

Notified Authority.
State of __________

Seal:]

EMBLEM

FORM J

[174][See clause 28(1)(b), 28(1)(ba), 28(1) (bb), 28(1)(bc) and 28(1)(bd)]

FORM INDICATING PARTICULARS OF FERTILISERS/ORGANIC FERTILISERS/BIO-FERTILSIERS SAMPLED

(1)     Name and address of dealer/manufacturer/importer [175][or Marketer]

(1A) Letter of authorisation number

(2)     Date of sampling

(3)     Details of markings on bags from where sample has been taken:

(i)       Type and grade of fertilizer

 

(ii)      Name of dealer/manufacturer/importer

 

(iii)     Batch No. (if applicable) and date of manufacture/import

 

(iv)    Composition

(4)     Date of receipt of the stock by the dealer/manufacture/importer/pool handling agency.

(5)     Code No. of sample

(6)     Stock position of the lot

(7)     Physical condition of fertilizer

(8)     Where samples drawn from open bags or stitched bags

(9)     Name & Address of Fertiliser Inspector drawing sample

Signature & Metallic Seal Impression of Fert. Inspector

Receipt of the dealer

Certified that the sample of fertilizer has been drawn in accordance with the procedure laid down in the Fertilizer (control) Order, 1985 from the stock of my possession and I have signed the test samples in the time of wax sealing. I have also received one test sample out of the three test samples prepared.

EMBLEM

FORM 'J-1'

[See clause 28 (bb)]

FORM INDICATING PARTICULARS OF

ORGANIC FERTILISER/ BIOFERTILISERS SAMPLED

(1)     Name and address of dealer/manufacturer/importer ______________

(1A) Certificate of Registration Number____________________

(2)     Date of sampling_______________________________

(3)     Details of markings of bags from where sample has been taken _________ ________________________________________________________

(i)       Type of organic fertiliser/biofertiliser ______________________

 

(ii)      Name of manufacturer/importer____________________________

 

(iii)     Batch No. (if applicable) and date of manufacture/import________

 

(iv)    Composition ___________________________

(4)     Date of receipt of the stock by the dealer/manufacturer/importer/pool handling agency_______________________________________

(5)     Code No. of sample_____________________________________

(6)     Stock position of the lot__________________________________

(7)     Physical condition of organic fertiliser/biofertiliser ________________

(8)     Whether samples drawn from open bags or stitched bags/with sealed packet_____________________

(9)     Name and Address of organic fertiliser/biofertiliser Inspector drawing sample______________________

For organic fertiliser

Signature and Metallic Seal

impression of Fertiliser Inspector

Receipt of the dealer

Certified that the sample of organic fertiliser/biofertiliser has been drawn in

accordance with the procedure laid down in the Fertiliser (Control) Order, 1985

from the stock in my possession, and I have signed the test samples at the time

of wax sealing. I have also received one test sample out of the three test samples

prepared.

Signature and Seal of

Fertiliser Inspector

Signature of dealer/manufacturer/

importer/pool handling agency

with address

EMBLEM

FORM K

[See clause 30(1)]

MEMORANDUM TO ACCOMPANY FERTILISER/ORGANIC FERTILISER/BIO-FERTILISER SAMPLE FOR

ANALYSIS

No.

From______________________

___________________________

To

Incharge

Fertiliser/ Organic Fertiliser/Bio-fertiliser Quality Control Laboratory

1.        The fertilizer samples as per details given below are sent for analysis:

(1)     Type of the fertilizer, Grade

(2)     Date of sampling__________________

(3)     Physical condition of fertilizer

(4)     Code number of sample

2.        The analysis report may please be forwarded to______________________________________

__________________________________________________________________________________________________________

Signature & Metallic Sea l Impression of Fert. Inspector

Place:

Date:

EMBLEM

FORM 'K-1'

[See clause 30]

MEMORANDUM TO ACCOMPANY ORGANIC FERTILISER/BIOFERTILISER

SAMPLE FOR ANALYSIS

No.

From

________________________________

________________________________

To,

Incharge

Organic fertiliser/Biofertiliser Quality Control Laboratory

1.        the biofertiliser samples as per details given below are sent for analysis:-

(1)     Name of organic fertiliser/biofertiliser _____________________

(2)     Date of sampling______________________________________

(3)     Physical condition of organic fertiliser/biofertiliser ____________

(4)     Code number of sample_________________________________

2.        the analysis report may be forwarded to__________________________

____________________________________________________________

Place:

Date:

Signature and metallic seal

impression of Fertiliser Inspector

EMBLEM

FORM 'L'

[See Clause 30(2)]

ANALYSIS REPORT OF FERTILISER SAMPLE

No.

Government of

(Name of the Laboratory)

Date

To,

the Fertiliser Inspector

………………………..

………………………..

the analysis report of the fertiliser sample forwarded vide your reference

No. …………………….... Dated ………………… is as per details given below :

(1)     Name of fertiliser, grade

 

(2)     Date of sampling

 

(3)     Omitted vide S.O. 49(E) dt.16.01.03

 

(4)     Code No. of sample as indicated by the Inspector

 

(5)     Date of receipt of the sample in the laboratory

 

(6)     Laboratory sample No

 

(7)     Date of analysis of sample

 

(8)     Chemical analysis of fertiliser (on fresh weight basis except in the case of Urea on dry weight basis)

____________________________________________________________________________________

Remarks :- the sample is/is not according to specifications and fails in......................

Signature of the Incharge

Fertiliser Quality Control Laboratory

Copy to :-

Director of Agriculture

EMBLEM

FORM 'L - 1'

(See clause 30 )

ANALYSIS REPORT OF ORGANIC FERTILISER SAMPLE

No.____________________

Government of _________________________

_____________________________________

_____________________________________

(Name of the Laboratory)

Date_____________________

To

the Fertiliser Inspector

____________________________________

____________________________________

the analysis report of the organic fertiliser sample forwarded vide your reference No.______________________________Dated_________________is as per details given below:

(1)     Name of Organic fertilizer

 

(2)     Date of Sampling

 

(3)     Code No. of sample as indicated by the Inspector

 

(4)     Date of receipt of the sample in the Laboratory

 

(5)     Laboratory sample No.

 

(6)     Date of analysis of sample

 

(7)     Analysis of Organic Fertiliser (on fresh weight basis)

(A)     Physical Characteristics -

(i)       Moisture content

 

(ii)      Bulk density

 

(iii)     Particle size

(B)     Chemical Characteristics -

(i)       Total Organic Carbon

 

(ii)      Total Nitrogen

 

(iii)     C:N

 

(iv)    Phosphorus

 

(v)      Potassium

 

(vi)    pH

 

(vii)   Conductivity

(C)     Heavy Metal

(i)       Cadmium

 

(ii)      Chromium

 

(iii)     Copper

 

(iv)    Mercury

 

(v)      Nickel

 

(vi)    Lead

 

(vii)   Zinc

Remarks : the sample is/is not according to specification and fails in__________

Signature of the Incharge

(Testing Laboratory

Copy to:-

Director of Agriculture

EMBLEM

FORM 'L - 2'

[See clause 30]

ANALYSIS REPORT OF BIOFERTILISER SAMPLE

No.

Government of

(Name of the Laboratory)

Date

To

the Fertiliser Inspector

the analysis report of the biofertiliser sample forwarded vide your reference

No.__________________________Dated_________________is as per details given below:

(1)     Name of Biofertiliser

 

(2)     Date of Sampling

 

(3)     Code No. of sample as indicated by by the Inspector

 

(4)     Date of receipt of the sample in the Laboratory

 

(5)     Laboratory sample No.

 

(6)     Date of analysis of sample

 

(7)     Analysis of biofertiliser (on fresh weight basis)

(A)     Physical Characteristics.

(i)       Moisture content

(ii)      Particle size

____________________________________________________________________________________

(B)     Chemical Characteristics

(i)       pH

____________________________________________________________________________________

(C)     Microbial Characteristics

(i)       Viable Cell Count

(ii)      Contamination Level

____________________________________________________________________________________

(D)     Efficiency Characteristics

(i)       Nodulation Test

(ii)      Nitrogen fixed (mg)/g of sucrose consumed

(iii)     Formation of transparent pellicle in semi solid Nitrogen free bromothymol blue media

(iv)    (a) Solubilization zone (mm)

(b) P- phosphorus (%) Spectro-photometer.

____________________________________________________________________________________

Rhizobium, ** Azotobacter, *** Azospirillum, + PSM

Remarks : the sample is/is not according to specification and fails in ___

___________________________________________________________

___________________________________________________________

Signature of the Incharge

(Testing Laboratory)

Copy to:-Director of Agriculture

EMBLEM

FORM 'L - 3'

[See clause 30]

ANALYSIS REPORT OF NON-EDIBLE DE-OILED CAKE FERTILISER SAMPLE

No.

Government of

(Name of the laboratory)

Date

To

the Fertiliser Inspector

the analysis report of the non-edible de-oiled cake fertiliser sample forwarded

vide your reference No. -------------dated---------------------- is as per details given below :

(1)     Name of Non-edible de-oiled cake fertilizer

 

(2)     Date of sampling

 

(3)     Code no. of sample as indicated by the inspector.

 

(4)     Date of receipt of the sample in the laboratory

 

(5)     Laboratory sample No.

 

(6)     Date of analysis of sample

 

(7)     Analysis of non-edible de-oiled cake fertilizer (on fresh weight basis

(A)     Physical Characteristics :

(i)       Moisture content ............................

(ii)      Particle size ...............................

(B)     Chemical Characteristics :

(i)       Total organic carbon

 

(ii)      Total nitrogen

 

(iii)     C:N

 

(iv)    Phosphorus

 

(v)      Potassium

 

(vi)    pH

 

(vii)   Conductivity

 

(viii)  Total ash

 

(ix)    Others

Remarks : the sample is/is not according to specification and fails in Signature of the incharge

(Testing Laboratory)

Copy to :

Director of Agriculture

EMBLEM

FORM 'M'

[See Clause 5]

FORM FOR CASH/CREDIT MEMORANDUM TO BE ISSUED BY thE DEALER/MANUFACTURER/IMPORTER/POOL

HANDLING AGENCY TO thE PURCHASER OF FERTILISERS

ST/CST No……………………….

Sl.No……………………… Date ………………………......

Certificate Registration No. …...........................………………..........…….

Name and Address of Firm : …...………………………………................…

Name and Address of Purchaser : …………………………….……........….

Total :

ST/CST @

G. Total

_______________________________________________________________________

Signature of purchaser

Signature of dealer, etc.

EMBLEM

FORM 'N'

[See Clause 35(1) (a)]

FORM FOR STOCK REGISTER TO BE MAINTAINED BY thE DEALER/ MANUFACTURER/IMPORTER/POOL

HANDLING AGENCY

Page Number : ___________

Name of the Fertiliser :_________________________________________

Date	Opening balance	Receipts During the day	Total	Sales During the day	Closing balance	Remarks	Signature of dealer
1	2	3	4	5	6	7	8

1.        Mention source of supply with bill No. and date

2.        Sl. No. of first and last cash/ credit memo issued

______________________________________________________________________________

Note : the pages of the stock register should be numbered. A Certificate should be recorded by the inspecting authority confirming the pages in the register.

EMBLEM

FORM 'O'

[See Clause 8 and 11]

CERTIFICATE OF SOURCE FOR CARRYING ON thE BUSINESS OF SELLING FERTILISERS IN

WHOLESALE/RETAIL FOR INDUSTRIAL USE

No. __________________ Date of issue ____________________

1.        Particulars of the concern issuing the certificate of source.

(a)      Name and full address

(b)      Status :

(i)       State Government

(ii)      Manufacturer

 

(iii)     Pool handling agency

 

(iv)    Wholesale dealer

 

(v)      Importer

(c)      If manufacturer of mixture of fertilisers, the details of certificate of manufacture of mixture of fertilisers possessed :

(i)       Number

 

(ii)      Date of issue

 

(iii)     Date of expiry

 

(iv)    Grades of mixturers of fertilisers allowed to be manufactured

 

(v)      Authority by whom issued

(d)      Details of certificate of registration :

(i)       Number

 

(ii)      Date of issue

 

(iii)     Date of expiry

 

(iv)    Authority by whom issued

2.        Particulars of the person to whom the certificate of source is being issued

(a)      Name and full address

(b)      Status :

(i)       Wholesale dealer

 

(ii)      Retail dealer

 

(iii)     Industrial dealer

(c)      If holds a valid certificate of registration, the details thereof :

(i)       Number

 

(ii)      Date of issue

 

(iii)     Date of expiry

 

(iv)    Authority by whom issued

(d)      Purpose of obtaining the certificate of source :

(i)       For obtaining a fresh certificate of registration

(ii)      For renewal of the certificate of registration

1.        Details of fertiliser(s) to be supplied :

S.No	Name of fertilisers	Trade mark/Brand name
1	2	3

_________________________________________________________________________________

4.    Declaration : Declared that the fertilisers mentioned above will be supplied conforming to the standards laid down under the Fertiliser (Control) Order, 1985 and, as the case may be, grades/formulations (of mixtures of fertilisers) notified by the Central/State Government and packed and marked in container as provided under clause 21 of the Fertiliser (Control) Order, 1985.

Signature with stamp of the

Authorised Officer

EMBLEM

FORM 'P'

[See Clause 28(1)(b)]

PARTICULARS OF SAMPLE DRAWN

1.        Name and Grade of Fertiliser :

 

2.        Composition :

 

3.        Physical Condition of Fertiliser :

 

4.        Code No. :

 

5.        Date of Sampling :

 

6.        Name & Address of Fertiliser Inspector drawing sample :

Signature and Metallic Seal

Impression of Fertiliser Inspector

Schedule III

[177][See clause (q)]

[178][Part A

SPECIFICATION OF BIOFERTILISER

1.        Rhizobium

2.        Azotobacter

3.        Azospirillum

4.        Phosphate Solubilising Bacteria

5.        Mycorrhizal Biofertilisers

6.        Potassium Mobilising Biofertilisers (KMB)

7.        Zinc Solubilising Bacteria

8.        Acetobacter

9.        Carrier Based Consortia

10.     Liquid Consortia

11.     Phosphate Solubilising Fungal biofertilisers

Part B

TOLERENCE LIMITS OF BIOFERTILIZER

1.        In case of Rhizobium, Azotobacter, Azospirillum Phosphate Solubilising Bacteria, Potash Mobilising Bacteria, Zinc Solubilising Bacteria, the total viable count shall not be less than 1x107   CFU/gm of carrier material in the form of powder or granules or 5x107   CFU/ml in case of liquid formulations.

2.        In case of Consortia, the total viable count shall not be less than 1x107   in case of carrier based and 1x108   in case of liquid formulations.

3.        In case of Mycorrhizal biofertilizers, total viable spores shall not be less than 8/gm of finished product.]

[186][PART C

'PROCEDURE FOR DRAWAL OF SAMPLE OF BIOFERTILISERS -

PROCEDURE FOR SAMPLING OF BIOFERTILIZERS', -

"1. General Requirements of Sampling -

1.0 In drawing, preparing and handling the samples, the following precautions and directions shall be observed.

1.1 Sampling shall be carried out by a trained and experienced person as it is essential that the sample should be representative of the lot to be examined.

1.2 Samples in their original unopened packets should be drawn and sent to the laboratory to prevent possible contamination of sample during handling and to help in revealing the true condition of the material.

1.3 Intact packets shall be drawn from a protected place not exposed to dampness, air, light, dust or soot."

2. Scale of Sampling -

2.1 Lot -

All units (containers in a single consignment of type of material belonging to the same batch of manufacture) shall constitute a lot. If a consignment consists of different batches of the manufacture the containers of the same batch shall be separated and shall constitute a separate lot.

2.2 Batch -

All inoculant prepared from a batch fermentor or a group of flasks (containers) constitute a batch.

2.3 For ascertaining conformity of the material to the requirements of the specification, samples shall be tested from each lot separately.

2.4 The number of packets to be selected from a lot shall depend on the size of the lot and these packets shall be selected at random and in order to ensure the randomness of selection procedure given in IS 4905 may be followed."

"3. Drawal of Samples

3.1 The Inspector shall take three packets as sample from the same batch. Each sample constitutes a test sample.

[187][3.2 Of the sample of biofertilisers drawn by the Inspector, the label affixed therein shall be defaced and a label containing generic name of bio fertilizers or organic fertilisers, expiry date, code number and date of sampling shall be pasted on the upper margin of sample packet/container. The sample shall be kept in cloth bag and be sealed with Inspector seal. The sealed cloth bag containing sample along with form 'P' shall be kept in another cloth bag and be sealed with inspector seal. The identifiable detail such as code number, date of sampling name of biofertiliser shall be put on cloth bag containing biofertiliser with form 'P'.

3.3 Out of three samples collected one sample so sealed shall be sent to Incharge of the laboratory notified by the State Government under clause 29 or the Director, National Centre of Organic Farming at Ghaziabad. In case where the sample is sent to Director National Centre of Organic Farming at Ghaziabad, or his authorized officer shall recode the sample and forward to any of the Regional Centre of Organic Farming at Bengaluru, Bhubaneshwar, Ghaziabad, Imphal, Jabalpur, Nagpur, and Panchkula for analysis. Another sample shall be given to manufacturer or dealer as the case may be. The third sample shall be sent by the inspector to the next higher authority for safe custody. The appellate authority shall be sent any of the latter two samples for referee analysis under sub-clause (2) of clause 29 B.]

3.4 The number of samples to be drawn from the lot

PART D

Method of Analysis of Biofertilisers

[188][1.C. Method of Analysis of Azospirillum Biofertilisers. 

1.        Apparatus: same as Rhizobium

2.        Reagents

3.        Medium

Use N-free semisolid medium (Nfb) of the following composition for preparation of MPN tubes

2.1.1 Trace element solution (g/litre)

 

2.2 Sterilization and preparation of MPN tubes -

2 2.1 Prepare Nitrogen free Bromothymol Blue malate medium as mentioned at paragraph 2.1. Boil to dissolve agar. Quickly dispense 10 ml molten media in 15 x 150 ml test tubes or screw capped culture tubes and close either with cotton plugs or screw caps. Minimum of 25 such tubes shall be needed for each sample.

2.2.2 Sterilize the tubes by autoclaving at 121°C for 20 minutes, as in Rhizobium at paragraph 2.3.2.

3. Preparation of serial dilution for MPN count -

Dispense 30 g of Azospirillum biofertilizers in 270 ml of sterile water and shake for 10 minutes on a reciprocal shaker. Make serial dilutions up to 10-8 dilution. Pipette out 1 ml aliquots of 10-4 to 10-8 dilution and deliver it to screw cap tubes or test tubes containing N-free semi solid Nfb media.

4. Incubation of tubes -

Label the tubes and incubate at 36 ± 1°C for 3-4 days in vertical position in a test tubes stand. Do not disturb the medium during the entire period of incubation.

5. Counting

5.1 Count the tubes which have turned blue and have developed typical transparent sub-surface pellicle.

5.2 Count the tubes as +ve or -ve for the presence of sub-surface pellicle and consider for the purpose of calculation.

5.3 Method for Estimating MPN Count

5.3.1 To calculate the most probable number of organisms in the original sample, select as P1 the number of positive tubes in the least concentrated dilution in which all tubes are positive or in which the greatest number of tubes is +ve, and let P2 and P3 represent the numbers of positive tubes in the next two higher dilutions.

5.3.2 Then find the row of numbers in Table 1 in which P1 and P2 correspond to the values observed experimentally. Follow that row of numbers across the table to the column headed by the observed value of P.

5.3.3 The figure at the point of intersection is the most probable number of organisms in the quantity of original sample represented in the inoculum added in the second dilution. Multiply this figure by the appropriate dilution factor to obtain the MPN value.

5.3.4 Azospirillum count/g of carrier = Value from MPN table* x Dilution level

  ___________________________________

   Dry mass of product

Table 1

*Most Probable Numbers for use with 10 fold dilution and 5 tubes per dilution (Cochran, 1950)

1D. Method of Analysis of Phosphate Solubilising Bacterial Biofertiliser

Determination of Soluble Phosphorus Using Ascorbic Acid

[189][5.33 Procedure

"(i) Preparation of Sample -

Pure culture medium same as at 2.1 above excluding agar.

Prepare broth medium in 100 ml aliquots in 6 no., 250 ml conical flasks and sterilize in autoclave at 121°C for 20 min.

(ii) Inoculation of Medium -

Select one PSB colony of the type that has been counted as PSB (showing sufficient zone of solubilization) and streak on set medium as described at 2.1 in a Petri dish. Use this pure culture for inoculating the broth. Inoculate 3 flasks and keep 3 flasks as uninoculated control. Incubate the flasks over rotary shaker for 12 days at 28 +.1°C. After 12 days, filter the contents of each flask separately through Whatman No. 42 filter paper or centrifuge at 10,000 rpm for 15 min.

(iii) Add 10 ml of filtrate/ centrifugate to 50 ml of olsen extractant and shake for 30 min over rotary shaker.

(iv) Filter the suspension through Whatman filter paper No. 40. If the filtrate is coloured then add a tea spoon of Dacro-60 (activated phosphorous free carbon), reshake and filter.

(v)   Take a known aliquot (5 to 25 ml) of the extract in a 50 ml volumetric flask.

(vi)   Add 5 drops of p-nitrophenol indicator (1.5 per cent solution in water) and adjust the pH of the extract between 2 and 3 with the help of 4NH2SO4. The yellow colour will disappear when the pH of the solution becomes 3. Swirl gently to avoid loss of the solution along with the evolution of CO2.

(vii)  When the CO2 evolution has subsided, wash down the neck of the flask and dilute the solution to about 40 ml.

(viii) Add 5 ml of the sulphomolybdic acid mixed reagent containing ascorbic acid, swirl the content and make up the volume.

(ix)   Measure the transmission after 30 min at 880 nm using red filter. The blue colour developed remains stable upto 60 minutes.

(x)   Record the concentration of phosphorous (P) in the extract form from the standard curve and calculate the concentration of soluble phosphorous as follows:]

1(E). Method of Analysis for Mycorhizal Biofertilisers

[190][(b) Procedure

(i)       Mix 100 gram Mycorrhizal biofertiliser in a substantial volume of water and decant through a series of sieves arranged in descending order of mesh size;

(ii)      Vigorous washing with water is necessary to free spores from aggregates of clay carrier material or organic materials;

(iii)     Roots and coarse debris are collected on coarse sieves (1mm and 450 micron), while spores are captured on all the respective finer sieves (250micron, 100 micron and 40/50 micron);

(iv)    Collect the sieving in jars and view the aliquots for spore count during continuous stirring on magnetic stirrer so that proper separation of spores and carrier could occur (as per suggestions from TERI experts);

(v)      Transfer aliquots from all the finer sieves (250 micron 100 micron and40/50micron) are mixed and observed properly on the gridded Petri dishes or plate under stereomicroscope for total viable spore count; and

(vi)    Count the number of spores in plate/dish and express it as spores or gram of the sample.]

[191][1F. Method of analysis for [192][Potash Mobilising Biofertilisers] (KSB)

Estimation of total viable count and contamination

1.        Apparatus -

1.1 Pippettes graduated 1 ml and 10 ml

1.2 Dilution bottles or flasks

1.3 Petri dishes clear, uniform, flat-bottomed

1.4 Hot -air oven

Capable of giving uniform and adequate temperature, equipped with a thermometer, calibrated to read upto 250øC and with venus suitably located to assure prompt and uniform heating.

1.5 Autoclave

1.6 Incubator

1.7 Hand tally or mechanical counting device

1.8 pH meter

2.        Reagents

2.1 Medium

Use plating medium of the following composition for total viable count and contamination

Medium for analysis of total viable count and contamination (Ingredients g/lit)

Medium for studying zone of solubilization in KSB(Ingredients g/lit)

2.2 Sterilizing and preparation procedure for plates

2.2.1 Sterlize the sampling and plating equipment with dry heat in a hot air oven at less than 160øC for not less than 2 hours;

2.2.2 Sterilize the media by autoclaving at 120øC for 20 min. To permit passage of steam into and from closed containers when auto claved, keep stoppers slightly lossened or plugged with cotton. Air from within the chamber of the sterilizer should be ejected allowing steam pressure to rise.

2.3 Preparation of plating medium and pouring

2.3.1 Prepare growth medium in accordance with the composition of the specific biofertiliser.

2.3.2 Melt the required amount of medium in boiling water or by exposure to flowing steam in partially closed container but avoid prolonged exposure to unnecessarily high temperature during and after melting. Melt enough medium which will be used within 3 h. Re-sterlisation of the medium may cause partial precipitation of ingredients.

2.3.3 When holding time is less than 30 min. promptly cool the molten medium to about 45øC, and store until used, in a water bath or incubator at 43 to 45øC. Introduce 12 to 15 ml of liquefied medium or appropriate quantity depending on size of the petri dish at 42 to 44øC into each plate. Gently lift the cover of the dish just enough to pour in the medium. Sterlise the lips of the medium containers by exposure to flame.

(a)      Immediately before pouring.

(b)      Periodically during pouring, and

(c)      When pouring is complete for each batch of plates, if portions of molten medium remain in containers and are to be used without subsequent sterilization for pouring additional plates. As each plate is poured thoroughly mix the medium with test portions in the petri dish.

2.3.4 By rotating and tilting the dish and without splashing the medium over edge, spread the medium evenly over the bottom of the plate. Provide conditions so that the medium solidifies with reasonable promptness (5-10 min) before removing the plates from level surface.

3.        Preparation of Serial Dilution for Plate Counts:

3.1. Dispense 10 g of inoculants to 90 ml of sterile distilled demineralized water and shake for 10 min on a reciprocal shaker or homogenizer. Make serial dilutions upto 10 Take 1:0 ml or suitable aliquots of 106 to 109 dilutions using sterile pipettes and deliver to petri dishes containing set medium as given in 2.1 and spread it uniformly with a spreader or use droplet method. Invert the plates and promptly place them in the incubator.

4.        Incubation of Plates:

4.1 Label the plates and incubate at 28 N2øC for 4 to 6 days.

4.2 Colony counting aids:

Count the colonies with the aid of magnifying lens under uniform and properly controlled, artificial illumination. Use a colony counter, equipped with a guide plate and rules in centimeter square. Record the total number of colonies with the hand tally. To distinguish colonies from dirt, specks and other foreign matter, examine doubtful objects carefully.

4.3 Count all plates but consider for the purpose of calculation plates showing more than 30 and less than 300 colonies per plate. Disregard colonies which absorb congo red and stand out as reddish colonies. Fraturia aurentia (KMB) stand out as transparent-opaque glistening and domed colonies. Count such colony numbers and calculate figures in terms of per litre, of carrier. Also check for freedom from contamination at 105 dilution.

5.        Counting

Count the total number of colonies on the plates including colonies with solubilisation zone with the help of a colony counter.

6.        Method for estimation of K solubilization zones

6.1 Take 10 g of KSB in 90 ml sterile distilled water

6.2 Make a tenfold dilution series up to 107.

6.3 Take 1.0 ml aliquot of 105 to 107 dilutions using sterile pipettes and deliver to petri dishes containing K-solubilization zone media.

6.4 Spread it uniformly, Invert the plates and incubate for up to 2 weeks at 28 N2øC.

6.5 Count the colonies showing solubilization zones and measure the diameter of solubilization zone. Calculate average zone of solubilization in mm.

[193][7. Method of Analysis for estimation of Potassium solubilisation:

Determination of soluble potash using Flame Photometer

1.        Preparation of Sample

Prepare Aleksandrov broth media comprising of 5.0g glucose; 0.5g MgSO4.7H2O; 0.1g CaCO3; 0.006g FeCl3; 2.0g Ca3(PO4)2; 3.0g potassium aluminium silicate in 1: 1 of distilled water. The pH of this media is adjusted to 7.2+0.2 by using 1 N NaOH. Prepare broth media in 100 ml aliquots in 6 no., 250 ml conical flasks and sterilize in autoclave at 121oC for 20 min.

2.        Inoculation of Media

Select one Potash Mobilising Biofertilisers colony of the type that has been counted as KSB (showing sufficient zone of solubilization) and streak on Aleksandrov agar medium as described above in a Petri dish. Use this pure culture for inoculating the broth. Inoculate 3 flasks and keep 3 flasks as uninoculated control. Incubate the flasks over rotary shaker for 7 days at 30+1oC.

3.        Determination of Soluble K.

(1)     After 7 days, centrifuge the broth at 10,000 rpm for 15 min. Collect the supernatant for estimation of potassium by Flame Photometer.

(2)     Add 1 ml of filtrate/supernatant to 50 ml volumetric flask and make up the volume to 50 ml. Estimate K content by feeding the solution to Flame Photometer. The amount of potassium solubilized is calculated from the standard curve by multiplying the observed value with dilution factor.

4.        Preparation of Standard curve.

(1)     Make a stock solution of 1000 ppm K by dissolving 1.909g. of AR grade potassium chloride (dried at 60oC for 1 h) in distilled water in a 1000 ml volumetric flask; and make up to 1 litre with distilled water. Prepare 100 ppm standard by diluting 100 ml of 1000 ppm stock solution to 1 litre with distilled water.

(2)     Pipette 0.5, 1.0, 1.5 and 2.0 ml of 100 ppm solution into 100 ml volumetric flasks and make up the volume up to the mark. These solutions contain 0.5, 1.0, 1.5 & 2.0 ppm K (mg/Kg) respectively. Plot standard curve using concentrations against flame photometer values.

Express K solubilized as mg/lit of broth]

[194][1G. Method of analysis for Zinc Solubilizing Biofertilizers

2. Estimation of total viable count and contamination

1.        Apparatus -

1.1 Pippettes graduated 1 ml and 10 ml

1.2 Dilution bottles or flasks

1.3 Petri dishes clear, uniform, flat-bottomed

1.4 Hot-air oven - Capable of giving uniform and adequate temperature, equipped with a thermometer, calibrated to read upto 250øC and with venus suitably located to assure prompt and uniform heating.

1.5 Autoclave

1.6 Incubator

1.7 Hand tally or mechanical counting device

1.8 pH meter

2.        Reagents -

2.1 Medium

Use plating medium of the following composition for total viable count and contamination

Medium for analysis of Total Viable Count, Contamination and zone of solubilisation for Zn solubilizing biofertilizer (Ingredients g/lit)

2.2 Sterilizing and preparation procedure for plates:

2.2.1 Sterlize the sampling and plating equipment with dry heat in a hot air oven at less than 160øC for not less than 2 hours;

2.2.2 Sterilize the media by autoclaving at 120øC for 20 min. To permit passage of steam into and from closed containers when auto claved, keep stoppers slightly lossened or plugged with cotton. Air from within the chamber of the sterilizer should be ejected allowing steam pressure to rise.

2.3 Preparation of plating medium and pouring

2.3.1 Prepare growth medium in accordance with the composition of the specific Biofertiliser.

2.3.2 Melt the required amount of medium in boiling water or by exposure to flowing steam in partially closed container but avoid prolonged exposure to unnecessarily high temperature during and after melting. Melt enough medium which will be used within 3 hours. Re-sterlization of the medium may cause partial precipitation of ingredients.

2.3.3 When holding time is less than 30 min. promptly cool the molten medium to about 45øC, and store until used, in a water bath or incubator at 43 to 45øC. Introduce 12 to 15 ml of liquefied medium or appropriate quantity depending on size of the petri dish at 42 to 44øC into each plate. Gently lift the cover of the dish just enough to pour in the medium. Sterlise the lips of the medium containers by exposure to flame.

a.        Immediately before pouring.

b.        Periodically during pouring, and

c.        When pouring is complete for each batch of plates, if portions of molten medium remain in containers and are to be used without subsequent sterilization for pouring additional plates. As each plate is poured thoroughly mix the medium with test portions in the petri dish.

2.3.4 By rotating and tilting the dish and without splashing the medium over edge, spread the medium evenly over the bottom of the plate. Provide conditions so that the medium solidifies with reasonable promptness (5-10 min) before removing the plates from level surface.

3.        Preparation of Serial Dilution for Plate Counts:

3.1 Dispense 10 g of inoculants to 90 ml of sterile distilled de-mineralized water and shake for 10 min on a reciprocal shaker or homogenizer. Make serial dilutions upto 1010 Take 1.0 ml or suitable aliquots of 106 to 109 dilutions using sterile pipettes and deliver to petri dishes containing set medium as given in 2.1 and spread it uniformly with a spreader or used droplet method. Invert the plates and promptly place them in the incubator.

4.        Incubation of Plates:

4.1 Label the plates and incubate-at 28 N2øC for 4 to 6 days.

4.2 Colony counting aids:

Count the colonies with the aid of magnifying lens under uniform and properly controlled, artificial illumination. Use a colony counter, equipped with a guide plate and rules in centimeter square. Record the total number of colonies with the hand tally.

4.3 Count all plates but consider for the purpose of calculation plates showing more than 30 and less than 300 colonies per plate. Disregard colonies which absorb congo red and stand out as reddish colonies. Zinc solubilising biofertilisers stands out as transparent, translucent, glistening and elevated colonies. Count such colony numbers and calculate figures in terms of per litre, of carrier. Also check for freedom from contamination at 105 dilution.

5.        Counting -

Count the total number of colonies on the plates including colonies with solubilization zone with the help of a colony counter.

6.        Method for estimation of Zinc solubilisation zones.

6.1 Take 10 g of ZSB in 90 ml sterile distilled water

6.2 Make a tenfold dilution series up to 107.

6.3 1.0 ml aliquot of 105 to 107 dilutions using sterile pipettes and deliver to petri dishes containing Zinc - solubilization zone media.

6.4 Spread it uniformly, Invert the plates and incubate for up to 2 weeks at 28 N2øC.

6.5 Count the colonies showing solubilization zones and measure the diameter of solubilization zone. Calculate average zone of solubilization in mm.]

[195][7. Determination of soluble Zinc using Atomic Absorption Spectrophotometer

(1)     Preparation of Sample

Prepare Zinc solubilizing broth media comprising of glucose-10.0g; ammonium sulphate-1.0g; potassium chloride-0.2g, dipotassium hydrogen phosphate-0.1g, magnesium sulphate-0.2g and zinc carbonate/zinc oxide 1gm in 1:1 of distilled water. The pH of this media is adjusted to 7.0 by using 1 N NaOH. Prepare broth media in 100 ml aliquots in 6 no., 250 ml conical flasks and sterilize in autoclave at 121oC for 20 min.

(2)     Inoculation of Media

Select one ZnSB colony of the type that has been counted as ZnSB (showing sufficient zone of solubilization) and streak on ZnSB agar media as described above in a Petri dish. Use this pure culture for inoculating the broth. Inoculate 3 flasks and keep 3 flasks as uninoculated control. Incubate the flasks over rotary shaker for 7 days at 30+1oC.

(3)     Determination of Soluble Zinc.

(a)  After 7 days, centrifuge the broth at 10,000 rpm for 15 min. Collect the supernatant for estimation of solubilized Zinc.

(b)  Add 1 ml of filtrate/supernatant to 50 ml volumetric flask and make up the volume to 50 ml. Estimate Zn content by feeding the solution to Atomic Absorption Spectrophotometer. The amount of zinc solubilized was estimated by subtracting the soluble zinc of the inoculated sample from the uninoculated control.

(c)  Standard curve should be made by diluting 0.5, 1.0, 1.5, 2.0 and 3.0 ml of 100ppm standard stock solution (commercially available) of Zinc Sulphate with doubled distilled water in volumetric flasks and make up the volume to 100ml to obtain standards having concentrations of 0.5, 1.0, 1.5, 2.0, 3.0 ppm.

(d)  The amount of zinc solubilized is calculated from the standard curve by multiplying the observed value with dilution factor (50).

Express Zn solubilized as mg/lit of broth.]

[196][1 H Methods of analysis for Acetobacter (spp).

1.        Appartus-As specified in the Method of Analysis of Rhizobium at serial number 1. A.

2.        Reagents.

2.1 Medium: Use plating medium of the following composition for total viable count and contamination:-

Medium for analysis of total viable count and contamination (ingredients gram/litre)

3.        Sterilising and preparation procedure for plates

(Same as specified in the Method of Analysis of Rhizobium)

3.1 Preparation of plating medium and pouring

(Same as specified in the Method of Analysis of Rhizobium.)

4.        Preparation of serial dilutions for plate counts

(Same as specified in the Method of Analysis of Rhizobium)

5.        Incubation of plates

(Same as specified in the Method of Analysis of Rhizobium)

5.1 Colony counting Aids

Count the' colonies with the aid of magnifying lens under uniform and properely controlled, artifical illumination. Use a colony counter, equipped with guide plate and rules in centimeter square. Record the total number of colonies with hand tally. Avoid mistaking particles of undissolved medium or precipitated matter in plates for pin point colonies. To distinguish colonies from dirt, specks and foreign matter, examine doubtful objects carefully

5.2 Count all plates but consider for the purpose of calculation only those plates showing more than 30 and less than 300 colonies per plate. Acetobacter a nitrogen fixing bacteria stand out as irregular 2-3 mm diameter, smooth flat with bright yellow or yellow with orange centre colour. Count such colony numbers and calculate figures in terms of per litre, of carrier. Also check freedom from contamination at 105.

6.        Test for confirmation.

1.        Appartus (same as specified in the Method of Analysis of Azospirillum at serial number 1C).

2.        Reagent.

2.1 Medium (semi solid for pellicle formation) (ingredients gm per liter)

3.        Sterilization and preparation of MPN tubes

(Same as specified in the Method of Analysis of Azospirillum at serial number 1C)

4.        Preparation of serial dilution for MPN count

(Same as specified in the Method of Analysis of Azospirillum at serial number 1C)

5.        Incubation of tubes

(Same as specified in the Method of Analysis of Azospirillum at serial number 1C)

6.        Counting-Yellowish pellicle formation below 1 mm of upper surface of nitrogen free semi solid media. Counting the tubes or plates which have turned yellowish in colour after inoculation and ascertained the presence of pellicle in undistributed medium. To determine usual contamination on the same examine doubtful objects carefully.

7.        Method for Estimating MPN count

Count all tubes which have turned yellowish and consider them for the purpose of calculation. Count such type of tubes and tally this count with MPN table (as specified in the Method of Analysis of Azospirillum at serial number 1C in Table 1) to get the number of cells per gram of carrier or number of cells per ml of liquid.]

[197][1.I. Method of analysis of carrier based Consortia of Biofertiliser and liquid consortia of Biofertiliser

(I)      Methods of Analysis of Rhizobium Biofertiliser - Same as specified for Rhizobium at Serial number 1.A.

(II)     Methods of Analysis of Azotobacter - Same as specified for Azotobacter at serial number 1B

(III)   Methods of Analysis Azospirillum - Same as specified for Azospirillum at serial number 1C

(IV)   Methods of Analysis of Phosphate Solubilising Bacteria PSB - Same as specified for Phosphate Solubilising Bacteria at serial number 1 D

(V)     Methods of Analysis of Potash Mobilising Bacteria (KMB) - Same as specified for Phosphate Solubilising Bacteria at serial number 1 F]

 

SCHEDULE IV

[see clause 2(h) and (q)]

[198][PART - A

1.        City compost:

 

2.        Vermicompost:

3.        [205][Phosphate Rich Organic Manure (PROM)

4.        [206][Organic Manure

Note: The source of organic manure is any of the plant biomass/animal biomass/animal Excreta.]

5.        [210][Bio-enriched Organic Manure

6.        [213][Bone meal, raw

7.        Bone meal, steamed

8.        [214][Potash derived from Rhodophytes

9.        [215][Fermented Organic Manure

[220][Note:- Every manufacturer shall categorically indicate on bags that Fermented Organic Manure shall be added 15-25 days prior to sowing of crop in the field.']

10.    [221][Liquid Fermented Organic manure

[225][Note:-Every manufacturer shall categorically indicate on container that Liquid Fermented Organic Manure shall be added 15-25 days prior to sowing of crop in the field.]

Part- B

TOLERANCE LIMIT OF ORGANIC FERTILISER

[226][A sum total of nitrogen, phosphorus and potassium nutrients shall not be less than 1.5% in City Compost and shall be not less than 2.5% in case of vermicom post]

GRANT OF PERMISSION FOR USE OF FERTILISIER FOR INDUSTRIAL PURPOSE.

The manufacturer of industrial product who intend to use fertilizer as raw material for manufacturing the product may apply to the Central Government in the Proforma I (appended below) along with the recommendation from the State Government/Central Government/ District Industry Centre of the concern State.

PROFORMA - I

Signature of Authorized Signatory

Document to be attached

1.        Application in prescribed proforma.

2.        Certificate from the Chartered Accountant of fertilizer purchase/consum for industrial use.

3.        Recommendation from the State Government/ Central Government/ District Industry Centre of the concerned State Government.

4.        GRANT OF CERTIFICATE OF REGISTRATION FOR SALE OF FERTILISER FOR INDUSTRIAL PURPOSE-

Under Clause 8 of Fertiliser (Control) Order, 1985 for Certificate of Registration is granted for carrying on the business of selling of Fertiliser for industrial purpose.

For this purpose the application is required to be made to Controller of fertilizer in prescribed Form 'A' (appended below) together with fee of Rs. 1500/- and certificate of source in Form 'O' issued by the manufacture of fertilizer.

Currently, the Government of India is granting industrial dealership for sale of Urea only.

[227][PART D

METHODS OF ANALYSIS OF ORGANIC FERTILISERS

1.        Estimation of pH

Make 25 g of compost into a suspension in 50ml of distitled water and shake on a rotary shaker for 2 hours.

Filter through Whatman No. 1 or equivalent filter paper under vacuum using a Buchner funnel.

Determine pH of the filtrate by pH meter.

2.        Estimation of Moisture

Method :

Weigh to the nearest mg about 5 gm of the prepared sample in a weighed clean, dry Petri dish. Heat in an oven for about 5 hours at 65° +. 1° c to constant weigh, Cool in a desicator and weigh. Report percentage loss in weight as moisture content.

Calculation

A = Weight of the Petri dish

B = Weight of the Petri dish plus material before drying

C = Weight of the Petri dish plus material after drying

3.        Estimation of Bulk density

Method

Weigh a dry 100ml cylinder (W 1 gill)

Cylinder is filled with the sample upto the 100 ml mark. Note the volume (VI ml)

Weigh the cylinder along with the sample (W2gm)

Tap the cylinder for two minutes.

Measure the compact volume (V2 ml).

4.        Estimation of Electrical Conductivity

Method

Pass fresh sample of organic fertilizer through a 2-4 mm sieve.

Take 20gm of the sample and add 100ml of distitled water to it to give a ratio of 1:5.

Stir for about an hour at regular intervals.

Calibrate the conductivity meter by using 0.01M potassium chloride solution.

Measure the conductivity of the unfiltered organic fertilizer suspension.

Calculation

Express the results as millimho's or ds/cm at 25°C specifying the dilution of the organic fertilizer suspension viz., 1:5 organic fertilizer suspension.

5.        Estimation of Organic Carbon

Apparatus

(i)       Silica/Platinum crucible 25 g cap.

(ii)      Muffle Furnace

Procedure

Accurately weigh 10 gm of sample dried in oven at 105°C for 6 hrs, in a pre weighed crucible and ignite the material in a Muffle furnace at 650 - 700°C for 6-8 hrs. Cool to room temperature and keep in Desiccator for 12 hrs.

Weigh the contents with crucible

Calculation

Calculate the total organic carbon by the following formulae:-

6.        Estimation of total Nitrogen

As mentioned under Schedule - II, Part-B, 3 (v) of FCO, 1985.

7.        Estimation of C: N Ratio

Method

Calculate the C:N ratio by dividing the organic carbon value with the total nitrogen value.

8.        Estimation of phosphate

Preparation of sample - Accurately weigh 10 gm oven dried sample in 50 g cap. silica crucible and ignite it to 650° - 700°C for 6-8 hrs to obtain ash. Cool and keep in a Dessicator.

Transfer the contents to a 100 ml beaker. Add 30 ml 25% HCl. Wash the crucible with 10 ml 25% HCl twice and transfer the contents to Beaker. Heat over hot plate for 10-15 min. Keep for 4 hrs. Filter through Whatman No. 1 filter paper. Wash with distilled water 4-5 times (till acid free).

Make up the volume of filtrate to 250 ml in a volumetric flask.

Estimate total P by gravimetric quinoline molybdate method as described under Schedule -II, Part B,4(ii)of FCO 1985.

9.        Estimation of Potassium

Flame photometry method:- Total Potassium are usually determined by dry ashing at 650-700 Degree Centigrade and dissolving in concentrated hydrochloric acid. Reagent and Standard curve

(1)     Potassium chloride standard solution: Make a stock solution of 1000 ppm K by dissolving 1.909 g. of AR grade potassium chloride (dried at 60 Degree C. for 1 h) in distilled water 1; and diluting up to 1 litre. Prepare 100 ppm standard by diluting 100 ml of 1000 ppm stock solution to 1 litre with extracting solution.

(2)     Standard curve: Pipette 0,5, 10,15 and 20 ml of 100 ppm solution into 100 ml volumetric flasks and make up the volume upto the mark. The solution contain 0,5, 15 & 20 ppm K respectively.

Procedure:

Take 5g sample in a porceline crucible and ignite the material to ash at 650-700 C in a muffle furnace.

Cool it and dissolve in 5 ml concentrated hydrochloric acid, transfer in a 250 ml beaker with several washing of distilled water and heat it. Again transfer it to a 100 ml volumetric flask and make up the volume.

Filter the solution and dilute the filtrate with distilled water so that the concentration of K in the working solution remains in the range of 0 to 20 ppm, if required.

Determine K by flame photometer using the K- filter after necessary setting and calibration of the instrument.

Read similarly the different concentration of K of the standard solution in flame photometer and prepare the standard curve by plotting the reading against the different concentration of the K.

Calculation: Potash (K) %by weight = R X 20 X diluting factor, where R= ppm of K in the sample solution (obtained by extra plotting from stand curve).

10.    Estimation of Cadmium, Copper, Chromium, Lead, Nickel and Zinc

Material Required

1.        Triacid mixture: Mix 10 parts of HNO3 (Nitric acid), 1 part of H2SO4
(Sulphuric Acid) and 4 parts of HClO3 (Perchloric Acid)

2.        Conical flask, 250ml

3.        Hot plate

4.        Whatman filter paper No. 42

5.        Atomic Absorption Spectrophotometer

Processing of sample

Take 5.0 g or suitable quantity of oven dried (105°C) sample thoroughly ground and sieved through 0.2 mm sieve in a conical flask.

Add 30 ml triacid mixture, cover it with a small glass funnel for refluxing. Digest the sample at 200°C on a hot plate till the volume is significantly reduced with a whitish residue.

After cooling, filter the sample with Whatman No. 42 filter paper, make up to 100 ml in a volumetric flask.

Preparation of working standards

Cadmium - As mentioned under Schedule - II, Part B, 8(x) of FCO (1985)

Copper - As mentioned under Schedule - II, Part B, 8(iv) of FCO (1985)

Chromium - Dilute 1, 2, 3 and 4 ml of standard 199 ppm Chromium standard solution with doubled distilled water in volumetric flasks and make up the volume to 100 ml to obtain standards having concentrations of 1, 2, 3, 4 ppm

Lead - As mentioned under Schedule - II, Part B, 8(v) of FCO (1985) Nickel - Dilute 1,2,3 and 4 ml of standard 100 ppm Nickel standard solution with doubled distilled water in volumetric flasks and make up the volume to 100ml to obtain standards having concentrations of 1,2,3,4 ppm

Zinc - As mentioned under Schedule - II, Part B, 8(ii) of FCO (1985)

Measurement of Result

Estimate the metal concentrations of Cd, Cu, Cr, Fe, Pb, Ni, Zn by flaming the standard solution and samples using atomic absorption spectrophotometer (AAS) as per the method given for instrument at recommended wavelength for each element. Run a blank following the same procedure.

Expression of Result

Express the metal concentration as mg/g on oven dry weight basis in 3 decimal units.

(Reference: Manual for Analysis of Municipal Solid Waste (compost): Central Pollution Control Board)."

11.    'Estimation of Mercury

Reagents:

(a)      Concentrated Nitric acid (HNO3)

(b)      Concentrated Sulphuric acid (H2SO4)

(c)      Potassium persulphate (5% solution): Dissolve 50g of K2S2O8 in 1 litre of distilled water.

(d)      Potassium permagnate (5% solution): Dissolve 50g of KMnO4 in 1 litre of distilled water.

(e)      Hydroxylamine sodium chloride solution: Dissolve 120 g of Hydroxyl amine salt and 120 g of sodium chloride (NaCI) in 1 litre distilled water.

(f)       Stannous chloride (20%): Dissolve 20 g of SnCI2 in 100 ml distilled water.

Materials required

(a)      Water bath

(b)      Flameless atomic absorption spectrophotometer or cold vapour mercury analyzer.

(c)      BOD bottle, 300 ml

Processing of sample:

(a)      Take 5g (finely ground but not dried) sample in an oven at a temperature of 105°C for 8 hours for moisture estimation.

(b)      Take another 5g sample (finaly ground but not dried) in a BOD bottle, add to it 2.5 ml of conc. HNO3, 5ml of cone. H2SO4 and 15 ml of 5% KMnO4.

(c)      After 15 minutes add 8 ml of 5% K2S2O8.

(d)      Close the bottle with the lid and digest it on a water bath at 95°C for 2 hours.

(e)      After cooling to room temperature add 5 ml hydroxylamine sodium chloride soln.

Measurement:

Reduction of the digested sample is brought out with 5 ml of 20% SnCl2 immediately before taking the reading, using a cold vapour mercury analyzer.

Expression of results:

Express the mercury concentration as mg/g on oven dry weight basis in 3 decimal units.

(Reference: Manual for Analysis of Municipal Solid Waste (compost). Central Pollution Control Board).

12.    Estimation of Arsenic

Processing of sample - Suspend 10 gm finely ground sample in 30 ml aquaregia (HNO3 + HCl in a ratio of 1:3) in a beaker. Keep on hot plate till moist black residue is obtained (do not dry). Add 5 ml aquaregia and allow to dry on hot plate till residue is moist. Dissolve the residue in 30 ml conc. HCl and filter through Whatman No.1 filter paper in 100 ml volumetric flask. Wash filter paper 3-4 times with double distilled water. Make up the volume to 100 ml. Take 1 ml of this solution in 100 ml volumetric flask, add 5ml conc. HCl and 2 gm KI and make up the volume to 100 ml.

Prepare standards having concentration of 0.05, 0.1 and 0.2 ppm by diluting 0.05, 0.1 and 0.2 ml, respectively of standard Arsenic solution with double distilled water in volumetric flask and make up the volume to 100 ml

Measurement - Estimate Arsenic using vapour generation assembly attached to Atomic Absorption Spectrophotometer as per the procedure given for the instrument.

13.    Pathogenicity Test

Apparatus

1.        Samples of Compost

2.        Lactose Broth of Single and Double Strength

3.        Culture Tubes

4.        Durham Tubes

5.        Bunsen Burner

6.        Sterile Pipettes

7.        Incubator, Autoclaves,

8.        Petri-Plates

9.        Inoculation Loops

Preparation of Culture Media

A.       For Presumptive Test

1.        Lactose Broth

B.       For Confirmative Test

1. Eosine Methylene Blue Agar Media (EMB Media)

C.        For Completed Test

1. Nutrient Agar

Procedures

A.       Presumptive Test

1.        Prepare 12 tubes of lactose broth for each sample and close the tube with cotton plugs/caps and autoclave at 121°C for 20 min.

2.        Fill Durham tubes with sterilized distilled water and keep in beaker and autoclave at 121°C for 20 min.

3.        Suspend 30g of compost sample in 270 ml of sterile distilled water and serially dilute upto 10-4 dilution as per Schedule III, Part D, serial number 3 of FCO (1985)

4.        Suspend 1 ml suspension from 10-1 to 10-4 in 3 tubes for each dilution

5.        Insert distilled water filled Durham tube in inverted position in each tube and close the tube again

6.        Inoculate tubes at 36°C for 24h in incubator

Result

B.       Confirmative Test

Confirmative test is for differentiating the coliforms from non-coliforms as well as Gram negative and Gram positive bacteria. In this test, the EMB agar plates are inoculated with sample from positive tubes producing gas. Emergence of small colonies with dark centres confirms the presence of Gram negative, lactose fermenting coliform bacteria. Sometimes some of the non-coliforms also produce gas, therefore, this test is necessary.

1.        Prepare EMB agar plates with the composition as per the method at Schedule III, Part D, paragraphs 2.3.3 to 2.3.6

2.        Inoculate plates with the help of inoculation loop with streaking of samples showing positive/doubtful tests in the presumptive test

3.        Incubate plates at 30 ± 1°C for 12 h in incubator

4.        Dark centred or nucleated colonies appear which may differentiate between E. coli and E. aerogenes based on size of colonies and metallic sheen

Result

E. coli colonies on this medium are small with metallic sheen, where as E. aerogenes colonies are usually large and lack the sheen.

C. Completed Test

This test is required for further confirmation. Procedure

1.        Pick up a single colony from EMB agar plate

2.        Inoculate it into lactose broth and streak on a nutrient agar slant

3.        Incubate the slants

4.        Perform Gram reaction after attaining the growth

Result

Gram-negative nature of bacteria is indicative of a positive completed test.]

14.    [228][Method of analysis of Bone Meal Raw and Bone Meal Steamed

(i)       Acid insoluble matter:

(a)      Reagent

Dilute Nitric Acid-1:1 (v/v)

(b)      Procedure

Weigh accurately about 2 to 3g of the sample into a crucible and ignite gently until all organic matter is burnt away, leaving behind grey or transparent ash. Cool and extract the residue twice with warm dilute nitric acid. Filter through a filter paper (Whatman No. 40 or equivalent) and wash the residue on the filter paper with water. Dry the residue in an air-oven at 150 + 2oC for one hour. Incinerate the filter paper with the residue to constant weight in a previously weighed crucible, cool in a desiccator and weigh.

(c)      Calculation

Acid-insoluble matter, percent by weight = 

where

W1 = weight in g of the residue, and

W2 = weight in g of the prepared sample taken for the test.

Note: Indian Standard Specification for Bone Meal Raw (Revised), Fourth Reprint April 1998, by Bureau of Indian Standards

(ii)      Total Phosphorus:

(a)      Preparation of sample

Accurately weigh 1g sample and transfer it to 100 ml beaker. Add 30 ml HNO3 and 10 ml concentrated HCl. Heat over hot plate for 10-15 mins or till the brown fumes disappears. Keep for 4 hrs. Filter through Whatman No. 42 filter paper. Wash with distilled water 4-5 times (till acid free). Make up volume of filtrate to 250 ml in a volumetric flask.

(b)      Estimate total P by gravimetric quinoline molybdate method as described under Schedule-II, Part B, 4(ii) of Order, 1985.

(iii)     Citric acid soluble phosphorus:

(a)      Reagents

Citric Acid solution: To dissolve 20g of citric acid in water and make up the volume to 1 litre.

(b)      Preparation of sample

(a)      Accurately weigh 5g of the sample into a 500-ml dry flask. Make up the volume to 500-ml mark with citric acid solution. Close the flask with a suitable stopper, place it at once in rotary shaking apparatus and shake the flask at the rate of 30 to 40 rev/min for 30 minutes. At the end of this period, remove the flask, filter the solution through a dry filter paper (Whatman No. 42) into a clean dry container.

(b)      Estimate P by gravimetric quinoline molybdate method as described under Schedule-II, Part B, 4(ii) of Order, 1985.

(iv)    Nitrogen content of water insoluble portion:

Preparation of sample

Accurately weigh 1g sample into a clean beaker. Stir well with water for a few minutes and filter through a filter paper (Whatman No. 2 or equivalent). Complete the washing until filtrate measures 200-250 ml. Carefully put the filter paper containing the residue into a 500-ml Kjeldahl flask.

Note: Determine N as Schedule-II, Part B, 3 (iv) of Order, 1985.

15.     Potash Derived from Rhodophytes

(i)       Water soluble Potash:

As mentioned for mixed fertilisers under Schedule-II, Part-B, paragraph 5 of Order, 1985.

(ii)      Determination of Sulphate Sulphur

As mentioned under Schedule-II, Part-B, paragraph 24 (A) Procedure (a) of Order, 1985.

(iii)     Determination of elemental sulphur

As mentioned under Schedule-II, Part-B, paragraph 24 (B) of Order, 1985.

(iv)    Total sulphur (as S) (It is the sum of sulphur present in sulphate and elemental form)

As mentioned under Schedule-II, Part-B, paragraph 24 (C) of Order, 1985.]

[229][SCHEDULE V

See clause 2 (h) and (q)

Part -A

Specification of Non-edible De-oiled Cake Fertilizers

[230][Note.-A company can sell the deoiled cake under its source name as Castor, Neem, Karanj (Pongamiapinnata), Mahua (madhucalongifolia) and Jatropha deoiled cake and can also print any specification of nutrient content over and above the minimum specification of nutrient prescribed under the general specifications of Non edible deoiled cake specified in FCO.]

Part-B

TOLERANCE LIMIT OF NON-EDIBLE DE-OILED

CAKE FERTILISERS

0.5 Unit for Nitrogen, Phosphorous and Potassium nutrients combined.

Part- C

PROCEDURE FOR DRAWL OF SAMPLE OF NON-EDIBLE DE-OILED CAKE FERTILISER

The Inspector shall draw any sample of Non-edible de-oiled cake fertilizer in accordance with the procedure of drawl mentioned under Schedule-II, Part-A.

Part- D

METHODS OF ANALYSIS FOR NON-EDIBLE DE-01LED CAKE FERTILIZERS

1.        Estimation of pH

As mentioned in Schedule IV Part D at serial number 1.

2.        Estimation of moisture

As mentioned in Schedule IV Part D at serial number 2.

3.        Estimation of ash Content

(a)      Apparatus

(i)       Silica/Platinum crucible 25 g cap.

 

(ii)      Muffle Furnace

 

(iii)     Desiccator

Weigh to the nearest mg about 5 gm of oven dried powdered sample in a weighed clean, dry Petri Dish. Incinerate in a muffle furnace for about 6-8 hours at 650-700 °C to constant weight. Cool in a dessicator and weigh. Report percentage of ash content obtained.

(b)      Calculation :

Ash content in per cent by weight = 100 x (C-A)/B - A

A = Weight of the empty crucible

B = Weight of the empty crucible plus material before ashing

C = Weight of the empty crucible plus material after ashing

4.        Estimation of conductivity-

As mentioned in Schedule IV Part D at serial number 4.

5.        Estimation of organic carbon-

As mentioned in Schedule IV Part D at serial number 5.

6.        Estimation of total nitrogen

(a)      Apparatus

1.        Suitable Kjeldahl assembly consisting of 500-800 ml round bottom, digestion flask and Kjeldahl distillation assembly consisting of 500-800 ml distillation flask, splash head tube and condenser, all with appropriate glass joints. The length of the condenser's delivery tube should be long enough to keep immersed in a flask for ammonia absorption.

2.        Kjeldahl digestion unit with heating control, suitable for 500-800 ml flasks.

(b)      Reagents

(a)      Sulphuric acid -- 93-98% H₂SO₄, N-free

 

(b)      Salicylic acid, reagent grade, N-free

 

(c)      Sodium thiosulphate (Na₂S₂O₃ 5H₂0), reagent grade

 

(d)      Zinc dust--impalpable powder

 

(e)      Copper sulphate

 

(f)       Potassium or sodium sulphate

 

(g)      Selanium powder

 

(h)     Red Mercury oxide (HgO)

 

(i)       45% NaOH solution. Dissolve 450 gm of Sodium hydroxide pellets in distilled water and make up the volume to 1000 ml

 

(j)       Methyl red indicator -Dissolve 1 gm methyl red in 200 ml alcohol

 

(k)      Hydrochloric or sulphuric acid standard solution -- 0.1 N or as per requirement

 

(l)       Sodium hydroxide standard solution 0.1 N or as per requirement.

(c)      Procedure.

(1)     Place weighed finely powdered sample (0.5 1.0 gm) in digestion flask,

 

(2)     Add 1 gm digestion mixture (20 g CuSO4 + 3 gm selenium dust + 1 gm HgO).

 

(3)     Add 50 ml conc H₂SO₄.

 

(4)     Shake the flask and let it stand for five minutes then heat over low flame until frothing ceases.

 

(5)     Turn off heat, add 15 --20 gm powdered K,SO4 (or anhydrous Na2SO4 ), and boil briskly until solution clears.

 

(6)     Add 5 gm Sodium thiosulphate, continue boiling for another at least 2-3 hours.

 

(7)     Remove from burner and cool, add 200 ml of water and swirl the flask to dissolve all the contents.

 

(8)     Transfer to 500 ml volumetric flask, giving several washings with water to the digestion flask. Make up the volume to 500 ml.

 

(9)     Take 25 ml aliquot in the distillation flask, add 300 ml water and a pinch of zinc dust.

 

(10)   Take 20 ml of standard acid solution (N,10 H2SO4) in the receiving conical flask, add 4 drops of methyl red indicator and keep the flask at the lower end of the condenser in such a way that the lower tip of the condenser is hilly immersed in acid solution.

 

(11)   Add 40 ml of45%NaOH to the distillation flask gently so that the contents do not mix,

 

(12)   Immediately connect the flask to distillation assembly and swirl to mix the contents. Heat until all the ammonia is distilled (at least 150 ml distillate).

 

(13)   Remove from receiving flask. Rinse outlet tube into receiving flask with a small amount of distilled water.

 

(14)   Titrate the contents in the receiver conical flask with standard NaOH solution.

 

(15)   Determine blank on reagents using same quantity of standard acid in receiving conical flask.

(d)      Calculation

Nitrogen % by weight = 1.401(V₁-N₁-V₂N₂)-(V₃N₁-V₄N₂) X df/W

where

V1- Volume in ml of standard acid taken in receiver flask for sample

V2= Volume in ml of standard NaOH used in titrating standard acid in receiver flask after distillation of test sample

V₃= Volume in ml of standard acid taken in receiver flask for blank

V4= Volume in ml of standard NaOH used in titrating standard acid in receiver flask after distillation in blank

N₁ = Normality of standard acid

N₂ = Normality of standard NaOH

W = Weight in gm of sample taken 

df= Dilution factor of sample

7.        Estimation of C:N ratio

Calculate the C:N ratio by dividing the organic carbon value with the total nitrogen value

8.        Estimation of Phosphate

As mentioned in Schedule IV Part D at serial number 8.

9.        Estimation of Potassium

As mentioned in Schedule IV Part D at serial number 9.]

[231][Schedule VI

[See clause 2(ab) and (q) and clause 20C]

Part-A

SPECIFICATIONS OF BIOSTIMULANTS

Part-B

TOLERANCE LIMIT

Part-C

PROCEDURE FOR DRAWAL OF SAMPLES OF BIOSTIMULANTS

1.        General Requirements of Sampling

1.0 In drawing, preparing and handling of samples, the following precautions and directions shall be observed:

1.1 Sampling shall be carried out by a trained and experienced person as it is essential that the sample should be representative of the lot to be examined.

1.2 Samples in their original unopened packets should be drawn and sent to the laboratory to prevent possible contamination of sample during handling and to help in revealing the true condition of the material.

1.3 Intact packets shall be drawn from a protected place not exposed to dampness, air, light, dust or soot.

2.        Scale of Sampling

2.1 Lot;

All units (containers in a single consignment of type of material belonging to the same batch of manufacture) shall constitute a lot. If a consignment consists of different batches of the manufacture, the containers of the same batch shall be separated and shall constitute a separate lot.

2.2 Batch:-All biostimulants prepared simultaneously in the same process constitute a batch.

2.3 For ascertaining conformity of the material to the requirements of the specification, samples shall be tested from each lot separately.

2.4 The number of packets to be selected from a lot shall depend on the size of the lot and these packets shall be selected at random.

3.        Drawal of Samples

3.1 The Inspector shall take three packets as samples from the same batch. Each sample constitutes a test sample.

3.2 Each sample shall be sealed in a cloth bag and be sealed with the Inspector's seal. The sealed cloth bag containing the sample and Form-P shall be kept in another cloth bag which shall also be sealed with the Inspector's seal. Identifiable details such as sample number, code number or any other details shall be put on the cloth bag containing sample and Form-P which enable its identification.

3.3 Out of the three samples collected, one sample so sealed shall be sent to in-charge of the laboratory notified by the State Government under the sub-clause (1C) of clause 29 or any laboratory notified by the Central Government. Another sample shall be given to the manufacturer or importer or dealer, as the case may be. The third sample shall be sent by the Inspector to his next higher authority for keeping in safe custody. Any of the latter two samples shall be sent for reference analysis under sub-clause (2) of clause 29B.

3.4 The number of samples to be drawn from the lot;

Part-D

METHODOLOGY OF TESTING.]

[232][Schedule VII

[(See clause 20D(1)]

GENERAL SPECIFICATIONS OF NANO FERTILISER

1.        Nano Nitrogen

2.        [237][Nano Nitrogen and Phosphorus fertilizer

3.        [238][Nano Phosphorus fertilizer

4.        [239][Nano Zinc

5.        Nano Copper

 

 

 

 

 

 

 

 

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FERTILISER [(INORGANIC, ORGANIC OR MIXED)] (CONTROL) ORDER, 1985

[FERTILISER [1][(INORGANIC, ORGANIC OR MIXED)] (CONTROL) ORDER, 1985]

PREAMBLE

In exercise of the powers conferred by section 3 of the Essential Commodities Act, 1955 (10 of 1955), the Central Government hereby makes the following Order, namely:-

Order - 1. Short title and commencement.

(1)     This Order may be called the Fertiliser [2][(Inorganic, Organic or Mixed)] (Control) Order, 1985.

(2)     It shall come into force on the date of its publication in the Official Gazette.

Order - 2. Definitions.

In this Order, unless the context otherwise requires:

(i)       "Act" means the Essential Commodities Act, 1955 (10 of 1955).

(aa) "Biofertiliser" means the product containing carrier based (solid or liquid) living microorganisms which are agriculturally useful in terms of nitrogen fixation, phosphorus solubilisation or nutrient mobilization, to increase the productivity of the soil and/or crop/

[3][(ab) "biostimulant" means a substance or microorganism or a combination of both whose primary function when applied to plants, seeds or rhizosphere is to stimulate physiological processes in plants and to enhance its nutrient uptake, growth, yield, nutrition efficiency, crop quality and tolerance to stress, regardless of its nutrient content, but does not include pesticides or plant growth regulators which are regulated under the Insecticide Act, 1968 (46 of 1968);]

(ii)      "certificate of source" means a certificate given by a State Government, Commodity Board, manufacturer, + importer, pool handling agency or as the case may be, wholesale dealer indicating therein the source from which fertiliser for purpose of sale is obtained.

(iii)     "Commodity Board" means the Coffee Board constituted under section 4 of the Coffee Act, 1942 (7 of 1942) or the Rubber Board constituted under section 4 of the Rubber Act, 1947 (24 of 1947), or the Tea Board constituted under section 4 of the Tea Act, 1953 (29 of 1953), or as the case may be, the Cardamom Board constituted under section 4 of the Cardamom Act, 1965 (42 of 1965).

(iv)    "compound or complex fertiliser" means a fertiliser containing two or more nutrients during the production of which chemical reaction takes place:-

(v)      "controller" means the person appointed as Controller of Fertilisers by the Central Government and includes any other person empowered by the Central Government to exercise or perform all or any of the powers, or as the case may be, functions of the Controller under this Order.

[4][(ee) "Customised Fertiliser" means a granular multi nutrient carrier which contains Primary, Secondary and /or micro nutrient forms, both from inorganic and/or organic sources, manufactured through a systematic process of Fusion blend granulation [5][or precision blend technology], formulated on the basis of soil fertility data and include 100% water soluble specialty fertilizer as customized combination products;]

(vi)    "dealer" means a person carrying on the business of selling fertilisers whether wholesale or retail or industrial use* and includes a manufacturer, +Importer, and a pool handling agency carrying on such business and the agents of such person, manufacturer, +importer or pool handling agency.

(vii)   Clause 'g' deleted vide S.O. 725 (E) dated 28.7.88.

(viii)  "fertilizer" means any substance used or intended to be used as a fertiliser of the soil and/or crop and specified in Part A of Schedule I and includes a mixture of fertilizer and special mixture of fertilizers provisional fertiliser, customised fertilizer, Bio-fertilizers specified in Schedule III and Organic fertilizers specified in Schedule IV.

[6][(h) "Fertiliser" means any essential substance, either in straight or mixed form and derived from either inorganic, organic or mixed sources, that is used or intended to be used to provide essential plant nutrients or beneficial elements or both for the soil or for the crop or makes essential plant nutrients available to the plants either directly or by biological process or by both in the soil or plant as notified from time to time by Central Government and specified in the schedules appended to this order or as may be notified by the State Governments [7][and includes a biostimulant] [8][and nano fertiliser].

Explanation:-For the purpose of Fertiliser,-

(i)       "the essential plant nutrients" include Primary Nutrients (Nitrogen, Phosphorous and Potassium), Secondary Nutrients (Calcium, Magnesium and Sulphur) and Micro Nutrients (Zinc, Manganese, Copper, Iron, Boron and Molybdenum);

(ii)      "Beneficial element" means any element as notified by the Central Government from time to time.;]

(i) "Form" means a form appended to this Order.

(j) "grade" means the nutrient element contents in the fertiliser expressed in percentage.

(k) "granulated mixture" means a mixture of fertilisers made by intimately mixing two or more fertilisers with or without inert material, and granulating them together, without involving any chemical reaction.

(Kk) "importer" means a person who imports fertiliser in accordance with the Export and Import Policy of the Central Government, as amended from time to time.

I.         "inspector" means an Inspector of Fertilisers appointed under clause 27.

II.       "industrial dealer" means a dealer who sells fertilisers for industrial purposes.

III.     "industrial purposes" means the use of fertiliser for purposes other than fertilisation of soil and Increasing productivity of crops.

(m) "manufacturer" means a person who produces fertilisers or mixtures of fertilisers and the expression "manufacture" with its grammatical variations shall be construed accordingly.

[9][(mb) the mixture of micronutrient are those which are made by mixing of micronutrient notified in Schedule-I under the sub-heading "1(g) MICRONUTRIENTS" of said Order.]

(n) "mixture of fertilisers" ***means a mixture of fertilisers made by physical mixing two or more fertilisers with or without inert material in physical or granular form and includes a mixture of NPK fertilisers, a mixture of micronutrient fertilisers and a mixture of NPK with micronutrient fertilisers.

(nn) Notified Authority "means an authority appointed under clause 26 A.

(n) "offer for sale" includes a reference to an intimation by a person of a proposal by him for the sale of any fertiliser, made by publication of a price list, by exposing the fertilizer for sale indicating the price, by furnishing of a quotation or otherwise howsoever.

[10][(na) "nano fertiliser" means the fertiliser of nano scale complying with the specifications as provided in clause 20 D]

(nna) "Non-edible de-olied cake fertiliser" means substances obtained as residue after oli extraction (by expeller and/ or thought solvent extraction) form crused seeds of non-edible oilseeds [11][including Castor, Neem, Karanj (Pongamiapinnata), Mahua (madhucalongifolia) and Jatropha] for use in soil as fertilizer.

(oo) Organic fertilizer means substances made up of one or more unprocessed materials of a biological nature (plant/animal) and may include unprocessed mineral materials that have been altered through microbiological decomposition process.

(p) 'physical mixture" means a mixture of fertilisers made by physically mixing two or more fertilisers with or without inert material necessary to make a required grade, without involving any chemical reaction.

(pp) "Provisional fertilizer" means fertilizer specified under clause 20 A.

(q) "prescribed standard" means:-

i.         in relation to a fertiliser included in column 1 of Part A of Schedule-I, the standard set out in the corresponding entry in column 2, subject to the limits of permissible variation as specified in Part B of that [12][Schedule and includes all such fertilizers whose standards are specified in such Schedule and are fortified with such micronutrients as given below.

Explanation:- The specification of the fertilizer which shall be fortified with above mentioned micronutrient shall remain the same as specified in Schedule -I.]

ii.        in relation to a mixture of fertilisers, the standard set out in respect of that mixture under sub-clause (1) of clause 13 by the Central Government, subject to the limits of permissible variation as specified in Part B of Schedule-I

iii.       in relation to mixture of fertilisers, standard set out in respect of that mixture under sub-clause (2) of clause 13 by the State Government, subject to limits of permissible variation as specified in Part B of Schedule-I.

iv.       in relation to a Biofertiliser included in column 1 of Part A of Schedule-III, the standard set out in the corresponding entry in column 2, subject to the limits of permissible variation as specified in Part B of that Schedule;

v.        in relation to a Organic fertiliser included in column 1 of Part A of Schedule-IV, the standard set out in the corresponding entry in column 2, subject to the limits of permissible variation as specified in Part B of that Schedule.

vi.       In relation to a non-edible de-oiled cake fertiliser specified in column (2) of Part A of Schedule V, the standard set out in the corresponding entry in column (2) of the said part, subject to the limits of permissible variation as specified in part B of the said Schedule.]

vii.      [13][prescribed standard means in relation to Customised Fertilizers, standards set out in respect of Customised Fertilizers under clause 20B by the Central Government, subject to limits of permissible variation as specified in part B of Schedule I]

viii.    [14][in relation to a biostimulant included in column (2) of Part-A of Schedule VI, the standard set out in the corresponding entry in column (3), subject to the limits of permissible variations as specified in Part-B of the said Schedule;]

ix.       [15][in relation to a nano fertiliser, means the specifications set out under clause 20D;]

(r) "pool handling agency" means an agency entrusted by the Central Government with functions relating to handling and distribution of imported fertilisers.

(s) "registering authority" means a registering authority appointed under clause 26 in respect of mixture of fertilizers and special mixture of fertilizers

(t) "retail dealer" means a dealer who sells fertilisers to farmers or plantations for **agricultural use such as for fertilisation of soil and increasing productivity of crops.

(u) "Schedule" means a Schedule appended to this Order.

(v) "special mixture of fertilisers" means any mixture of fertilisers prepared for experimental purposes in pursuance of a requisition made by any person (including a person engaged in the cultivation of tea, coffee or rubber) for sale to that person in such quantity and within such period as may be specified in such requisition; and.

(w) "wholesale dealer" means a dealer who sells fertilisers otherwise than in retail-for agricultural use such as for fertilisation of soil and increasing productivity of crops.

II. PRICE CONTROL

Order - 3. Fixation of prices of fertilisers.

(1)     The Central Government may, with a view to regulating equitable distribution of fertilisers and making fertilisers available at fair prices, by notification in the Official Gazette, fix the maximum prices or rates at which any fertiliser may be sold by a dealer, manufacturer, importer or a pool handling agency.

 

(2)     The Central Government may having regard to the local conditions of any area, the period of storage of fertilisers and other relevant circumstances, fix different prices or rates for fertilisers having different periods of storage or for different areas or for different classes of consumers.

 

(3)     No dealer, manufacturer +importer or pool handling agency shall sell or offer for sale any fertiliser at a price exceeding the maximum price or rate fixed under this clause.

Order - 4. Display of stock position and price list of fertilisers.

Every dealer, who makes or offers to make a retail sale of any fertilisers, shall prominently display in his place of business:-

(a)      the quantities of opening stock of different fertilisers held by him on each day;

Explanation -The actual stocks at any point of time during the day may be different from that of the displayed opening stocks to the extent of sale and receipt of such fertilisers upto the time of inspection during that day

(b)      a list of prices or rates of such fertilisers fixed under clause 3 and for the time being in force.

Order - 5. Issue of cash/credit memorandum.

(a)      Every dealer shall issue a cash or credit memorandum to a purchaser of a fertiliser in Form M*

III. CONTROL ON DISTRIBUTION OF FERTILISERS BY MANUFACTURER/IMPORTER

Order - 6. Allocation of fertilisers to various States.

The Central Government may, with a view to securing equitable distribution and availability of fertilisers to the farmers in time, by notification in the Official Gazette, direct any manufacturer/importer to sell the fertilisers produced by him in such quantities and In such State or States and within such period as may be specified in the said notification.

IV. AUTHORISATION OR REGISTRATION OF DEALERS"

Order - 7. Registration of Industrial dealers and authorization of other dealers.

No person shall sell, offer for sale or carry on the business of selling of fertilizer at any place as wholesale dealer or retail dealer except under and in accordance with clause 8 :

Provided that a State Government may, if it considers it necessary or expedient, by notification in the Official Gazette, exempt from the provisions of this clause any person selling fertilizer to farmers in such areas and subject to such conditions as may be specified in that notification.

Order - 8. Application for intimation or registration.

(1)     Every person intending to sell or offer for sale or carrying on the business of selling of fertilizer as Industrial Dealer shall obtain a certificate of registration from the controller by making an application in Form A together with the fee prescribed under clause 36 and a Certificate of source in Form O.

(2)     Every person including a manufacturer, an importer, a pool handling agency, wholesaler and a retail dealer intending to sell or offer for sale or carrying on the business of selling of fertilizer shall make a Memorandum of Intimation to the Notified Authority, in Form A1 duly filled in, in duplicate, together with the fee prescribed under clause 36 and certificate of source in Form O.

(3)     On receipt of a Memorandum of Intimation, complete in all respects, the Notified Authority shall issue an acknowledgement of receipt in Form A2 and it shall be deemed to be an authorization letter granted and the concerned person as authorised dealer for the purposes of this Order.

Provided that a certificate of registration granted before the commencement of the Fertiliser (Control) Amendment Order, 2003, shall be deemed to be an authorization letter granted under the provisions of this Order:

Provided further that where the applicant is a State Government, a manufacturer or an importer or a pool-handling agency, it shall not be necessary for it or him to submit Form O.

Provided also that a separate Memorandum of Intimation shall be submitted by an applicant for whole sale business or retail dealership, as the case may be:

Provided also that where fertilizers are obtained for sale from different sources, a certificate of source from each such source shall be furnished in Form O."

[16][Provided also that where the manufacturer of organic fertilizer is a State Government or municipality, it shall not be necessary for it to obtain the authorisation letter:

Provided also that where the manufacturer of vermi-compost, other than a State Government or municipality, has annual production capacity less than 50 metric tonnes, it shall not be necessary for him to obtain the authorisation letter.]

[17][Provided also that the manufacturer of Fermented Organic Manure and Liquid Fermented Organic Manure, shall not be required to obtain the authorisation letter under sub-clause (3) of clause 8 of the said Order for a period of three years from the date of issue of notification.]

(4)     [18][No authorisation letter shall be granted to any applicant for retail dealership, unless the applicant possess the certificate course of fifteen days from any State Agriculture University or Krishi Vigyan Kendras or National Institute of Agricultural Extension Management (MANAGE) or National Institute of Rural Development and Panchayati Raj (NIDPR) or Fetiliser Association of India or any other approved Government Institute:

Provided that a person in possession of Bachelor of Science in Agriculture or chemistry or Diploma in Agriculture Science from a recognised University or Institute or equivalent course having one of the subject on fertiliser or agri inputs, as notified by the State Government shall not be required to possess separate certificate course:

Provided further that a dealer who has been granted authorisation letter before commencement of the Fertiliser (Inorganic, Organic or Mixed) (Control) Fourth Amendment Order, 2018 shall not be required to possess the qualification at the time of renewal of their authorisation letter:

Provided also that the said qualification shall not be applicable for renewal of the authorisation letter of the registered Agricultural Cooperative Societies and State Marketing Federations subject to condition that such Society or Federation shall engage a person who possesses the qualification under this clause.]

Order - 9. Grant or refusal of certificate of registration.

The Controller, shall grant a certificate of registration in Form 'B' within thirty days of the receipt of application to any person who applies for it under clause 8;

Provided that no certificate of registration shall be granted to a person: -

(a)      if his previous certificate of registration is under suspension; or

 

(b)      if his previous certificate of registration has been cancelled within a period of one year immediately preceding the date of application; or

 

(c)      if he has been convicted of an offence under the Act, or any Order made there under within three years immediately preceding the date of making the.

 

(d)      if he fails to enclose with the application a certificate of source ; or

 

(e)      if the application is incomplete in any respect; or

 

(f)       if he makes an application for obtaining the certificate of registration for industrial dealer and, excepting if he is a manufacturer ,+ importer or pool handling agency, holds an authorization letter for wholesale dealer or retail dealer or both, and as the case may be, the vice-versa.

Order - 10. Period of validity of certificate of registration and letter of authorization.

Every certificate of registration granted under clause 9 and every authorization letter issued under clause 8 shall, unless renewed, suspended or cancelled, be valid for a period of [19][five years] from the date of its issue.

[20][Notwithstanding anything contained in the said clause, the letter of Authorisation granted to the manufacture of City Compost issued under clause 8, unless suspended or cancelled is valid in perpetuity.]

Order - 11. Renewal of certificates of registration and authorization letters.

(1)     Every holder of a certificate of registration granted under clause 9 or authorization letter granted or deemed to have been granted under clause 8, desiring to renew such certificate or authorization letter shall, before the date of expiry of such certificate of registration or authorization letter, as the case may be, make an application for renewal to the Controller, in Form C, or to the Notified Authority in Form A1, respectively, in duplicate, together with the fee prescribed under clause 36 for such renewal and a certificate of source as required under clause 8.

 

(2)     On receipt of an application under sub-clause (1), together with such fee and certificate of source, the controller may renew the certificate of registration or the Notified Authority, as the case may be shall issue acknowledgement receipt of renewal in form A 2. Provided that a certificate of registration shall not be renewed if the holder of the same did not sell any fertiliser during the period of one year immediately preceding the date of expiry of the period of validity.

 

(3)     If any application for renewal is not made before the expiry of the period of validity of the certificate of registration or, as the case may be, the authorization letter but is made within one month from the date of such expiry, the certificate of registration or, as the case may be, the authorization letter shall be dealt as provided in sub-clause (2) on payment of such additional fee as may be prescribed under clause 36 in addition to the fee for renewal.

 

(4)     Where the application for renewal of certificate of registration is made within the time specified in sub- clause (1) or sub-clause (3), the applicant shall be deemed to have held a valid certificate of registration until such date as the controller passes orders on the application for renewal.

 

(5)     If an application for renewal of a certificate of registration or authorization letter is not made within one month from the date of expiry of their period of validity, the same shall be deemed to have lapsed on the date on which its validity expired and any business carried on after that date shall be deemed to have been carried on in contravention of clause 7.

V. MANUFACTURE OF MIXTURES OF FERTlLIZERS, ORGANIC FERTILISER AND BIO- FERTILISER

Order - 12. Restriction on preparation of mixtures of fertilizer.

No person shall carry on the business of preparing any mixture of fertilisers or special mixture of fertilizers, Bio-fertilizers or Organic fertilisers except under and in accordance with the terms and conditions of a certificate of manufacture granted to him under clauses 15 or 16.

Order - 13. Standards of mixtures of Fertilisers.

(1)     Subject to the other provisions of the order

(a)      no person shall manufacture any *mixture of fertilisers whether of solid or liquid fertilizers specified in Part a of schedule I unless such mixture conforms to the standards set out in the notification to be issued by the Central Government in the Official Gazette;

 

(b)      no person shall manufacture any biofertiliser unlessl such biofertiliser conforms to the standards set out in the part A of Schedule - III.

 

(c)      no person shall manufacture any Organic fertilizer unless such organic fertilizer conforms to the standards set out in the part A of Schedule IV.

(2)     Subject to the other provisions of this order, no person shall manufacture any "mixture of fertilisers unless such mixture conforms to the standards set out in the notification to be issued by the State Government in the Official Gazette;

Explanation- For the purposes of this sub-clause, mixture of fertilizers shall not include liquid fertilizers and 100% water soluble fertilizers, containing N,P,K.

(3)     [omitted]

(4)     No Certificate of manufacture shall be granted in respect of any fertiliser which does not conform to the standards set out in the notification referred in sub- clause (1) or (2);

(5)     Nothing in this clause shall apply to special mixtures of fertilisers

Order - 14. Application for certificate of manufacture of mixtures of fertilisers.

(1)     Every person desiring to obtain a certificate of manufacture for preparation of any mixture of fertilisers or special mixture of fertilisers shall possess such mixture, *and possess the minimum laboratory facility as specified in clause 21A of this Order.

(2)     An applicant for a certificate of manufacture for preparation of mixture of fertilisers or special mixture of fertilisers shall make an application to the registering authority

(a)      if he is an applicant for a certificate of manufacture for any mixture of fertilisers in Form D, in duplicate, together with the fee prescribed there for under clause 36; or,

(b)      if he is an applicant for a certificate of manufacture for any special mixture, in Form E, in duplicate, together with the fee prescribed there for under the said clause 36 and an attested copy of the requisition of the purchaser.

(3)     Every person desiring to obtain a Certificate of Manufacture for preparation or organic fertilizer or biofertiliser shall make an application in Form D, in duplicate, together with a fee prescribed therefore under clause 36, to Registering authority.

[21][Provided that where the manufacturer of organic fertilizer is a State Government or a municipality, it shall not be necessary for it to obtain the Certificate of Manufacture:

Provided further that where the manufacturer of vermi-compost, other than a State Government or municipality, has annual production capacity less than fifty metric tonnes, it shall not be necessary for him to obtain the Certificate of Manufacture for preparation of vermi-compost.]

Order - 15. Grant or refusal of certificate of manufacture for preparation of mixtures of fertilizers, Biofertilisers or Organic fertilizer..

(1)     On receipt of an application under clause 14, the registering authority shall, by order in writing, either grant or refuse to grant the certificate of manufacture in respect of any mixture of fertilizer, Biofertiliser, Organic fertiliser or special mixture of fertilizer and shall, within forty-five days from the date of receipt of the application, furnish to the applicant a copy of the order so passed;

(2)     Where an application for a certificate of manufacture for mixture of fertilizers, Biofertiliser, Organic fertiliser is not refused under sub-clause (1), the registering authority shall grant a certificate of manufacture in Form F and where an application for a certificate of manufacture for a special mixture is not refused under that sub-clause, *[such authority shall within forty five dates from the date of receipt of the application, ]grant a certificate of manufacture to the applicant in Form G

Order - 16. Conditions for grant of certificate of manufacture in respect of special mixture of fertilisers and period of validity of such certificate.

(1)     No certificate of manufacture in respect of any special mixture of fertilisers shall be granted to an applicant unless he holds a valid certificate of manufacture under this Order for any mixture of fertilisers.

(2)     Every certificate of manufacture granted in respect of any special mixture of fertilisers shall be valid for a period of six months from the date of its issue;

Provided that the registering authority may, if it is satisfied that it is necessary so to do, extend the said period to such further period or periods as it may deem fit, so however, that the total period or periods so extended shall not exceed twelve months.

Order - 17. Period of validity of a certificate of manufacture for preparation of mixtures of fertilizers, Biofertilisers or Organic fertilizer.

Every certificate of manufacture granted under clause 15 for preparation of a mixture of fertilizers, Biofertiliser or Organic fertilizers shall, unless suspended or cancelled, be valid for a period of three years from the date of issue.

Order - 18. Renewal of certificate of manufacture for preparation of mixtures of fertilizers, Biofertiliser or Organic fertiliser.

(1)     Every holder of a certificate of manufacture for preparation of a mixture of fertilizers, Biofertiliser, Organic fertiliser desiring to renew the certificate, shall, before the date of expiry of the said certificate of manufacture make an application to the registering authority in Form D in duplicate, together with the fee prescribed for this purpose under clause 36.

 

(2)     On receipt of an application for renewal as provided in sub-clause (1), and keeping in view the performance of the applicant and other relevant circumstances, the registering authority may, if he so decides, renew the certificate of manufacture by endorsement on Form F and in case the certificate of registration is not renewed, the registering authority shall record in writing his reasons for not renewing the certificate of manufacture.

 

(3)     If an application for renewal is not made before the expiry of the certificate of manufacture but is made within one month from the date of expiry of the certificate of manufacture, the certificate of manufacture may be renewed on payment of such additional fee as may be prescribed by the State Government for this purpose.

 

(4)     Where the application for renewal is made within the time specified in sub-clause (1) or sub-clause (3), the applicant shall be deemed to have held a valid certificate of manufacture until such date as the registering authority passes order on the application for renewal.

 

(5)     If an application for renewal of a certificate of manufacture is not made within the period stipulated under sub-clause (1) or, as the case may be, under sub-clause (3), the certificate of manufacture shall be deemed to have expired immediately on the expiry of its validity period, and any business carried on after that date shall be deemed to have been carried on in contravention of clause 12.

VI. RESTRICTIONS ON MANUFACTURE/ IMPORT, SALE, ETC. OF FERTlLISER

Order - 19. Restriction on manufacture/import, sale and distribution of fertilisers.

No person shall himself or by any other person on his behalf:-

(a)      manufacture/import for sale, sell, offer for sale, stock or exhibit for sale or distribute any fertlliser which Is not of prescribed standard;

(b)      manufacture/Import for sale, sell, offer for sale, stock or exhibit for sale, or distribute any mixture of fertilisers, which is not of prescribed standard** (subject to such limits of permissible variation as may be specified from time to time by the Central Government) or special mixture of fertilisers which does not conform to the particulars specified In the certificate of manufacture granted to him under this Order in respect of such special mixture.

(c)      sell, offer for sale, stock or exhibit for sale or distribute:-

(i)       any fertiliser the container whereof is not packed and marked in the manner laid down In this Order

(ii)      any fertiliser which is an [imitation of or] a substitute for another fertiliser under the name of which It Is sold;

(iii)     any fertiliser which Is adulterated;

Explanation:- A fertiliser shall be deemed to be adulterated, If It contains any substance the addition of which is likely to eliminate or decrease Its nutrient contents or make the fertiliser not conforming to the prescribed standard.

(iv)    any fertiliser the label or container whereof bears the name of any individual firm or company purporting to be manufacturer/Importer of the fertiliser, which individual, firm or company Is fictitious or does not exsist.

(v)      any fertiliser, the label or container whereof or anything accompanying therewith bears any statement which makes a false claim for the fertiliser of which s false or misleading in any material particular.

(vi)    any substance as a fertiliser which substance is not, in fact, a fertiliser; or

(vii)   any fertiliser without exhibiting the minimum guaranteed percentage by weight of plant nutrient.

[22][Provided that specifications of city compost in Schedule IV shall, in case of municipalities, be applicable only when it is traded in packaged form for use in agriculture:

Provided further that the specifications of vermi-compost in Schedule IV shall be applicable only in such cases where it is sold in packaged form and for agricultural purposes.]

Order - [19A.

In cases where the samples were drawn from the dealers out of original sound bags (without any mark of tempering) and are found non-standard, then in such circumstances both dealer and manufacturer shall be made party for filling the case in the concerned court under the Act and proceedings under clause 31 of this Order.][23]

Order - 20. Specifications In respect of imported fertilisers.

Notwithstanding anything contained in this Order, the Central Government may by an order, published in the Official Gazette, fix separate specifications in respect of imported fertilisers [24][which shall valid for a period not exceeding three years].

Order - 20A. Specification in respect of provisional fertilizer

Notwithstanding anything contained in this Order, the Central Government may, by order published in the Official Gazette, notify specifications, valid for a period not exceeding three years, in respect of fertilizers to be manufactured by any manufacturing unit for conducting commercial trials.

Order - 20B.[Specification in respect of Customised Fertiliser.-

(i)       Notwithstanding anything contained in this Order, the Central Government may by notification in the Official Gazette notify the General specification of customised fertiliser [25][which shall valid for a period not exceeding four years][26].

(ii)      No person shall manufacture any grade of Customised Fertiliser unless such customised fertiliser conforms to the standards set out in the notification to be issued by the Central Government in the Official Gazette under sub-clause (i):

Provided that the grades of customized fertiliser, which the company will manufacture, must be based on the soil fertility data maintained by the Ministry of Agriculture and Farmers Welfare or State Governments:

Provided further that in case, the data for a district for which the company intending to formulate the grade is not available or still under process by the State Government, then the company shall use the scientific data obtained from soil testing results generated by testing in their own laboratories.

(iii)     No person, except with the prior permission of Controller shall, manufacture any particular grade of customized fertilizer formulated as per the General specification notified under sub-clause (i).

(iv)    Every person, desirous of obtaining a specific product approval of any particular grade of customised fertilizer, shall make an application in form Q in duplicate to the Controller of Fertiliser, Government of India.

(v)      On receipt of application under clause (ii), the Controller shall by order in writing either grant or refuse to grant the permission, in respect of manufacturing of any particular grade of customised fertiliser and shall within three months from the date of receipt of application shall furnish a copy of order so passed to the applicant:

Provided that on completion of three years or earlier, manufacturing company of customised fertiliser shall again submit an application for approval for manufacturing of the said grade:

Provided further that the permission for manufacture and sale of Customised Fertiliser shall be granted to only such Fertiliser Companies whose annual production of fertilisers other than CFs is 5.00 lakh metric tonne:

Provided also that such manufacturing companies, having annual production of 5 LMT of fertilizer other than CFs, can set up manufacturing units of CF either on their own or through subsidiaries or joint venture through a minimum stake of 51% in such joint ventures.]

Order - [20C. Specifications in respect of biostimulants.

(1)     Notwithstanding anything contained in this Order, the specifications of biostimulants, including its name, active ingredients or where it is not possible to indicate its active ingredients, then its chemical composition, name of the crop to which it may be applied, its benefits and the method of analysis for determination of its active ingredients or chemical composition shall be specified by the Central Government in Schedule VI.][27]

(2)     The biostimulants specified in Schedule VI shall be classified under any of the following categories, namely:

(i)       botanical extracts, including seaweed extracts;

 

(ii)      bio-chemicals;

 

(iii)     protein hydrolysates and amino acids;

 

(iv)    vitamins;

 

(v)      cell free microbial products;

 

(vi)    antioxidants;

 

(vii)   anti-transpirants;

 

(viii)  humic and fulvic acid and their derivatives

(3)     Notwithstanding anything contained in this order, every manufacturer or importer of a biostimulant shall make an application to the Controller in Form G along with the following data relating to such product for specifying it as a biostimulant in Schedule VI, namely;

A.        Chemistry:

(1)     Source (natural extracts of plant/microbe/animal/synthetic)

 

(2)     Product Specification (with analysis from Good Laboratory Practice (GLP) or National Accreditation Board for Testing and Calibration Laboratory (NABL) accredited laboratory, Physical  and Chemical properties of active ingredients and adjuvants, if any.

 

(3)     Method of analysis conforming to the specifications.

 

(4)     Shelf-life;

B.        Bio-efficacy Trials:

1.        Agronomic Bio-efficiency trials shall be conducted at National Agricultural Research System, including Indian Council of Agricultural Research, State Agricultural Universities.

2.        Bio-efficacy trials shall be conducted at minimum three different doses for one season at three agro-ecological locations;

C.        Toxicity: Name of the Institute (where the manufacturer of biostimulant obtained the certificate)

The test report along with recommendation of following five basic acute toxicity tests (i) to (v) and four Eco toxicity tests (vi) to (ix) of GLP accredited laboratory shall be submitted along with the application, namely:-

(i)       Acute oral (Rat)

 

(ii)      Acute dermal (Rat)

 

(iii)     Acute Inhalation (Rat)

 

(iv)    Primary skin Irritation (Rabbit)

 

(v)      Eye irritation (Rabbit)

 

(vi)    Toxicity to bird

 

(vii)   Toxicity to Fish (Freshwater)

 

(viii)  Toxicity to honeybee

 

(ix)    Toxicity to earthworm

Note:-Long-term chronic studies as in case of pesticides are not needed to be conducted;

D.       Heavy metal analysis report;

E.        The sample of the product along with an Affidavit by the manufacturer or importer on non-judicial stamp paper of rupees ten stating that the product is not laced with pesticide beyond permissible limit of 0.01ppm

Provided that in case of a biostimulant having natural origin or other, the requirement of necessary data shall be as decided by the Central Biostimulants Committee as per the guidelines formulated by it in this regard:

Provided further that every manufacturer or importer of a biostimulant shall, notwithstanding that such biostimulant has been specified in Schedule VI, be required to make an application under this sub-clause

(4)     Notwithstanding anything contained in this order, any person manufacturing [28][or importing] a biostimulant as on the date of publication of this order for which no standards have been specified, may, subject to making an application for grant of provisional registration under sub-clause (5), [29][continue to manufacture or import] for sale, sell, offer for sale, stock or exhibit such biostimulant for a period of two years [30][four years] from the date of publication of this order.

(5)     The manufacturer [31][or importing] referred to in sub-clause (4) shall, [32][31st March, 2023], submit an application to the Controller for grant of provisional registration in Form G-1 along with

(a)      details of the product, its specifications, label and such other particulars as may be required;

(b)      a certificate issued by the State Government in Form G-2 to the effect that

(i)       the product is available in the market prior to the publication of the said order; and

(ii)      no incident has come to its notice about harmful effect of the product.

(6)     On receipt of an application under sub-clause (5) for provisional registration, the Controller shall, by an order in writing, grant a provisional certificate of registration of biostimulant in Form G-3.

(7)     No person shall manufacture or import any biostimulant unless such biostimulant is included in schedule VI.

(8)     The Controller shall, by notification in the Official Gazette, publish the name of the manufacturer or importer of the biostimulant included in Schedule VI.

(9)     No biostimulant shall contain heavy metals content over and above the following maximum limit prescribed for various metals, namely,

(10)   No biostimulant shall contain any pesticide beyond the permissible limit of 0.01ppm.]

Order - [20D.

(1)     "Notwithstanding anything contained in this Order, the Central Government may, by order published in the Official Gazette, notify specifications, valid for a period not exceeding three years, conforming to the general specifications as specified in Schedule VII, in respect of nano fertilisers to be manufactured by such manufacturing unit, as may be specified therein.

 

(2)     No person shall manufacture any nano fertiliser unless such fertiliser conforms to the standard set out in the order issued under sub-clause (1).

 

(3)     Every person, desirous of obtaining approval of any nano fertiliser shall make an application in Form-G-4 in duplicate to the Controller along with a report of the State Agriculture University or of the Indian Council of Agricultural Research on multi-locational and multi crop bio-efficacy trial of minimum one season and also a report from any of the NABL accredited laboratories on biosafety, biotoxicity and quality trial as per the guidelines issued by the Department of Bio-Technology.

 

(4)     Every manufacturer shall inform the Central Government and the Director (Agriculture) of the concerned State Government as to where it intends to make said fertiliser available to the farmers.

 

(5)     Every manufacturer shall ensure training to farmers on the safety aspects of the use of nano fertiliser.

 

(6)     Every manufacturer shall print necessary precautions on the label of the container of the nano fertiliser or on a separate leaflet to be packed with the nano fertiliser.

 

(7)     Every manufacturer shall provide to the Central Government a test report of each batch from any of the NABL accredited Laboratories before its distribution or dispatch of nano fertiliser.

 

(8)     Every manufacturer shall print the batch number on the container or shall have the label securely affixed on the container having weight less than 5 litre.][33]

Order - 21. Manufacturers/Importers pool handling agencies to comply with certain requirements in regard to packing and marking, etc.

every manufacturer/importer and pool handling agency shall, in regard to packing and marking of containers of fertilisers, Biofertiliser or Organic fertiliser comply with the following requirements, namely:-

(a)      Every container in which any fertiliser is packed shall conspicuously be superscribed with the word "FERTILISER" and shall bear only such particulars and unless otherwise required under any law nothing else, as may from time to time, be specified by the Controller in this behalf, and;]

(aa) Every container in which any Biofertiliser or Organic fertilizer is packed shall conspicuously be superscribed with the word "BIO-FERTILISER/ ORGANIC FERTILISER" and shall bear only such particulars and unless otherwise required under any law nothing else, as may from time to time, be specified by the Controller in this behalf,

Provided that in case of containers the gross weight of which is 5 kg or less, no such printing of superscription and other particular shall be necessary if such super superscription and other particulars are printed on a separate label which is securely affixed to such container.

(b)      Every container shall be so packed and sealed that the contents thereof cannot be tampered with without breaking the seal;

Provided that where fertilizer manufactured in India are packed in bags stitched on hand, such bags shall bear lead seals, so that the contents thereof cannot be tampered with without breaking the seals;

Provided further that lead sealing shall not be necessary:-

(i)       if such bags are machine stitched in such a manner that contents thereof cannot be tampered with without a visible break in the stitching; and

(ii)      in the case of fertilizers imported from abroad and packed a in bags stitched in hand, in such a manner that the contents thereof cannot be tampered with without visible break in the stitching.

Provided also that in case fertilizer bags are in cut, torn or damaged condition during transportation or mishandling during loading or unloading operation, the manufacturer of such fertilizer may, under intimation to the State Government and the Central Government, repack he fertilizer in new bags or restandardise the quantity in terms of declared weight.

(c)      Every fertiliser bag in which any fertiliser is packed for sale shall be of such weight and size as may be specified by the Central Government from time to time in this behalf

(d)      [34][every container in which any biostimulant is packed shall be conspicuously superscribed with the word "Biostimulant" and shall bear only such particulars as the Central Government may, by notification in the Official Gazette, specify in this behalf, unless any other particulars are required under any other law for the time being in force.]

Order - 21A. Manufacturers to comply with certain requirements for laboratory facilities.

Every manufacturer shall, in order to ensure quality of their product, possess minimum laboratory facility, as may be specified from time to time by the Controller.

Order - 22. Bulk sale of fertilisers.

Notwithstanding anything contained In this Order:-

(a)      a retail dealer may retain at any time one bag or container of each variety of fertiliser in an open and unsealed condition for the purpose of sale;

 

(b)      a manufacturer/importer may sell the fertiliser manufactured/imported by him in bulk to a manufacturer of mixture of fertilisers, compound / complex fertilisers or special mixture of fertilisers; and

 

(c)      the Central Government may by notification published in the Official Gazette in this behalf authorise a manufacturer/importer to sell any fertiliser manufactured/ imported by him In bulk also direct to farmers for such period as may be specified in that notification: 

[35][Provided that where the municipality is the manufacturer of city compost, it shall not for the Central Government to notify it for bulk sale;

Provided further that a certificate indicating the minimum guaranteed percentage of plant nutrients is issued by the manufacturer/importer to each farmer at the time of such sale.]

Order - 23. Disposal of non-standard fertilisers.

(1)     Notwithstanding anything contained In this Order, a person may sell, offer for sale, stock or exhibit for sale or distribute, [any fertiliser except any fertiliser imported by the Central Government] which, not being an adulterated fertiliser, does not conform to the prescribed standard (hereinafter in this Order referred to as non-standard fertiliser) subject to the conditions that:

(a)      the container of such non-standard fertilizer is conspicuously superscribed in red colour with the words "non-standard" and also with the sign "X"; and

 

(b)      an application for the disposal of non-standard fertilisers in Form H is submitted to the [Notified authority] to grant a certificate of authorisation for sale of such fertilisers and a certificate of authorisation with regard to their disposal and price is obtained in Form I.

 

(c)      such non-standard fertiliser shall be sold only to the manufacturers of mixtures of fertilisers or special mixtures of fertilisers or research farms of Government or Universities or such bodies.

(2)     The price per unit of the non-standard fertiliser shall be fixed by the [notified authority] after satisfying itself that the sample taken is a representative one, and after considering the nutrient contents in the sample determined on the basis of a chemical analysis of the non-standard fertilizer.

(3)     The Central Government may, by notification in the official Gazette and subject to the conditions, if any, laid down in that notification, and subject to guidelines issued in this regard by the Central Government exempt such pool handling agencies, as it deems fit, from complying with conditions laid down in paragraphs (a) and (b) of the sub-clause (1)

(4)     Where any fertiliser imported by the Central Government is found to be of non-standard and the Central Government decides that the fertilizer cannot be permitted for direct use in agriculture, it may permit the use of such fertiliser by manufacturers of complex fertilisers, mixture of fertilisers or special mixture of fertilisers to be sold at such price as may be fixed by the Central Government.

(5)     If a manufacture or importer detects or as reasonable doubt about the standard of the fertilizer manufactured or imported by him, and dispatched for sale as deteriorated in quality during transit due to natural calamity and is not of the prescribed standards, he may, within fifteen days from the date of dispatch from factory or port, apply with detailed justifications to the Central Government for obtaining permission for reprocessing the same in a factory to meet the prescribed standards and the Central Government may, after considering the facts, permit the re-processing of such fertilizer on the terms and conditions as may be notified by the Central Government in this behalf.

Provided that no such application for permission to reprocess the fertilizer by the manufacturer or importer shall be accepted by the Central Government after the expiry of the said period of fifteen days.

[36][6. Disposal of Biofertilizers (non-standard or expired)

Notwithstanding anything contained in this (Order), every manufacturer shall recycle the carrier based biofertiliser after sterilisation of the stock lying at manufacture's site, is not of prescribed standard (hereinafter referred as non-standard), or can dispose solid or liquid biofertiliser or both by spraying or by sprinkling over the compost piles or windrows; in case of liquid biofertiliser it shall be destroyed by autoclaved first and then spread or sprinkled on the soil in nearby fields.]

Order - [23A. Reprocessing of fertiliser damaged during storage.-

(1)     Notwithstanding anything contained in this order, where the stock of fertiliser damaged during its storage, the manufacturer or the importer of such fertiliser may make an application for grant of certificate of reprocessing in Form I-1 along with prescribed fee to the Notified Authority for reprocessing such fertiliser in the manufacturing unit of such manufacturer or the unit mentioned by the importer in his application.

(2)     The Notified Authority may, on being satisfied, allow the application made under sub-clause (1) and grant the certificate of reprocessing in Form-I-2, subject to the following conditions, namely:-

(a)      the container of such damaged material shall be conspicuously superscribed in red color with the word "Damaged" and also with sign "X".

(b)      the damaged fertiliser shall be moved from the godown within one week from the date of grant of certificate of reprocessing.][37]

Order - [23B. Disposal of Damaged and Expired stock of Bio-fertilisers/Organic fertilisers.-

(1)     Notwithstanding anything contained in this order where the stock of biofertiliser damaged during storage or expired or does not conform to the prescribed standard at dealer end or during transit from manufacturing unit to dealer end, such material shall be taken back by manufacturer or returned by dealer by intimating to the Notified authority within seven days, in case where the material is damaged during transit or in case where the material get expired, the manufacturer shall intimate the authority within seven days from the date of expiry for transacting the material for its disposal as per the procedure prescribed in sub-clause (6) of clause 26.

Provided that the material of such damaged material shall be conspicuously superscribed in red color with word damaged and also with sign "X";

(2)     Notwithstanding anything contained in this order where the stock of organic fertiliser damaged during storage or during transit and does not conform to the prescribed standard, such material shall be taken by manufacturer for reprocessing it by mixing with fresh biomass or in case where it is non-standard due to heavy metal content then the manufacturer immediately with draw the material for reprocessing by mixing with fresh biomass or such material shall be used in gardens, golf courses etc. or sent to landfills. If stock is at dealers end, it shall be taken back or returned to the manufacturer for disposal as mentioned above.

(3)     The manufacturer shall intimate to the Notified authority within seven days in case where the material is damaged during transit or, within seven days in case the material damaged or not of prescribed standard during storage at any dealer level or in storage godown:

Provided that such damaged material shall be conspicuously superscribed in red color with word damaged and also with sign "X".][38]

Order - 24. Manufacturers/Pool handling agencies to appoint officers responsible with compliance of the Order.

Every manufacturing organization, ***importer and pool handling agency shall appoint in that organization and in consultation with the Central Government, an officer, who shall be responsible for compliance with the provisions of this Order.

Order - 25. Restriction on sale/use of fertilisers.

(1)     No person shall, except with the prior permission of the Central Government and subject to such terms and conditions as may be imposed by such Government, sell or use fertiliser, for purposes other than fertilisation of soils and increasing productivity of crops.

Provided that the price of fertilisers permitted for sale for industrial use shall be no profit no loss price, excluding all subsidies at the production, import, handling or on sale for agricultural consumers;

Provided further that wherever customs or excise duties are chargeable, these may be added to the price so fixed.

Provided also that in the case of non-standard fertilisers, reductions shall be made from the no profit no loss price, indicated above, proportionate to the loss of nutrient contents.

(2)     Notwithstanding anything contained in sub-clause (1), no prior permission for use of fertiliser for industrial purposes shall be necessary when the fertiliser for such purposes is purchased from the Industrial dealer possessing a valid certificate of registration granted under clause 9.

(3)     Any person possessing a valid certificate of registration for Industrial dealer, unless such person is a State Government, a manufacturer/importer or a pool handling agency, shall not carry on the business of selling fertilisers for agricultural purposes, including a wholesale dealer or a retail dealer. However, in case of a State Government, a manufacturer or a importer or a pool handling agency possessing a valid certificate of registration for sale of fertiliser for industrial use, and also for sale of fertiliser for agricultural use, whether in wholesale or retail or both, shall not carryon the business of selling fertilisers both for Industrial use and agricultural use In the same premises.

VII. ENFORCEMENT AUTHORITIES

Order - 26.

Appointment of registering authority The State Government may, by notification in the Official Gazette, appoint such number of persons, as it thinks necessary, to be registering authorities for the purpose of this Order and may, in any such notification define the limits of local area within which each such registering authority shall exercise his jurisdiction.

Order - 26A. Notified Authority-

The State Government may, by notification in the Official Gazette, appoint such number of persons, as it thinks necessary, to be Notified Authorities for the purpose of this Order and define the local limits within which each such Notified Authority shall exercise his jurisdiction.

Order - 27. Appointment of inspectors.

The State Government, or the Central Government may, by notification in the Official Gazette appoint such number of persons, as it thinks necessary, to be inspectors of fertilisers for the purpose of this Order, and may, in any such notification, define the limits of local area within which each such inspector shall exercise his jurisdictions.

Order - 27A. Qualifications for appointment of fertiliser Inspectors.

No person shall be eligible for appointment as Fertiliser Inspector under this Order unless he possesses the following qualifications, namely:-

(1)     Graduate In agriculture or science with chemistry as one of the subjects, from a recognised university; and

(2)     Training or experience in the quality control of fertilisers and working in the State or Central Government Department of Agriculture.

Order - 27AA.[Regular training of Fertiliser Inspectors.

Every Fertiliser Inspector shall undergo training after every three years in the Central Fertiliser Quality Control and Training Institute or any Regional Fertiliser Quality Control Laboratory at Mumbai, Kalyani or Chennai.][39]

Order - 27B. Qualifications for appointment of fertiliser Inspectors for Biofertiliser and Organic Fertiliser.

No person shall be eligible for appointment as inspector of biofertiliser and Organic fertilizer under this Order unless he may possess the following qualifications, namely:

(1)     Graduate in agriculture or science with chemistry/microbiology as one of the subject; and

(2)     Training or experience in the field of quality control of biofertilisers/organic fertilizers.

Order - 28. Powers of Inspectors.

(1)     An inspector may, with a view to securing compliance with this Order:-

(a)      require any manufacturer, importer, pool handling agency, wholesale dealer or retail dealer to give any information in his possession with respect to the manufacture, storage and disposal of any fertilizer manufactured or, in any manner handled by him

(b)      draw samples of any fertiliser in accordance with the procedure of drawal of samples laid down in Schedule II. Provided that the inspector shall prepare the sampling details in duplicate In Form J, and hand over one copy of the same to the dealer or his representative from whom the sample has been drawn;

(ba) draw samples of any biofertilisers in accordance with the procedure of drawl of samples laid down in schedule III.

(bb) draw samples of any organic fertilisers in accordance with the procedure of drawl of samples laid down in schedule IV.

(c)      enter upon and search any premises where any fertiliser is manufactured/ Imported or stored or exhibited for sale, if he has reason to believe that any fertiliser has been or is being manufactured/imported, sold, offered for sale, stored, exhibited for sale or distributed contrary to the provisions of this Order;

 

(d)      seize or detain any fertiliser in respect of which he has reason to believe that a contravention of this Order has been or is being or is [attempted] to be committed;

 

(e)      seize any books of accounts or documents relating to manufacture, storage or sale of fertilisers, etc. in respect of which he has reason to believe that any contravention of this Order has been or is being or is about to be committed;

Provided that the Inspector shall give a receipt for such fertilisers or books of accounts or documents so seized to the person from whom the same have been seized;

Provided further that the books of accounts or documents so seized shall be returned to the person from whom they were seized after copies thereof or extracts thereform as certified by such person, have been taken.

(2)     Subject to the proviso to paragraphs (d) and (e) of sub-clause (1), the provisions of the Code of Criminal Procedure, 1973 (2 of 1974) relating to search and seizure shall, so far as may be, apply to searches and seizures under this clause.

Provided also that the inspector shall give the stop sale notice in writing to the person whose stocks have been detained and initiate appropriate action as per the provisions of this order within a period of twenty one days. If no action has been initiated by the inspector within the said period of twenty one days from the date of issue of the said notice, the notice of stop sale shall be deemed to have been revoked.

(3)     Where any fertiliser is seized by an inspector under this clause, he shall forthwith report the fact of such seizure to the collector whereupon the provisions of sections 6A, 6B, 6C, 6D and 6E of the Act, shall apply to the custody, disposal and confiscation of such fertilisers.

(4)     Every person, if so required by an inspector, shall be bound to afford all necessary facilities to him for the purpose of enabling him to exercise his powers under sub-clause (1).

Order - [28A. Appointment of officer for keeping the sample in custody

The State Government may, by notification in Official Gazette, appoints an officer not below the rank of Joint Director of Agriculture Department for keeping the samples in its custody and for sending the second part for analysis to National test House and the third part for referee analysis.][40]

Order - [28B. Sample drawn by the Inspector

(1)     Out of three parts made by the Inspector drawn under sub- clause (6) of clause 28, the first part shall be sent to any of the State Government notified lab by the state Inspector under intimation to the officer notified under clause 28 A and the second part and third part shall be kept in custody of officer nominated by the State Government.

(2)     The company or dealer, from whom sample is drawn may request to such authority within one week from the date of drawal of sample, to send the second part of the sample to any of the National Test House Laboratories on payment of fees as provided by the Central Government from time to time and in case, there is variation in the results of the first and second analysis, then the said authority invariably shall send the third part of the sample to Central Fertiliser Quality Control and Training Institute, Faridabad for final referee analysis.

(3)     In case where the sample is drawn by the Central Government Inspector then out of three parts made by the Inspector, the first part shall be sent to any of the Regional Quality Control Laboratory at Mumbai, Kalyani or Chennai and, the second part and third part shall be kept in custody of incharge of the Regional Fertiliser Quality Control Laboratory at Chennai, Kalyani or Mumbai as the case may be.

(4)     The company or dealer, from whom sample is drawn may request within one week to such authority to send the second part of the sample to any of the National Test House Laboratories on payment of fees as provided by the Central Government from time to time and in case, there is variation in the result of the first and second analysis, then such authority invariably send the third part of the sample to Central Fertiliser Quality Control and Training Institute, Faridabad for final referee analysis.

(5)     The referee analysis report received from the laboratory shall be treated as final.

(6)     In case, where the appeal of non- standard fertiliser under sub-clause (3) of clause 32 and sub -clause (3) of clause 32A have not been considered then the report of the regional fertiliser Quality Control Laboratory or the notified Fertiliser Testing Laboratory, as the case may be shall be treated as final.][41]

Order - [28C. Inspection Team

The Central Government shall constitute a Inspection team or teams headed by an officer not below the rank of Director or equivalent and comprising of four other officers not below the rank of Assistant Section Officer or equivalent:

Provided that one of the member shall possess the minimum qualification and training prescribed for Fertiliser Inspector in clause 27 A of FCO.

Order - 28D. Power of Inspection Team

The Inspection team shall exercise all the power assigned to Fertiliser Inspector under item (a), (b), (c), (d) and (e) of sub-clause (1) of clause 28 and sub-clauses (2), (3), and (4) of clause 28 of the Fertiliser (Inorganic, Organic or Mixed) (Control) Order, 1985.][42]

VIII. ANALYSIS OF SAMPLES

Order - 29. Laboratory for analysis.

[43][(1) A fertilizer sample drawn by an Inspector [44][Inspection team constituted by Central Government], shall be analysed in accordance with the instructions contained in Schedule II-

(a)      in regional fertilizer control laboratories at Mumbai, Chennai or Kalyani (Kolkata) and the National Test House Laboratories at Mumbai, Chennai, Kolkatta, Ghaziabad and Jaipur as per sub- clause (2) of clause 28B; or

(b)      in any laboratory notified for this purpose by the State Government with the prior approval of the Central Government and the National Test House Laboratories at Mumbai, Chennai, Kolkatta, Ghaziabad and Jaipur as per sub- clause (4) of clause 28B;]

(1A) Biofertiliser samples, drawn by an inspector, shall be analyzed in accordance with the instructions contained in Schedule III in the [45][Regional centre of Organic farming at Bengaluru, Bhubaneswar, Ghaziabad, Imphal, Jabalpur, Nagpur and Panchkula] or in any other laboratory notified by the Central or State Government.

(1B) Organic fertiliser samples, drawn by an inspector, shall be analyzed in accordance with the instructions contained in Schedule IV in the [46][Regional centre of Organic farming at Bengaluru, Bhubaneswar, Ghaziabad, Imphal, Jabalpur, Nagpur and Panchkula] or in any other laboratory notified by the Central or State Government.

[47][(1C) A biostimulant sample drawn by an inspector shall be analysed in accordance with the procedure contained in Part C of Schedule VI in the Central Fertiliser Quality Control and Training Institute, Faridabad or its regional laboratories or in any other laboratory notified for this purpose by the State Government with prior approval of Central Government.]

(2)   Every laboratory referred to in sub-clause (1) shall, in order to ensure accurate analysis, of fertiliser samples, possess minimum equipment and other laboratory facilities, as may be specified from time to time by the Controller in this behalf.

[48][(3) Every fertiliser testing laboratories specified or notified by the State Government under sub-clause (1) shall be required to obtain the accreditation of the National Accreditation Board for Testing and Calibration Laboratories within a period of [49][six months] from 28th day of September, [50][2023].]

Order - 29A. Qualifications for appointment of fertiliser analyst in the fertiliser control laboratories.

No person shall be eligible for appointment as fertiliser analyst for analysis of fertiliser samples in the laboratories notified under clause 29 of the Order, unless he possesses the following qualifications, namely:-

(1)     graduate in Agriculture or Science with chemistry as one of the subjects from a recognised university; and

 

(2)     training In fertiliser quality control and analysis at Central Fertilizer Quality Control and Training Institute, Faridabad.

Provided that the fertiliser analysts appointed before the commencement of this Order, who do not possess the requisite training, shall undergo prescribed training, within a period of three years, in the Central Fertiliser Quality Control " and Training Institute, Faridabad from the date of commencement of this Order.

Order - 29AA.[Regular training of Fertiliser Analysts.

Every Fertiliser Analyst shall undergo training after every three years in the Central Fertiliser Quality Control and Training Institute or any Regional Fertiliser Quality Control Laboratory at Mumbai, Kalyani or Chennai.][51]

Order - 29AB.

[52][No person shall be eligible to be notified as analyst for analysis of sample of Biofertiliser, Organic fertiliser and non edible de-oiled cake fertilizers in the laboratories notified under sub clauses (1A) and (1B) of clause 29, unless the analyst possesses the following qualifications, namely:-

(a)      Postgraduate degree in Agriculture Chemistry and Soil Science or Microbiology or Plant Pathology or Chemistry or Biotechnology or Horticulture or Bio-Engineering;

(b)      training in analysis of Biofertiliser, Organic fertiliser and non edible de-oiled cake fertilizers at National Centre of Organic Farming or at a recognized laboratory or Institute:

Provided that the analyst who has been appointed prior to the date of commencement of this Order, but does not possess the requisite training or experience in analysis of Biofertiliser, Organic fertiliser and non edible de-oiled cake shall undergo prescribed training at the National Centre of Organic Farming or at a recognized lab or Institute within a period of three years from the date of such commencement.]

Order - [29B.

The Central Fertiliser Quality Control and Training Institute, Faridabad shall be designated as referee laboratory for the purpose of analysis of any sample of fertiliser under sub-clauses (1), (2) and (3) of clause 28 B.][53]

Order - [29C. Laboratories for referee analysis of Biofertiliser.

(1)     [54][Regional centre of Organic Farming at Bengaluru, Bhubaneswar, Ghaziabad, Imphal, Jabalpur, Nagpur and Panchkula] and every laboratory referred to in clause 29 (1A) shall be designated as referee laboratory for the purpose of analysis of any sample of Biofertiliser:

Provided that no such laboratory which carried out the first analysis of fertiliser sample shall be so designated in respect of that sample:

Provided further that in respect of any sample the analysis of which has been challenged, may be sent for referee analysis to any one of the other laboratories except those which are located in the state or where the first analysis has been done: 

Provided that [55][Regional centre of Organic Farming at Bengaluru, Bhubaneswar, Ghaziabad, Imphal, Jabalpur, Nagpur and Panchkula] shall be considered as one group of laboratories and a sample first analysed by any one of them, shall not be sent for referee analysis to any other in that group, but only to any other laboratory notified by a State Government or Central Government.][56]

(2)     Notwithstanding anything contained in this Order, the Appellate Authority as specified in sub-clause 1 of clause 32A in case of sample collected by the state Government laboratory, or the Controller, in case of sample collected by [57][Regional centre of Organic Farming at Bengaluru, Bhubaneswar, Ghaziabad, Imphal, Jabalpur, Nagpur and Panchkula], as the case may be, shall decide and send, one of the two remaining samples, for reference analysis as provided under sub-clause (1).

Order - 29D. Laboratories for referee analysis of Organic fertilizer.

(1)     [58][Regional centre of Organic Farming at Bengaluru, Bhubaneswar, Ghaziabad, Imphal, Jabalpur, Nagpur and Panchkula] and every laboratory referred to in clause 29 (1A) shall be designated as referee laboratory for the purpose of analysis of any sample of Organic fertiliser Provided that no such laboratory which carried out the first analysis of fertiliser sample shall be so designated in respect of that sample;

Provided further that in respect of any sample the analysis of which has been challenged, may be sent for referee analysis to any one of the other laboratories except those which are located in the state or where the first analysis has been done;

Provided that [59][Regional centre of Organic Farming at Bengaluru, Bhubaneswar, Ghaziabad, Imphal, Jabalpur, Nagpur and Panchkula] shall be considered as one group of laboratories and a sample first analysed by any one of them, shall not be sent for referee analysis to any other in that group, but only to any other laboratory notified by a State Government or Central Government.

(2)     Notwithstanding anything contained in this Order, the Appellate Authority as specified in sub-clause 1 of clause 32 A in case of sample collected by the State Government laboratory, or the Controller, in case of sample collected by [60][Regional centre of Organic Farming at Bengaluru, Bhubaneswar, Ghaziabad, Imphal, Jabalpur, Nagpur and Panchkula], as the case may be, shall decide and send, one of the two remaining samples, for reference analysis as provided under sub-clause (1)]

Order - 30. Time limit for analysis, and communication of result.

(1)  Where sample of a fertlliser has been drawn, the same shall be dispatched alongwith a memorandum in Form K and in case of Organic fertilizers and Biofertilisers in Form KI to the laboratory for analysis within a period of [61][three working days] from the date of its drawal.

[62][(2) The laboratory shall analyse the sample and forward the analysis report to the authority specified in the memorandum referred to in sub-clause (1) in the following manner, namely:-

(a)      in case of fertiliser, other than biofertilizer, organic fertilizer and de oiled cake fertilizer, the analyzing report shall be in Form L and forwarded within fifteen days;

(b)      in case of the sample of organic fertilizer, the analysis report shall be in Form L1, and forwarded within thirty days;

(c)      in case of biofertilizer, the analysis report shall be in Form L2 and forwarded within forty-five days;

(d)      in case of deoiled cake fertilizer, the analysis report shall be in Form L3 and forwarded within thirty days from the date of receipt of sample in the laboratory.]

(3)   The authority to whom the analysis report is sent under sub-clause (2) shall communicate the result of the analysis to the dealer/manufacturer/Importer/pool handling agency from whom the sample was drawn within [63][seven days] from the date of receipt of the analysis report of the laboratory.

IX. MISCELLANEOUS

Order - 31.Suspension, Cancellation Or Debarment.

(1)     A Notified Authority, registering authority, or as the case may be, the controller may, after giving the authorized dealer or the holder of certificate of registration or certificate of manufacture or any other certificate granted under this Order, an opportunity of being heard, suspend such authorization letter or certificate or debar the dealer from carrying on the business of fertilizer on one or more of the following grounds, namely:-

(a)      that the authorization letter or certificate of registration or certificate of manufacture, as the case may be, has been obtained by wilful suppression of material facts or by misrepresentation of relevant particulars:

(b)      that any of the provisions of this Order or any terms and condition of the Memorandum of Intimation or certificate of registration or the certificate of manufacture, as the case may be, has been contravened or not fulfilled:

Provided that while debarring from carrying on the business of fertiliser or canceling the certificate, the dealer or the certificate holder thereof may be allowed for a period of thirty days to dispose of the balance stock of fertilizers, if any, held by him:

Provided further that the stock of fertilizer lying with the dealer after the expiry of the said period of thirty days shall be confiscated.

(2)     Where the contravention alleged to have been committed by a person is such as would, on being proved, justify his debarment from carrying on the business of selling of fertilizer or, cancellation of authorization letter or certificate of registration or certificate of manufacture or any other certificate granted under this Order to such person the Notified Authority or registering authority or, as the case may be, the controller may, without any notice, suspend such certificate, authorization letter, as an interim measure:

Provided that the registering authority, Notified Authority or, as the case may be, the controller shall immediately furnish to the affected person details and the nature of contravention alleged to have been committed by such person and, after giving him an opportunity of being heard, pass final orders either revoking the order of suspension or debarment within fifteen days from the date of issue of the order of suspension:

Provided further that where no final order is passed within the period as specified above, the order of interim suspension shall be deemed to have been revoked without prejudice, however, to any further action which the registering authority, Notified Authority or, as the case may be, the controller may take against the affected person under sub-clause (1).

(3)     Wherever an authorization letter or certificate is suspended, cancelled or the person is debarred from carrying on the business of fertiliser, the Notified Authority, registering authority, or as the case may be, the Controller shall record a brief statement of the reasons for such suspension or, as the case may be, cancellation or debarment and furnish a copy thereof to the person whose certificate or authorization letter has been suspended or cancelled or business has been debarred.

(4)     Wherever the person alleged to have committed the contravention is an industrial dealer, the Notified Authority may take action against the holder of such certificate of registration under sub-clause (1) and sub-clause (2):

Provided that where such certificate is suspended or cancelled, the Notified Authority shall, within a period of fifteen days from the date of issue of such order of suspension or cancellation, furnish to the controller also, besides sending the same to the person whose certificate has been suspended or cancelled, a detailed report about the nature of contravention committed and a brief statement of the reasons for such suspension or, as the case may be, cancellation:

Provided further that the controller, shall, in case of the order for suspension passed by the Notified Authority, on receipt of the detailed report and after giving the person an opportunity of being heard, pass final order either revoking the order of suspension or canceling the certificate of registration, within fifteen days from the date of receipt of the detailed report from the Notified Authority, failing which the order of interim suspension passed by the Notified Authority shall be deemed to have been revoked, without prejudice however, to further action which the controller may take against the holder of certificate under sub-clause (1):

Provided also that the order of cancellation passed by the Notified Authority shall remain effective as if it had been passed by the controller till such time the Controller, on receipt of the detailed report from the Notified Authority, and if deemed necessary, after giving the person a fresh opportunity of being heard, pass the final order either revoking or confirming the order of cancellation.

Order - 32. Appeals at Central Government level.

(1)     In any State, where the fertiliser allocation is made by the Central Government under this Order and if the suspension or cancellation of authorization letter of the manufacturer and or pool handling agency or debarment of business, in any way, has an effect of dislocating the said allocation and if the Central Government is of the opinion that it is necessary or expedient so to do for maintaining the supplies, may direct the concerned State Government to furnish detailed report about the nature of contravention and a brief statement of the reasons for such suspension or cancellation and pass such order as it may think fit, confirming, modifying or annulling the order of State Government

Provided that if the report called by the Central Government is not received from the State Government within a period of fifteen days from the date of issue of the communication, the Central Government may decide the case without the report, on merit.

(2)     [64][****]

(3)     [65][in cases where the company or dealer has not applied for the second analysis due to some valid reason then the company or dealer may made an appeal to the Controller, as the case may be, within seven days from the date of receipt of analysis report of first part of the sample and the Controller shall decide on the grounds of the facts whether the matter qualifies to be considered for third analysis.]

Provided that in case where the sample is declared as non-standard both in the first analysis report and referee analysis report but in different parameters or there is wide variation in the analysis report of first analysis and referee analysis, as the case may be, the aggrieved person may appeal to the controller for third analysis within thirty days from the date of receipt of the report of referee analysis on payment of such charges as may be required for such analysis.

(4)     The Controller after providing an opportunity to the aggrieved party of being heard may send the third sample for analysis to the Laboratory and specified under sub-clause (3) of clause 29 B.

(5)     The result of the third analysis referred to in sub-clause (4) shall supersede the first analysis and referee analysis report and shall be treated as final.]

Order - 32A. Appeal at the State Government level.

(1)     The State Government shall, by notification in the Official Gazette, specify such authority as the Appellate authority before whom the appeals may be filed within 30 days from the date of the order appealed against by any person, except by an industrial dealer, aggrieved by any of the following Orders or action of registering authority or a Notified Authority, namely:

(i)       Refusing to grant a certificate of manufacture for preparation of mixture of fertilisers or special mixture of fertilizers; or

 

(ii)      Suspending or canceling a certificate of manufacture; or

 

(iii)     Suspending or canceling authorization letter or debarring from carrying on the business of selling of fertilizer, or

 

(iv)    non-issuance of certificate of manufacture within the stipulated period; or

(v)      non-issuance of amendment in authorization letter within the stipulated period.

(2)     [66][****]

(3)     [67][In cases where the company or dealer has not applied for the second analysis due to some valid reason then the company or dealer may made an appeal in the Fertiliser (Inorganic, Organic or Mixed) (Control) Order, 1985 to the Appellate authority and the Appellate Authority shall decide on the grounds of the facts whether the matter qualifies to be considered for third analysis.]

(4)     The appellate authority after providing an opportunity to the aggrieved party of being heard may send the third sample for analysis to the laboratory specified under sub-clause (3) of clause 29B.

(5)     The result of the third analysis referred to in sub-clause (4) shall supersede the report of first analysis and referee analysis and shall be treated as final.]

Order - 33. Grant of duplicate copies of [authorization letter or Certificate of manufacture] certificate of registrations, etc.

Where [authorization letter or] a certificate of registration or a certificate of manufacture or any other certificate granted or, as the case may be, renewed under this Order is lost or [defaced, the notified authority] registering authority or, as the case may be, the Controller may, on an application made in this behalf, together with the fee prescribed for this purpose under clause 36, grant a duplicate copy of such certificate.

Order - 34. Amendment of certificate of registration.

The Notified Authority, registering or controller, as the case may be, may, on application being made by the holder of an authorization letter, a certificate of registration or certificate of manufacture, together with the fee prescribed for the purpose under clause 36, amend an entry in such authorization letter, certificate of registration or certificate of manufacture as the case may be.

Order - 35. Maintenance of records and submission of returns, etc.

(1)     The controller may by an order made in writing direct the dealers. manufacturers/ importers, and pool handling agencies:-

(a)      to maintain such books of accounts, records, etc. relating to their business in Form 'N' [68][or maintain digital stock register in the form which clearly exhibits the date wise stock position, opening balance, receipts during the day, sales during the day and closing stock]. And

(b)      to submit to such authority, returns and statements in such form and containing such information relating to their business and within such time as may be specified in that order.

(2)     Where a person holds certificates of registration for retail sale and wholesale sale of fertilisers, he shall maintain separate books of accounts for these two types of sales made by him.

(3)     Where a State Government, a manufacturer, +an importer and a pool handling agency holds valid certificates of registration for sale of fertilisers in, wholesale or retail or both and also for sale for industrial use, he shall maintain separate books of accounts for these two or three types of sales made by him.

(4)     Every importer shall inform the Director of Agriculture of the State in which he intends to discharge the imported fertilizer, under intimation to the Central Government, before the import is made or within a period of fifteen days after an indent for import is placed, the following details, namely ;-

(i)       name of fertilizer

 

(ii)      name of country of import.

 

(iii)     name of manufacturer.

 

(iv)    quantity to be imported

 

(v)      date of arrival of the consignment.

 

(vi)    name of the discharge port.

 

(vii)   other information

Order - 36. Fees.

(1)     The fees payable for grant, amendment or renewal of a [n authorization letter] or certificate of registration or certificate of manufacture [69][or certificate of authorisation for sale of non-standard fertiliser or certificate for reprocessing of fertiliser damaged during storage] a duplicate of such certificates or, renewal thereof under this Order shall be such as the State Government may, from time to time fix, subject to the maximum fees fixed for different purposes by the Central Government and different fees may be fixed for different purposes or for different classes of dealers or for different types of mixtures of fertiliser or special mixture.

 

(2)     The authority to whom and the manner in which the fee fixed under sub-clause (1) shall be paid, shall be such as may be specified by the State Government by notification in the Official Gazette.

 

(3)     Any fee paid under sub-clause (1) shall not be refundable unless the grant or renewal of any certificate of registration or certificate of manufacture or duplicate copy of such certificate or renewal under this Order has been refused.

 

(4)     The fees payable for grant, amendment, renewal or duplicate copy of certificate of registration for industrial dealer and the authority to whom and the manner in which such fee shall be paid, shall be such as may be specified by the Controller from time to time by notification in the Official Gazette*.

Order - 37. Service of orders and directions.

Any order or direction made or issued by the controller or by any other authority under this order shall be served in the same manner as provided in sub-section (5) of section 3 of the Act.

Order - 38. Advisory Committee.

(1)     The Central Government may by notification in the Official Gazette and on such terms and conditions as may be specified in such notification, constitute a Committee called the Central Fertiliser Committee consisting of a Chairman and not more than ten other persons having experience or knowledge in the field, who shall be members of the Committee, to advise the Central Government regarding:

(i)       inclusion of a new fertiliser, under this Order;

 

(ii)      specifications of various fertilisers;

 

(iii)     grades/formulations of physical/granulated mixtures of fertilisers that can be allowed to be prepared in a State;

 

(iv)    requirements of laboratory facilities in a manufacturing unit, including a unit manufacturing physical/granulated mixtures of fertilisers;

 

(v)      methods of drawal and analysis of samples.

 

(vi)    any other matter referred by the Central Government to the Committee.

(2)     The Committee may, subject to the previous approval of the Central Government, make bye-laws fixing the quorum and regulating its own procedure and the conduct of all business to be transacted by it.

(3)     The Committee may co-opt such number of experts and for such purposes or periods as it may deem fit, but any expert so co-opted shall not have the right to vote.

(4)     The Committee may appoint one or more sub-committees, consisting wholly of members of the Committee or or partly of the members of the Committee and partly of co-opted members as it thinks fit, for the purpose of discharging such of its functions as may be delegated to such subcommittee or sub-committees by the Central Fertiliser Committee.

(5)     The State Government may by notification in the Official Gazette and on such terms and conditions as may be specified in such notification, constitute a Committee called the State Fertiliser Committee consisting of a Chairman and not more than 4 other members, having experience or knowledge in the field, including a representative from State Agricultural University, the Fertiliser Industry and Indian Micro Fertilisers Manufacturers Association to advise the State Government regarding the grades/formulations of *mixture or of fertilisers.

Order - [38A. Central Biostimulant Committee.

(1)     The Central Government may, by notification in the Official Gazette, constitute a Committee to be called 'Central Biostimulant Committee' with the Agriculture Commissioner as its Chairperson and seven other members, subject to such terms and conditions, as may be specified therein.

(2)     The Central Biostimulant Committee shall advise the Central Government on the following issues, namely:

(i)       inclusion of a new biostimulant;

 

(ii)      specifications of various biostimulants;

 

(iii)     methods of drawing of samples and its analysis;

 

(iv)    minimum requirements of laboratory;

 

(v)      method of testing of biostimulants;

 

(vi)    any other matter referred to the Committee by the Central Government.

(3)     The Committee may, subject to the previous approval of the Central Government, make bye-laws fixing the quorum and regulating its own procedure and the conduct of all business to be transacted by it.

(4)     The committee may co-opt such number of experts and for such purposes or periods as it may deem fit, but any expert so co-opted shall not have the right to vote.

(5)     The committee may appoint one or more sub-committees, consisting wholly of its members or partly of its members and co-opted members, as it thinks fit, for the purpose of discharging such for its functions as may be delegated to such sub-committee.

(6)     The Central Biostimulants Committee shall frame guidelines laying down the requirements of toxicology testing and other related tests.][70]

Order - 39. Repeal and saving.

(1)     The Fertiliser Control) Order, 1957 is hereby repealed except as respects things done or omitted to be done under the said Order before the commencement of this Order.

(2)     Notwithstanding such repeal, an order made by any authority, which is in force immediately before the commencement of this Order and which is consistent with this Order, shall continue in force and all appointments made, prices fixed, certificates granted and directions issued under repealed Order and in force immediately before such commencement shall likewise continue in force and be deemed to be made, fixed, granted or issued in pursuance of this Order till revoked.

[71][Schedule I

Part A

[See clause 2 (h) and (q)]

SPECIFICATIONS OF FERTILISERS

 

 

 

 

 

 

 

 

 

 

 

 

[122][3. Chelated Zinc as Zinc-Glycine (liquid)

4. Chelated Calcium as Calcium-Glycine (liquid)

5. Chelated Boron as Boron-Glycine (liquid)

[123][6. NK 6:0:18 Fortified with Calcium, Magnesium & Boron (suspension)

7. NPK 11: 11: 8 Fortified with Zinc & Boron (suspension)

8. Calcium Nitrate Fortified with Magnesium (suspension)

[124][9. Potassium Thiosulphate (K₂S₂O₃)

10. Calcium Thiosulphate (CaS₂O₃)

[125][11. Fortified NP (7-21-0) Liquid

12. Fortified Calcium Suspension

 

 

 

 SCHEDULE II

(See clause 28 (1) (b) and 29)

PART A

PROCEDURE FOR DRAWAL OF SAMPLES OF FERTILIZERS

1. General requirement of sampling

In drawing samples, the following measures and precautions should be observed.

(a)      Samples shall not be taken at a place exposed to rain/sun;

 

(b)      The sampling instruments shall be clean and dry when used;

 

(c)      The material being sampled, the sampling instrument and the bags of samples should be free from any adventitious contaminations;

 

(d)      To draw a representative sample, the contents of each bag selected for sampling should be mixed as thoroughly as possible by suitable means;

 

(e)      The sample should be kept in suitable, clean dry and air tight glass or screwed hard polythene bottle of about 400 gm capacity or in a thick gauged polythene bag. This should be put in a cloth bag which may be sealed with the Inspector's seal after putting inside the detailed description as specified in Form "J" Identifiable details may also be put on the cloth bag like sample No./Code No. or any other details which enables its identification;

 

(f)       Each sample bag should be sealed air tight after filling and marked with details of sample, type and brand of fertilizer, name of dealer/manufacturer/importer and the name of Inspector who has collected sample.

2. Sampling from bagged material

(i)       Scale of sampling

(a)      Lot (for manufacturers/importers)

All bags in a single consignment of the material of the same grade and type drawn from a single batch of the manufacturer/importer shall constitute a lot. If a consignment is declared to consist of different batches of manufacturer/import, all the bags of each batch shall constitute a separate lot. In the case of a consignment drawn from a continuous process,2000 bags (or 100 tones) of the material shall constitute a lot.

(b)      Lot (for dealers)

The lot is an identifiable quantity of same grade and type of fertilizer stored at an identifiable place subject to a maximum limit of 100 tones. The lot shall be identified by the inspector based on visible appearance of bags, their packing and storage conditions. The stock of less than 100 tones with a dealer may also constitute one or more lots, if the material (fertilizer) of different sources and brand is available in such quantities.

(c)      Selection of bags for sampling

The number of bags to be chosen from a lot shall depend upon the size of the lot as given in the table below.

All the bags of a lot should be arranged in a systematic manner. Start counting from any bag randomly, go on counting as 1,2,3,- up to r and so on, r being equal to the integral of N/n. Thus every rth bag counted shall be withdrawn and all bags shall constitute the sample bags from where the sample is to be drawn for preparing a composite sample.

(ii)      Sampling from big godowns/high stackings.

If the procedure given in Para 2(i) (c) is not possible to be adopted, the sample should be drawn from the randomly selected fertilizer bags from different layers, from top and from all open side in a zig fashion.

(iii)     Sampling from small godowns

All the fertilizer bags of the same grade and type of each manufacturer though received on different dates shall be segregated and properly stacked. All bags of same grade and type of fertilizer manufactured by a particular manufacturing unit may be considered as one lot based on their physical conditions and the sample shall be drawn as per procedure laid in Para 2(i) (c) and 4.

(iv)    Sampling from damaged stock.

(a)      In case of torn or lumpy bags, damaged fertilizer bags or sweepings, the stock should be arranged according to identifiable lots. From each lot the number of bags shall be selected as per procedure 2(i)(c). If the bags allow the use of sampling probe conveniently, the samples should be drawn by sampling probe.

(b)      In case it is not possible to use the sampling probe, the bags may be opened and fertilizer material mixed together uniformly by hammering the big lumps or putting pressure, if required and then samples drawn by using suitable sample device.

3. Sampling probe

(i)       An appropriate sampling instrument to be used by the Inspectors for collection of a representative sample is called sampling probe. The probe may comprise of a slotted single tube with soil cone tip made of stainless steel or brass. The length of the probe may be approximately 60 to 65 cms and the diameter of the tube may be approximately 1.5 cm and the slot width 1.2 to 1.3 cms. The probe may be use if the physical condition of the fertilizers and the packing material permits it use. 

(ii)      In case of High Density Polyethylene packing and also when the fertilizer material is not in free flowing condition, the use of sampling probe may not be possible. In such a case, selected bags for drawing samples may be opened and the fertilizers may be taken out of the bags and spread on a clean surface and samples drawn with the help of a suitable Sampling device which may be made of stainless steel or brass cup.

4. Drawal of samples from bags.

(i)       Drawal of sample and preparation of composite samples. Draw, with an appropriate sampling instrument, (sampling probe) small portions of the material from the selected bags as per procedure in para 2(i) (b) 2(ii) 2(iii)and 2 (iv) (a). The sampling probe shall be inserted in the bag from one corner to another diagonally and when filled with fertilizer, the probe is withdrawn and fertilizer is emptied in a container/or on polythene sheet/or on a clean hard surface and made into one composite sample.

(ii)      If the bags do not permit the use of sampling probe, empty the contents of the bags on a level, clean and hard surface and draw a composite sample by the process of quartering as described under para 3 (ii) or 5.+(iii) In case of chelated micro-nutrients and mixtures of micro-nutrients, the three identical containers of the batch, grade, type and manufacturer, shall be selected which shall constitute the composite samples, provided it is not possible to draw a composite sample of the size given under para 4A (iii)."

4A. Weight of one sample

One sample of fertilizer shall have the approximate weight, as specified below:-

                              (i)          For straight micro-nutrient fertilizers- 100gms.

                             (ii)         For chelated micro-nutrient fertilizers and 50gms or mixtures of micro-nutrients the maximum  packing size of similar quantity.

                            (iii)         For other fertilizer and mixtures of fertilizers 400 gms.

[127][(iv) For 100 % Water Soluble fertiliser and 100% water soluble Mixture of fertiliser 100g.]

5. Preparation of composite sample

If the composite sample collected from the different selected bags is large than required weight, its size shall be reduced by method of quartering as detailed below:-

Spread the composite sample on a level, clean, hard surface, flatten it out and divide it into four equal parts. Remove any diagonally opposite parts. Mix the tow remaining parts together to form a cone, flatten out the cone and repeat the operation of quartering till a composite sample of required weight is obtained.

6. Preparation of test sample and reference sample

              (i)          The composite sample obtained above shall be spread out on a clean, hard surface and divided into three approximately equal proportions + each of the weight as specified in Para 4A. Each of these samples shall constitute the test sample.

             (ii)         Each test sample shall be immediately transferred to a suitable container as defined under para 1(e). The slip with detailed description may be put inside the sample bag. Each bag shall also be properly labeled as mentioned in Para 1(f)

            (iii)         Each test sample container shall then be sealed with the seals of the inspector. If possible, seal of the manufacturer/importer/dealer or purchaser as the case may be, may also be affixed.

            (iv)        [128][****]

7. Sampling from the bulk fertilizers in ships, bulk carriers and bulk containers.

              (i)          Sampling equipments

(a)      Sampling cup

The sampling cup can be fabricated from non-corrosive metal, Inside dimensions of cup mouth may be 3/4" X 10" as per he diagram of the sampling cup given in Figure -1.

(b)      Sampling probe for bulk fertilizers.

The sampling probe should be made of non-corrodable material such as stainless steel or brass. It may be slotted double tube with solid cone tip having a length of about 4 1/2'-5' and diameter of about 1 1/4" to 1 1/2".

[129][(c) Sampling cup or scoop:

The samples from the wharf or silo, as the case may be, can be collected by a sampling cup or a suitable scoop made of stainless steel or brass.]

             (ii)         Sampling procedure

(a)      Drawal of samples from the ship of bulk fertilizers

A.        Sampling from conveyor belt.

When the material is unloaded from the ships transported to temporary/storage godowns through conveyor belts, the sample can be drawn by passing the sampling cup through the entire stream of material as the material drops from a transfer belt or spout. The long slot in the top of sampling cup should be perpendicular to the falling stream. pass the cup through the complete stream at a uniform speed, so that the cup will collect approximately equal amounts in each pass but will never overflow.

A minimum of 10 equally timed and speed stream must be taken during the transfer operation. However, the stream samples are not applicable unless uniform continuous flow of fertilizer is maintained for more than 3 minutes while lot is being sampled.

B.        [130][Sampling from ship

1.        Draw the samples, from the fertilizer being discharged from the ship on the wharf or silo as the case may be, periodically at the regular interval of five hours on first and last day of discharge and three hours on intermediate days. All the samples drawn on a particular day shall be mixed together to make day composite sample. If the day composite sample is larger than required weight, its size shall be reduced by method of quartering as described in Paragraph 5 of Schedule II of Part A.

2.        Then the ship composite sample shall be prepared by mixing part of each day composite. Further test sample and reference sample shall be prepared as given in Paragraph 6 of Schedule II of Part A.]

(b)      Drawal of samples from bulk carriers-trucks etc. The sample can be drawn as per vertical probing procedure of Association of Official Analytical Chemists. The sampling probe should be about 4 1/2' to 5' length. Draw 10 Vertical cuts from the following locations relative to the entire top of the conveyance. The 10 vertical cores are combined into a composite sample.

(c)      Drawal of samples from bulk material in storage.

 

(A)     The bulk storage piles (level or flat) up to 100 tones could be sampled as per Figure 2. Take 10 cores to the maximum possible depth of the probe from the position indicated in the Figure 2 and cores are composited.

(B)     A one sided or slopped pile may be sampled at the points illustrated in Figure3. Withdraw one vertical core of material from location 1 & 6 and two cores at locations 2, 3,4 & 5 composite all the probe samples and prepare the composite sample for analysis as per procedure laid down in para 1,5 & 6. (Figure 2- Sample points for coned or ridged pile)

[131][(d) Drawl of samples from containers

(1)     Minimum 5 bags shall be selected randomly from each container.

(2)     In case of large number of containers containing similar material, the containers shall be selected randomly as per following criteria:

(3)     The samples shall be drawn from the bags selected from each container as per the procedure given in Paragraph 4 of Schedule II of Part A. All the samples drawn from each bag of the selected container shall be mixed together to make container composite sample. If the container composite sample is larger than required weight, its size shall be reduced by method of quartering as described in Paragraph 5 of Schedule II of Part A.

(4)     All the container composite samples shall be mixed together and test sample and reference sample shall be prepared as given in Paragraph 6 of Schedule II of Part A.]

8. Method of sampling of anhydrous ammonia

(i)       Scope

This method is for use obtaining samples of anhydrous ammonia. The method is based on the assumption that the material to be sampled is as claimed and contains only a small amount of impurity primarily water. It is recommended that duplicate samples be taken form each tank or vessel sampled.

(ii)      Apparatus

(a)      Tubes for sampling tubes, heat resistant glass, conical centrifuge type 200ml with lower 100 ml graduated from 0.2 ml in 0.05 ml divisions, 2-4 ml in 0.1 division, 4-10 ml in 0.5 ml divisions and 10-100 ml in 1.0mldivisions. Tube type is shown in figure 5.

 

(b)      Stoppers for tubes, rubber, with bent tube vent as in Figures 5.

 

(c)      Samples carrier, constructed of plywood or aluminum as in Figure 5.

 

(d)      Sampling line and connection assembly constructed as in Figure 4, with flexible steel sampling nose 48" long, 1/4" NPT coupling at each end and 1/8" insulated steel tubing delivery tip at one end.

 

(e)      Sample tube adapter, constructed from rubber stopper and 6mm D. D. glass or steel tubing as in Figure 5.

 

(f)       Protective equipment: Rubber or other non-porous gloves, offering complete protection to the hands lower arms, full coverage goggles or approved gas mask.( Figure 4)

(iii)     Reagents

Charcoal, reagent, 14-20 mesh.

Note: If the sample is expected to contain excessive amount of water (one percent or more) one piece of the charcoal may be added to each tube before introduction of the sample

(iv)    Procedure

(a)      Place two dry, clean sampling tubes in the sample carrier

 

(b)      Connect the sampling line connection assembly to the unloading valve of the tank, vessel, or line to be sampled.

 

(c)      Open the valves slowly and purge the sampling line connection assembly thoroughly by venting 3 to 4 liters of ammonia. Close the sample line globe valve.

 

(d)      Remove the vented stoppers from the tubes and insert the adopter end of the sampling line connection assembly.

 

(e)      Open the sample line valve and slowly fill the sampling tube to the100ml mark, close the sample line valve.

 

(f)       Remove the sampling line adopter and insert the vented stopper in the sampling tube.

 

(g)      Repeat steps, d, e, and f and fill the second tube.

 

(h)     close tank discharge valve and remove the sampling line connection assembly.

 

(i)       Either know or note the vessel, container, or line pressure of material sampled.

 

(j)       Tag the collected samples for identification and submit to the laboratory for processing by following methods in this section

(v)      Precaution

(a)      Liquid anhydrous ammonia causes severe burns on contact. It evaporates readily releasing the gas which may cause varying degrees of irritation of the skin and mucus membrane and may injure severely the respiratory mucosa with possible fatal outcome.

 

(b)      Avoid contacting liquid ammonia. In case of contact, immediately flush the affected parts with plenty of water for atleast 15 minutes. Get medical attention at once in case of burns, especially to the eyes, nose and throat, or if the victim is unconscious.

 

(c)      Ammonium gas in concentrations of 6,000 to 10,000 ppm (by volume) is lethal within a few minutes. Irrigation of the eyes, respiratory tract and throat results from concentrations as low as 500 to 1,000 ppm' a concentration of 2,000 ppm produces convulsive coughing and may be fatal after a short exposure i.e. less than half an hour. The maximum concentration tolerated by the skin for more than few seconds is 2 percent (i.e. when suitable respiratory protection is worm) The maximum allowable concentration for 8 hour working exposure is 50 ppm. This is the least detectable order.

 

(d)      Obtain medical attention if exposure to the gas produce distress of any type.

 

(e)      Rubber or other no porous gloves, offering complete protection to the hands and lower arms must also be worn to protect the eyes unless an approved gas mask is used. The gas mask need only to be used if sampling can not be done without possible inhalation of the vapours.

PART B

METHOD OF ANALYSIS OF FERTILIZERS

1. Preparation of sample for analysis in the laboratory

(i)       Procedure.

(a)      Reduce gross sample to quantity sufficient for analysis or grind not < 250 Gm of reduced sample without previous sieving.

 

(b)      For fertilizer materials and moist fertilizer mixtures, that form a paste on putting pressure, grind in porcelain pestle and mortar to pass sieve with 1mm circular openings or No. 20 standard sieve.

 

(c)      For dry mixtures that tend to segregate, grind in a porcelain pestle and mortar to pass No. 40 standard sieve [132][in case of Potassium Magnesium Calcium Sulphate, the sample shall pass through 0.150 mm IS sieve to 0.180 mm IS sieve].

 

(d)      Grind as rapidly as possible to a avoid loss or gain of moisture during operation.

 

(e)      Mix thoroughly and store in tightly stoppered bottles.

2. Determination of moisture

(Not applicable to samples that yield volatile substances other than water at drying temperature)

(i)       Procedure

(a)      Weight to the nearest mg about 2gm of the prepared sample in a weighed, clean, dry squat form weighing bottle.

 

(b)      Heat in an oven for about 5 hours at 99-101 C to constant weight Cool in a desicator and weigh.

 

(c)      In case of sodium nitrate ammonium sulphate and potassium salts heat to constant weight at 129-131 C.

(d)      Report percentage loss in weight as moisture at temperature used.

Calculations

100(B-C)

Free moisture percent by weight = 100(B-C)/B-A

A= Weight of the bottle

B= Weight of bottle plus material before drying.

C= Weight of the bottle plus material after drying. (Reference - Methods of analysis. AOAC 1965)

(ii)      Moisture in ammonium chloride.

(a)      Weigh accurately about 5gm of prepared sample in a weighed shallow porcelain dish and dry for 24 hours in a vacuum desicator over sulphuric acid and re-weight.

(b)      Preserve the dried material for subsequent tests.

Calculations

Moisture percent by weight = 100 x W1/W3

W1= loss in weight in gm on drying and

W3= Weight in gm of the prepared sample taken for the test.

(iii)     Samples like urea, diammonium phosphate and ammonium nitrate which yield volatile substances other than water at drying temperature. the Karl Fischer method given below is use for the determination of moisture.

(iv)    Reagents

(a)      Iodine solution -add 125 gm of iodine to a mixture of 650 ml of methanol and 200 ml of pyridine contained in a flask, and immediately close the flask tightly.

(b)      Sulphur dioxide solution-pass dry sulphur dioxide into 100 ml of pyridine contained in a 250 ml graduated cylinder and cooled in an ice bath, until the volume reaches 200 ml.

(c)      Fisher Reagent- Slowly add iodine solution to the cooled sulphur dioxide solution stopper immediately and shake well until the iodine is dissolved. Transfer the solution to an automatic pipette, protected from absorption of moisture by a drying agent and allow to stand for 24 hours before standardizing. The reagent deteriorates continuously and it should be standardized within one hour before use.

(v)      Procedure.

(a)      Determination of end point in Karl Fischer Titration- In many cases, the end point can be detected visually by the change of colour

(b)      Sulphur dioxide solution -pass dry sulphur dioxide into to 100 ml of pyridine contained in a 250 ml graduated cylinder and cooled in an ice bath, until the volume reaches 200 ml.

(c)      Fisher reagent-Slowly add iodine solution to the cooled sulphur dioxide solution stopper immediately and shake well until the iodine is dissolved. Transfer the solution of moisture by a drying agent and allow to stand for 24 hours before standardizing. The reagent deteriorates continuously and it should be standardized within one hour before use.

(d)      Standard water solution- Measure exactly 2ml of water into a thoroughly dry 1 liter volumetric flask, dilute to volume with methanol. retain sufficient quantity of the same methanol for blank determination. Keep the solution in tightly closed containers.

(vi)    Procedure

(a)      Determination of end point in Karl Fischer Titration- In many cases, the end point can be detected visually by the change of colour from a light brownish yellow to amber. But when the end point is not clearly defined, the electrometric method for determining the end point should be adopted. Adjust the potentiometer so that when a small excess 90.02 ml) of the reagent is present a current of 50 to 150 microampers is recorded. The solution should be continuously and vigorously stirred. At the beginning of the titration, a current of only a few microampers will flow. After each addition of regent, the pointer of the micrometer deflected but rapidly returns to the original position. At the end point deflection is obtained which endures for a longer period.

(b)      Standardization of the Fischer reagent-Pipette exactly 10ml or methanol into a dry titration flask and titrate with the Fischer reagent to the end point (V1) Pipette exactly 10ml of the standard water solution into the flask and titrate to the end point (V2).

(c)      Titration of the material-Transfer 25ml. of methanol to the titration flask and titrate to the end point (V3) with the Fischer reagent. Do not record the volume consumed. Quickly transfer to the titrated liquid an accurately weighed quantity of the material containing 10 to 50 mg. of water, stir vigorously and titrate to the end point.

Calculation

Moisture percent by weight = 0.1 x W(V3 2.5V1) / (V2- V1)A

Where W= Weight in mg. of water contained in 10ml of standard

water solution.

V3= Total volume in ml of the reagent use in titration in (c)

V1= Volume in ml of reagent used in titration of methanol in(b)

V2= Total volume in ml of the reagent use in titration in (b)

A= Weight in gm. of the material taken for the test in (C)

(Reference- I.S. Specification for urea. technical and pure I.S. 1781-1961)

3. Determination of nitrogen

Methods of determination of total nitrogen have been described separately in this section. These methods can be adopted both for straight and mixed fertilizers. Scope of each method with various combinations have also been described with each method.

The relevant methods of analysis which have been described are as given below:

(i)       Total nitrogen--for nitrate free samples.

 

(ii)      Total nitrogen--for nitrate containing samples.

 

(iii)     Total nitrogen--for materials with high Cl: No3 ration and to materials containing only water soluble nitrogen.

 

(a)      Total nitrogen--for nitrate free samples.

 

(iv)    Determination of ammoniacal nitrogen.

 

(v)      Determination of ammoniacal and nitrate nitrogen.

 

(vi)    Determination of nitrate nitrogen.

 

(vii)   Determination of water insoluble nitrogen.

 

(viii)  Determination of urea nitrogen.

[133][(i) Determination of Cyanamide nitrogen;]

                                              (i)          Detection of nitrate

For adopting a specific method as described above, it is necessary to detect the presence of nitrates in the sample before a particular method is adopted. The procedure for detection of nitrates is given below:-

(a)      Mix 5gm sample with 25ml hot water and filter.

 

(b)      To one volume of this solution add 2 volume of sulphuric acid, free from HNO3 and oxides of N and let it cool.

 

(c)      Add a few drops of concentrated FesO4 solution in such a manner that fluids do not mix.

 

(d)      If the nitrates are present junction shows at first purple, afterward brown, or if only minute quantity is present, reddish colour.

 

(e)      To another portion of solution add 1ml. 1 percent Na NO3 and test as before to determine whether enough H2SO4 was added in the first test.

(Reference -methods of analysis. AOAC 1965)

                                             (ii)         Reagents for determination of total nitrogen.

(a)      Sulphuric acid - 93-98 percent H2SO4 N free.

(b)      Copper sulphate - Cu SO45H2O reagent grade. N free.

(c)      Potassium sulphate (or anhydrous sodium sulphate)-reagent grade.

(d)      Salicylic acid- reagent grade, N free.

(e)      Sulphide or the sulphate solution- Dissolve 40 gm. commercial K2S in liter distilled water. (Solution- of 40gm Na2S or 80gm Na2S2O3.5H2O in 1 liter may be use)

(f)       Sodium hydroxide- pellets or solution, nitrate free. for solution dissolve approximately 450 gm solid NaOH in distilled water and dilute to 1 liter (Sq. gr. of solution should be 1.36 or higher)

(g)      Zinc granule-- reagent grade.

(h)     Zinc dust-- Impalpable powder.

(i)       Methyl red indicator- Dissolve 1gm. methyl red in 200 ml. alcohol.

(j)       Hydrochloric or sulphuric acid standard solution,--0.5 N or 0.1 N when amount or N is small.

(k)      Sodium hydroxide standard solution-- 0.1 N(or other specified concentration)

(1)     Standardize each standard solution with primary standard and check one against another.

(2)     Test reagents before using, by blank determination with 2 gm. sugar which insures partial reduction of any nitrates present.

Caution: Use freshly opened sulphuric acid or add dry P2O5 to avoid hydrolysis of nitrites and cyanates. Ratio of salt to acid (wt: Vol) should be approximately 1:1 at end of digestion for proper temperature control. Digestion may be incomplete at lower ration, N may be lost at higher ration.

                                            (iii)         Apparatus

(a)      For digestion-- Use Kjeldahl flask of hard moderately thick, well annealed glass with total capacity approximately 500-800 ml. Conduct digestion over heating device, adjusted to bring 250 ml. water at 25C to rolling boil in a approximately for 5 minutes. Add 3-4 boiling chips to prevent superheating.

(b)      For distillation- Use Kjeldahl or other suitable flask of 500--800 ml. capacity filled with rubber stopper through which passes. lower end of efficient scrubber bulb or trap to prevent mechanical carryover of NaOH during distillation. Connect upper end of bulb tube to condenser tube by rubber tubing. Trap outlet of condenser in such a way as to insure complete absorption of ammonia distilled over into acid in receiver.

                                            (iv)        Total nitrogen (in nitrate free samples)

(a)      Procedure.

(1)     Place weighed sample (0.7-2.2gm.) in digestion flask.

(2)     Add 0.7 gm. copper sulphate, 15 gm. powdered K2SO4 at anhydrous Na2 SO4 and 25ml.H 2SO4.

(3)     If sample more than2.2 gm. is used, increase sulphuric acid by 10 ml. for each gm. sample.

(4)     Place flask in inclined position and heat gently until frothing ceases (if necessary add small amount of paraffin to reduce frothing)

(5)     Boil briskly until solution clears and then for at least 30 minutes longer (2 hours for sample containing organic material).

(6)     Cool add approximately 200ml. distilled. water, cool below 25C.

(7)     Add to the flask a layer of sodium hydroxide (25 gm. solid reagent or enough solution to make contents strongly alkaline ) without agitation.

(8)     Immediately connect flask to distilling bulb or condenser and with tip of condenser immerse in standard acid in receiver.

(9)     Rotate flask to mix contents thoroughly, then heat until all amonia has distilled (a least 150 ml. distillate)

(10)   Titrate excess standard acid in distillate with standard sodium hydroxide solution, using methyl red as an indicator.

(11)   Correct for blank determination on reagents.

Calculation: Percent nitrogen =(A Na-BNb)x0.01401 x 100 / W

A= ml. of standard acid used.

B= ml. of standard NaOH used.

Na = Normality of standard acid.

Nb = Normality of standard NaOH.

W= Weight of the sample taken in grams.

(Reference- Methods of Analysis, AOAC, 1965)

                                             (v)         Total nitrogen (for nitrate containing samples)

(Note applicable to samples containing high concentrations of nitrate nitrogen and chlorides)

(a)      Procedure.

(1)     Place weighed sample (0.7-2.2 gm) in digestion flask.

(2)     Add 40ml. H2SO4 containing 2 grams salicylic acid. Shake until thoroughly mixed and let stand, with occasional shaking, 30 minutes or more.

(3)     Then add (i) 5 grams Na2S2O3.5H2O or (ii) 2grams zinc dust (as impalpable powder not granulated zinc or filings)

(4)     Shake the flask and let it stand for five minutes. then heat over low flame until forthing ceases.

(5)     Turn off heat, add 0.7 grams copper sulphate.15 gm. powdered K2SO4) and boil briskly until solution clears, then at least 30 minutes longer (2 hours for samples containing organic material).

Proceed further as in 6-11 of 3 (iv)

Calculations: Same as in 3 (iv)

(Reference- Methods of Analysis, AOAC, 1965).

                                            (vi)        Total nitrogen (for materials with high Cl: NO3 ration and to materials containing only water soluble nitrogen).

(a)      Reagents

Reduced iron powder electrically reduced N.F. (National Formulary).

For other reagents see 3 (ii)

(b)      Procedure

Mixed fertilizers

(1)     Place 0.5-2.0 gm. sample in Kjeldahl flask and add 2-5 grams reduced Fe(5gms. is enough for 0.185 grams. NO3).

 

(2)     Add approximately 25ml. distilled water, rotating flask at angle to wash down the sample.

 

(3)     Let it stand for 15 minutes with occasional agitation, to insure complete solution of all soluble salts.

 

(4)     While rotating flask add 25ml. cold H2SO4 (1+1) and let it stand until visible reaction ceases, (use hood or vented digestion unit)

 

(5)     Add boiling chips and boil 15-20 minutes, but do not take to dryness (For samples containing organic matter use 50ml. cold H2SO4 (1+1) boil for 15-20 minutes add 0.7 gm. MgO and heat again for 40 minutes) Cool and proceed further as in 6-11 of 3 (iv).

Calculations: Same as in 3 (iv)

(Reference-methods of Analysis, AOAC 1965).

                                            (vii)        Determination of ammoniacal nitrogen (Distillation Method) (This method is for the determination if nitrogen present or available in the sample as ammonium ion. This method assumes that Urea is absent from the sample. Not applicable to MgNH4 PO4 and Fe4PO4)

(a)      Procedure

(1)     Place 0.7-3.5 grams according to HN3 content of the sample in distillation flask with approximately 300 ml. water and 2 grams of freshly ignited carbonate free MgO or NaOH solution.

(2)     Connect the flask to condenser by Kjeldahl connecting bulb.

(3)     Distill 100 ml. liquid into measured quantity of standard acid and titrate with standard NaOH solution, using methyl red as an indicator

Calculations: Percent nitrogen = (ANa -BNb) x 0.01401 x 100 / W 

A= ml. of standard acid used.

B= ml. of standard NaOH.

Na = normality of acid.

Nb = normality of NaOH.

W= weight of the sample taken in gm.

(Reference -Recommended analytical methods of the

National Plant Food Institute, Washington. D.C. 1961)

                                           (viii)       Determination of ammoniacal and nitrate nitrogen (Devarda Method) (This method is for the determination of total nitrogen when only nitrate or mixture of nitrate and ammoniacal nitrogen is present. This method assumes the absence of urea, calcium Cyanamid and organic matter from the sample.)

(a)      Procedure

(1)     Place 0.35-0.5 gms. sample in600-700ml. flask and add 300ml. water, 3 grams devarda Alloy, and 5ml. NaOH solution (42 percent by weight pouring later down side of flask so that it does not mix at once with contents)

 

(2)     Allow the flask to stand for 15 minutes.

 

(3)     By means of Davison [ J. Ind. Eng. Chem. 11,465 (1919)] or other suitable scrubbing bulb, that will prevent passing over of any spray, connect with condenser tip of which always extends beneath surface of standard acid in receiving flask.

 

(4)     Mix contents of distilling flask by rotating.

 

(5)     Heat slowly at first and then at a rate to yield 250 ml. distillate in 1 hour.

 

(6)     Collect distillate in measured quantity of standard acid and titrate with standard NaOH solution using methyl red as an indicator.

 

(7)     In analysis of nitrate salts dissolve 3.5 or 5.0 grams in water, to 250 ml. and use 25ml. aliquot.

Calculation: Same as in 3 (iv)

(reference- Methods of Analysis, AOAC, 1965)

                                            (ix)        Determination of nitrate nitrogen

(Applicable in presence of calcium Cyanamid and urea in the mixture)

(a)      Procedure

(1)     Determine total nitrogen as in 3(v)

 

(2)     Determine water insoluble N as in 3(x) but use 2.5 grams sample. Dilute to 250ml.

 

(3)     Determine ammoniacal N in 50ml filtrate as in (vii).

 

(4)     Place another 50ml. portion filtrate in 500 ml. Kjeldahl flask and 2 grams FeSO4.7H2O and 20ml. H2SO4 (if total N is 5percent use 5gm. Fe SO4.7H2O) Digest over hot flame until all water is evaporated and transparent fumes appear and continue digestion at least ten minutes to drive off nitrate N. If severe bumping occurs add 10-15 glass beads. Add 0.65 grams Hg or 0.7 grams HgO and digest until all organic matter is oxidized, cool, dilute add the K2S solution and complete determination as 3 (iv) Before distillation add pinch of mixture of zinc dust and granular "20 mesh". zinc to each flask to prevent bumping.

Calculations: Total N (a)-- water insoluble N(b)- water soluble N. Water Sol.

N-- N obtained in (d)- nitrate N.

(Reference -Methods of analysis, AOAC, 1965)

                                             (x)         Determination of water insoluble nitrogen

(a)      Procedure

(1)     Place 1 or 1.4 grams sample in 50ml. beaker, wet with alcohol.

(2)     Add 20ml. water and let it stand for 15 minutes stirring occasionally.

 

(3)     Transfer supernatant liquid to 11 cm. Whatman No. 42. paper in 60 long stem funnel 2.5" diameter and wash residue 4 or 5 times by decanting with water at room temperature (20-25C)

 

(4)     Finally transfer all residue to filter and complete washing until filtrate measures 250ml.

 

(5)     Determine N as in 3(iv)

                                            (xi)        Determination of urea nitrogen

(This method is for the determination of urea content of any mixed fertilizers.)

(a)      Reagents

(1)     Neutral urease solution - shake 1gm. jack bone meal with 100ml. water for 5 minutes. Transfer 10ml solution to 250 ml. Erlenmeyer flask, dilute with 50ml. water and add 4 drops methyl purple indicator. Tiltrate with 0.1 N NaOH. From difference in ml. calculate amount of 0.1 N HCL require to neutralize remainder of solution (usually approximately 2.5 ml. per 100ml.) add this amount of acid

(b)      Procedure

(1)     Weight 10+0.01 gm. sample and transfer to 15cm. Whatman No. 12 fluted filter paper.

 

(2)     Leach with approximately 300ml. water into 500ml. volumetric flask.

 

(3)     Add 75-100 ml. saturated barium hydroxide solution to precipitate phosphates.

 

(4)     Let it settle and test for complete precipitation with few drops of saturated barium hydroxide solution.

 

(5)     Add 20ml 10 percent sodium carbonate solution to precipitate excess barium and any soluble calcium salts.

 

(6)     Let it settle and test for complete precipitation.

 

(7)     Dilute to volume, mix and filter through 15cm. Whatman. No. 12 fluted paper.

 

(8)     Transfer 50ml. aliquot (equivalent to 1gm. sample)to 200 or 250 ml. Erlenmeyer flask and add 1 to 2 drops methyl 1 purple indicator.

 

(9)     Acidify solution with 2N HCl and add 2 to 3 dorps excess.

 

(10)   Neutralize solution with 0.1 N NaOH to first change in colour indicator.

 

(11)   Add 20ml. neutral urease solution, close flask with rubber stopper and let it stand for 1 hour at 20-25C.

 

(12)   Cool the flask in ice water slurry and titrate at once with 0.1 N HCl to full purple colour, then add approximately 5ml. excess.

 

(13)   Record total volume added, back titrate excess HCl with 0.1N NaOH to neutral end point.

Calculations: Percentage urea =(ml. 0.1 N HCl - ml 0.1 N NaOH) x0.3003 wt. of sample.

(Reference- methods of Analysis, AOAC, 1965)

[134][(xi a) Determination of Cyanamide nitrogen

Cyanamide nitrogen is precipitated as a silver complex and estimated in the precipitate by Kjeldahl's method.

(a)      Reagents:

                                                                              (i)          Ammonical Silver Nitrate Solution-Mix 500 ml of 10% silver nitrate (AgNO3) solution in water with 500 ml of 10% ammonia solution.

 

                                                                             (ii)         Glacial acetic acid

 

                                                                            (iii)         Remaining reagents as given in 3(ii).

(b)      Procedure:-

                                                                              (i)          Weigh 2.5 g (W) sample and place it in a small glass mortar.

 

                                                                             (ii)         Grind the sample 3 times with water, pouring off the water after each grinding into a 500 ml volumetric flask.

 

                                                                            (iii)         Transfer quantitatively the sample into 500 ml volumetric flask, washing the mortar, pestle and funnel with water.

 

                                                                            (iv)        Make up volume to approximately 400 ml.

 

                                                                             (v)         Add 15 ml of glacial acetic acid.

 

                                                                            (vi)        Shake on rotary shaker for 2 hours.

 

                                                                            (vii)        Make up the volume to 500 ml with water, mix and filter.

 

                                                                           (viii)       Transfer 25 ml of filterate into 250 ml beaker.

 

                                                                            (ix)        Add ammonia solution until slightly alkaline & add 20 ml of warm ammoniacal silver nitrate. Yellow precipitate will form.

 

                                                                             (x)         Leave over night. Filter using Whatman No. 40 filter paper and wash the precipitate with cold water until it is completely free of ammonia.

 

                                                                            (xi)        Place the filter& precipitate in a Kjeldahl flask.

 

                                                                            (xii)        Add 0.7 g copper sulphate, 15 g Potassium sulphate and 30 ml of H2SO4.

 

                                                                           (xiii)       Place flask in inclined position and heat gently.

 

                                                                           (xiv)       Boil bristly until solution becomes clear or pale green.

 

                                                                            (xv)        Continue digestion for 30 minutes more.

 

                                                                           (xvi)       Remove from burner and cool.

 

                                                                          (xvii)       Transfer the contents of Kjeldahl flask to 1 litre capacity, distillation flask, make volume to about 350 ml with water and a pinch of zinc dust. Mix and cool.

 

                                                                          (xviii)      Distill ammonia by adding 10 ml of NaOH (40%) and collect the distillate in receiver conical flask containing 25 ml of 0. 1N HCI or H2SO4 containing 5 drops of Methyl red indicator.

 

                                                                           (xix)       Titrate the contents in receiver conical flask with 0.1N NaOH & calculate the volume of 0.1 N HCl consumed (V).

 

                                                                            (xx)        Determine blank on reagents using same quantity of standard acid in receiver conical flask.

(c)      Calculation:

Cyanamide Nitrogen % (by weight) =Blank-V x 2.8./W]

                                            (xii)        Determination of biuret.

(a)      Reagents.

(1)     Alkaline tartarate solution-- Dissolve 40gm NaOH in 50ml. water cool, add 50gm. of NaK C4H4O64HP2Oand dilute to 1 liter. Let. it stand for one day before use.

 

(2)     Copper Sulphate solution - Dissolve 15 gm. CuSO4.5H2O in CO2P free water and dilute to 1 liter.

 

(3)     Biuret standard solution- 1mg./ml. Dissolve 100gm. reagent grade biuret in CO2free water and dilute to 100ml.

 

(4)     Ion exchange resin. Fill 50ml. burette with 30cm. column of Amberlite IR 120 (H) resin on glass wool plug.

Regenerate column after each use by passing 100ml. H2SO4 (1+9) or HCL (1+4) through the column approximately 5ml.per minute and then washing with water until pH of effluent is 6.0.

(b)      Preparation of standard curve.

(1)     Transfer series of aliquotes, 2-50 ml. of standard biuret solution to 100ml. volumetric flask.

 

(2)     Adjust volume to approximately 50ml with CO2 free water. Add one drop of methyl red and neutralize with 0.1 NH2SO4 to pink colour.

 

(3)     Add with swirling 20ml alkaline tartarate solution and then 20ml. CuSO4 solution.

 

(4)     Dilute to volume. Shake for 10 seconds and place in water bath for 15 minutes at 30+5C.

 

(5)     Also prepare reagent blank.

 

(6)     Determine absorbance of each solution against blank at 555 mw (instrument with 500-570 mw filter is also satisfactory ) with 2-4cm. cell. and plot standard curve.

(c)      Procedure.

A.        In urea.

(1)     Stir continuously 2-5 gm sample in 100ml. approximately 50C water for 30 minutes.

 

(2)     Filter and wash into 250 ml. volumetric flask and dilute to volume.

 

(3)     Transfer 25ml. aliquot to 100ml. volumetric flask and proceed as given under preparation of standard curve 3 (xii).

B.        In mixed fertilizers.

(1)     Stir continuously 10-20gm. sample in 150 ml. approximately (50 C) hot water for 30 minutes.

 

(2)     Filter and wash into 250ml volumetric flask and dilute to volume.

 

(3)     Transfer 25 ml aliquot to column 3 (xii) (a) (4) and adjust flow to 4- 5 ml./minute.

 

(4)     Receive elute in 100ml. beaker.

 

(5)     When liquid level falls to top of resin bed. wash with two 25ml portion water.

 

(6)     To eluate and washings add two drops of methyl red and then 0.1 N NaOH to yellow colour.

 

(7)     Add 0.1 NH2 SO4 until solution just turns pink .

 

(8)     Transfer to 100ml. volumetric flask and dilute to volume with CO2 free water.

 

(9)     Transfer 50ml. aliquot to 100ml. volumetric flask and proceed as in preparation of standard curve given above.

Calculation: From standard curve determine concentration of biuret in final dilution. then percent of

Biuret = C x 100 / W

Where C= concentration in mg/ml of biuret in final dilution obtained from standard curve.

W= Concentration of original sample in final dilution expressed as mg/ml.

(Reference -Methods of analysis, AOAC, 1965)

                                           (xiii)       Determination of free acidity in ammonium sulphate (as H2SO4)

(a)      Reagents

(1)     Standard sodium hydroxide solution- 0.02 N.

 

(2)     Methyl red indicator--Dissolve 0.15 gm. of water soluble methyl red in 500 ml. water.

 

(3)     Methyl red-- Methyl blue mixed indicator solution- prepared by mixing equal volumes of 0.2 percent solution in rectified spirit of methyl red and 0.1 percent solution in rectified spirit of methylene blue.

(b)      Procedure.

(1)     Dissolve about 20mg. of prepared sample, accurately weighed in about 50ml. cold natural water.

 

(2)     Filter and make up the volume to about 200ml.

 

(3)     Titrate with standard sodium hydroxide solution, using one or two drops of methyl red as indicator.

 

(4)     If satisfactory end point with methyl red is not obtained, methylene red-- methylene blue mixed indicator may be used.

 

(5)     Use- preferably a micro biuret for this titration.

The filtering medium shall be neutral and shall not contain any alkaline material which would neutralize free acid.

Calculations: Free acidity as H2SO4 percent by weight =4.904AN /W

A= Volume of ml. of standard NaOH solution.

N= Normality of standard NaOH Solution.

W= Weight in gm of prepared sample taken for the test.

(Reference - Specification of ammonium sulphate, fertilizer grade IS:826- 1967)

                                           (xiv)       Determination of arsenic in ammonium sulphate (A2O3)

(a)      Reagents

(1)     Lead acetate solution- prepare 10percent solution of lead acetate with sufficient acetic acid added to clear the solution.

 

(2)     Dry lead acetate paper-Cut filter paper (Whatman No.1 or equivalent) into strips 70x50 mm and keep them permanently suspended in lead acetate solution in a glass stopped bottle, Before use, take out the strips and cry them in an atmosphere free from hydrogen sulphide.

 

(3)     Mercuric bromide solution-- Dissolve 5gm of mercuric bromide in 100ml rectified spirit.

 

(4)     Sensitized mercuric bromide paper strips-- cut filter paper (Whatman NO. 1 or equivalent) into strips 120x2.5 mm. Keep the strips permanently suspended in dark in a glass stoppered cylinder or amber bottle having mercuric bromide solution. Before use take out a strip, press it between sheets of filter paper and dry it in an atmosphere free from hydrogen sulphide.

 

(5)     Dilute sulphuric acid- approximately 5N.

 

(6)     Concentrated hydrochloric acid.

 

(7)     Potassium iodide solution-15 percent.

 

(8)     Stannous chloride solution- Dissolve 80gm. of stannous chloride in 100ml. water containing 5ml. of concentrated hydrochloric acid and boil until clear solution is obtained. Add some metallic tin to the solution to prevent oxidation.

 

(9)     Zinc- It is recommended that zinc rods prepared as described below should be used for routine work. however, pellets described may be used.

(b)      Preparation of zinc rods.

(1)     Take a clean and dry hard glass test tube of 10mm internal diameter and 20 cm. length.

 

(2)     Heat the test tube over a flame of bunsen or blow pipe burner and add slowly arsenic free granulated zinc in small portion (1 to 2 gm at a time) the next portion being added after the first one has completely melted.)

 

(3)     Continue heating and adding zinc until the melt is about 10cm. high.

 

(4)     Heat the clean melt for half an hour and then cool to room temperature.

 

(5)     Break the tube to obtain the rod of zinc.

 

(6)     Cut rod into pieces 20mm long.

 

(7)     Coat the plane ends of the pieces with a paste of magnesium carbonate and gum arabic solution and dry.

 

(8)     Coat the pieces all over with 1.5 mm. thick layer or paraffin wax.

 

(9)     When required for use, scrap off the wax from the place ends with a knife, protecting wax colour round the rods.

 

(10)   Remove the paste from the plane ends by soaking in water and activate the exposed surface by dipping in a solution containing one part of stannous chloride solution and seven parts of concentrated hydrochloric acid.

(c)      Preparation of zinc pellets.

Treat zinc shots passing through IS sieve 570 (aperture 5660 microns) and retained on IS sieve 280 (aperture 2818 microns)with concentrated hydrochloric acid until the surface of zinc becomes clean and dully. Weight and keep under water, preventing contamination with dust.

(d)      Standard sodium hydroxide solution-- approximately 20 percent.

(e)      Standard arsenic trioxide solution.

(1)     Dissolve 1.0 gm. of resublimed arsenic trioxide (AS2 O3) in 25 ml. sodium hydroxide solution and neutralize with dilute sulphuric acid.

(2)     Dilute with freshly distilled water containing 10ml of concentrated sulphuric acid per liter and make up the volume to 1 liter.

(3)     Again dilute 10ml. of this solution to 1 liter with water containing sulphuric acid and finally dilute 100ml. of this solution to 1 liter with water containing sulphuric acid. One ml. of this solution contains 0.001 mg. of arsenic trioxide (AS2O3) the dilute solution shall be prepared freshly when required.

(f)       Procedure.

(1)     Dissolve 1.0 gm. of the prepared sample in 20ml water.

 

(2)     Place dry lead acetate paper in the lower portion of the tube B (in Figure 6) and glass wool moistened with lead acetate solution in its proper portion.

 

(3)     Place the sensitized strips of mercuric bromide paper in tube A and connect the tubes together with a rubber stopper.

 

(4)     Introduce the solution of the material into the bottle C (120 ml) and then add 10ml of dilute sulphuric acid. Add 0.5 ml. of stannous chloride solution 5ml. potassium iodide solution and make up the volume with water to about 50ml. (Figure No. 6- Modified Gutzet Method of test for arsenic.) 

 

(5)     Mix the contents and drop about 10mg. of zinc. Immediately fit in position the rubber stopper carrying the tube B.

 

(6)     Place the bottle.

 

(7)     At the end of two hours remove the test strip by means of tweezers.

 

(8)     Carry out the test prescribed above using a volume of standard arsenic trioxide solution containing 0.1 mg. of arsenic trioxide in place of the solution of the material and compare the stain produced with the material with that produced with arsenic trioxide solution.

 

(9)     The limit prescribed in the material specification shall be taken as not having been exceeded if the length of the stain as well as the intensity of its colour produced in the test with the material is not greater than those produced with the arsenic solution.

(Reference- Modified Gutzet Method of test for arsenic , IS-2088, 1962)

                                            (xv)        Determination of calcium nitrate (for calcium ammonium nitrate and nitrophosphates.)

(a)      Reagents

(1)     N-Amyl Alcohol.

 

(2)     Dilute hydrochloric acid- approximately 4N.

 

(3)     Standard calcium Solution-- weigh 1.0 gm of calcium carbonate dried at 1200+50C and dissolve in the minimum quantity of dilute hydrochloric acid. Dilute the solution to 1 litre in a graduated flask.

 

(4)     Ammonium chloride- ammonium hydroxide buffer solution . Dissolve 67.5 gm. ammonium chloride in a mixture of 570ml. of ammonium hydroxide (sp. gr. 0.92) and 250 ml. water. Also dissolve separately a mixture of 0.931 gm. of disodium ethylene diamine tetra-acetate dihydrate and 0.616 gm of disodium ethylene diamine tetra-acetate dihydrate and 0.616 gm of magnesium sulphate (Mg. SO4. 7H2O) in about 50ml. of water. Mix the two solutions and dilute to 1 liter.

 

(5)     Standard disodium ethylene diamine tetra-acetate (EDTA) solution- weight. 3.72gm. of disodium ethylene diamine tetraacetate dihydrate in water and dilute in a graduated flask to 1 liter. The solution shall be standardized frequently against standard calcium solution following the procedure given below.

 

(6)     Eriochrome black-T Indicator solution- Dissolve 0.1 gm in 20ml of rectified spirit. The solution shall be used for not more than a week.

(b)      Procedure.

(1)     Grind quickly about 5gm. of the material, accurately weighed, with about 50ml. of amyl alcohol in a pestle and mortar and transfer the contents to a conical flask.

 

(2)     Wash the pestle and mortar with a few ml. of amyl alcohol and add the washings to the flask.

 

(3)     Shake the content of the flask manually or in a mechanical shaker for about half an hour and then filter.

 

(4)     Transfer the filtrate to a separating funnel and extract calcium nitrate completely with water in five to six instalments.

 

(5)     A few drops of dilute hydrochloric acid may be added during the extraction with water to avoid formation of an emulsion of amyl alcohol with water.

 

(6)     Concentrate the water extract at low temperature to nearly half its volume.

 

(7)     Transfer the concentrated solution to a conical flask add 5ml. of ammonium chloride- ammonium hydroxide buffer solution, 5 drops of eriochrome black-T indicator solution and titrate against standard EDTA solution to a pure blue end point.

Calculations: Calcium nitrate percent by weight = 8.2 NV / W

Where N= Normality of standard EDTA solution

V= Volume in ml. of standard EDTA solution used in the titration and

W= Weight in gm. of the material taken for test.

(Reference--IS specifications of CAN IS: 2409-1963)

                                           (xvi)       Determination of chlorides other than ammonium chloride.

(a)      Reagents

(1)     Standard silver nitrate solution- 0.1N.

 

(2)     Concentrated nitric acid- conforming to IS:264-1950

 

(3)     Ferrous ammonium sulphate solution saturated in water and stabilized by addition of 50ml nitric acid.

 

(4)     Standard ammonium thiocyanate solution - 0.1 N.

(b)      Procedure.

(1)     Dissolve about 0.2 gm. of the prepared sample, previously dried as in procedure for determination of moisture and accurately weighted in about 40ml water.  

 

(2)     Add exactly 50ml. of standard silver nitrate solution and 5ml. of concentrated nitric acid.

 

(3)     Add 0.5 ml. of nitrobenzence and make up the volume of the mixture to exactly 100ml. with water.

 

(4)     Take exactly 50ml.. of the solution and add 2ml. of ferric ammonium sulphate solution.

 

(5)     Titrate the excesses of silver nitrate in this portion with standard ammonium thiocyanate solution.

 

(6)     Carry out a blank test following the procedure given as above but without using the material.

Calculations: Total chlorides (as Cl) percent = 7.07 (V1- V2)N

by weight (on dry basis) W

Where

V1= Volume in ml. of standard ammonium thiocyanate used in the blank determination.

V2= Volume in ml. of standard ammonium thiocyanate

solution used in the test with the material.

N= Normality of standard ammonium thiocyanate solution.

W= Weight in gm. of the drived prepared sample taken forthe test.

Express the ammoniacal nitrogen content percent by weight of the material determined earlier in terms of Cl as follows.Chloride equivalent of the ammoniacal nitrogen content percent by weight = 2.531 x A .....Y where A is the ammoniacal nitrogen content determined earlier. Balanced chloride equivalent to sodium chloride

(NaCl) percent by weight=1 - 648 x (X-Y)

(x-y) = Balanced chlorides other than ammonium chloride

(Reference- IS Specification for ammonium chloride Fertilizers grade (Revised) IS: 1114 -1964 calculations modified.)

                                          (xvii)       [135][Determination of oil in Neem Coated Urea

Principle :--Oil present in Neem coated urea is extracted with [136][a binary mixture of n-hexane and acetone] and separated from the aqueous phase. The solvent layer is then evaporated and the residue is weighed as oil.

Reagents : (i) [137][a binary mixture of n-hexane and acetone]

(ii) Dilute HCl: Prepare 1 : 1 HCl by adding 100 ml. conc. HCl to 100 ml. distilled water.

Procedure: (i) Weigh accurately about 200 gm Neem coated urea and transfer it to a 1000 ml separating funnel.

(ii) Add about 250 to 300 ml warm distilled water and shake gently to dissolve urea.

(iii) Add 50 ml [138][a binary mixture of n-hexane and acetone] and acidify with 5 ml dil. HCl. Mix well and separate the oily [139][a binary mixture of n-hexane and acetone] layer.

(iv) Repeat the extraction of oil from the aqueous layer with fresh 50 ml [140][a binary mixture of n-hexane and acetone] and mix the oily [141][a binary mixture of n-hexane and acetone] layer with that obtained in step (iii).

(v) Give washings to this oily [142][a binary mixture of n-hexane and acetone] with warm distilled water till it is completely free from urea.

(vi) Transfer the [143][a binary mixture of n-hexane and acetone] layer to an oil free 100 ml beaker. Give 2-3 washings to the separating funnel with about 10 ml [144][a binary mixture of n-hexane and acetone] each time to transfer completely the oil from the separating funnel to the beaker. '

(vii) Heat the contents in the beaker on a water bath to break any emulsion formed. Filter this oily layer into another previously weighed 100 ml beaker. Give two to three, 10 ml [145][a binary mixture of n-hexane and acetone] washings to the filter paper to transfer the oil completely into the weighed beaker. (viii) Evaporate [146][a binary mixture of n-hexane and acetone] by keeping beaker on a water bath at 105°C for about two hours. Cool in a dessiccator and weigh the contents to a constant weight. Find out the weight of this oil in the beaker.

(ix) Carry out a blank test with [147][a binary mixture of n-hexane and acetone] (with equivalent amount consumed in the test) for oily content present, if any, and subtract the same from the test results.

Calculation: [148][binary mixture of n-hexane-acetone soluble] (oil), ppm = 1000 x (W-Wb)/W

[149][binary mixture of n-hexane-acetone soluble] (oil), % = (W-Wb )/10 W

Where W is the weight of the oil in the beaker, in mg Wb in the weight of oil (in mg) in the blank, and W is the weight of the sample taken in gm.]

                                          (xviii)      [150][Method of Analysis for determination of Meliacin of Neem Oil in Neem Coated Urea by High Performance Liquid Chromatography.

1.        Take 2 kg of Urea sample in 5 ltr. capacity borosilicate glass beaker and add approximately 1 litre. of a binary mixture of n hexane and acetone so as to immerse completely the 2.0 kg Urea with n-hexaneacetone and keep it for 4-6 hours, preferably overnight with intermittent stirring the solution with a glass rod.

 

2.        Filter the content of the beaker containing urea dissolved in the n-hexane-acetone through Whatman filter paper no 41 with repeated washings of n hexane and acetone to complete washing of neem oil content from the Urea.

 

3.        Evaporate the collected n hexane and acetone soluble Neem extract by vacuum distillation maintaining temperature below 50oC and reduce the quantity of n-hexane-acetone to about 15 to 20 ml of Neem Oil extract, the temperature of flask should be maintained so that it should not be dried.

 

4.        Transfer the volume of n-hexane-acetone Soluble Extract from the distillation flask to the pre-weighed beaker of 100 ml capacity. Again evaporate the n hexane and acetone from the Neem Oil Extract at a controlled temperature on water bath.

 

5.        Add 5 ml of Methanol : Water (90:10) mixture to the beaker consisting Neem Oil Extract covered with Aluminum foil to check the spillage during the sonicating.

 

6.        Keep the beaker on sonicator and sonicate it for 10 minutes.

 

7.        Transfer the content of beaker into Centrifugal tube and centrifuge it at 2500 rpm for 10 minutes.

 

8.        Collect the upper layer and pass it through C-18 solid phase extraction Cartridge (Supelco or equivalent).

 

9.        Now analyze the Neem Oil Extract derived from the Neem Coated Urea to determine the Azadirachtin, Nimbin and Salannin content by HPLC of following main configuration :

Column : C-18

Detector : UV - Vis

Temp : Ambient

Wave length : 215 nm

Mobile phase : Aceto nitrile : Water (isocratic or gradient flow)

10.     Before analysis of sample standardize the HPLC using the good purity (>90%) Standard Reference Material of Azadirachtin (A & B,) Nimbin, Salannin, 6-deacetyl Nimbin and 3-deacetyl Sallanin.

11.     After calibration of the instrument, inject the 20 micro ltr. sample by Syringe or Loop into the HPLC. Wavelength 215 nm acetonitrile water

12.     Identify the peak of Azadirachtin (A & B) Nimbin, Salannin, 6-deacetyl Nimbin and 3-deacetyl Sallanin with their retention time.

13.     Measure the area of peak and calculate the content of Azadirachtin (A & B) Nimbin, Salannin, 6-deacetyl Nimbin and 3-deacetyl Sallanin with multiplying the dilution factor as per BIS-14299 1995.

Preparation of Reference standard : Weigh accurately approx 2.0 mg standard reference material (Azdirachtin, Nimbin & Salannin ) of known purity into 50 ml volumetric flask and dissolve in Methanol: Water (90:10). Make up to mark and shake well. Take 2 ml of this solution and transfer in solid phase extraction cartridge and elute it in to 10 ml volumetric flask with repeated washing with Methnaol : Water (90:10). Make upto mark and use for calibration of HPLC.

Calculation:

4. Determination of phosphates.

Methods of determination of total phosphates, [151][water soluble phosphorus, citrate soluble phosphates (available phosphorus)], citrate insoluble phosphates and citric acid soluble phosphates have been described separately in this section. These methods are applicable to straight as well as mixed phosphatic fertilizers.

(i)       Preparation of solution of the samples. (Separate methods of preparing solutions of the samples have been described according to the nature of the sample.)

(a)      Reagent

Magnesium nitrate solution- Dissolve 950mg.

P-free Mg(NO3)2 6H2 in water and dilute to 1litre.

(b)      Procedure.

(1)     Treat 1gm sample by (A), (B), (C), (D) or (E) method depending on the nature of the sample.

(2)     Cool solution transfer to 200 to 250ml. volumetric flask dilute to volume, mix and filter through dry filter.

(A)     (Suitable for materials containing small quantities of organic matter) Dissolve in 30ml. HNO3 and 3-5 ml. HCl and boil until organic matter is destroyed.

 

(B)     (Suitable for fertilizers containing much Fe or Al phosphate and basic slag). Dissolve in 15-30 ml. HCl and 3-10 ml. HNO3.

 

(C)     (Suitable for organic material like cotton seed meal alone or in mixture). Evaporate with 5ml. Of the Mg. (NO3)2 solution, ignite and dissolve in HCl.

 

(D)     (Generally applicable to materials or mixtures containing large quantities of organic matter). Boil with 20-30 ml. H2SO4 in 200ml.flask adding 2-4 gm of NaNO3 or KNO3at beginning of digestion and small quantity after solution is nearly colourless, or adding the nitrate in small portions from time to time. When solution is colourless, cool, add 150 ml. Water and boil for few minutes. Before adding NaNO3 or KNO3 let mixture digest, at gentle heat if necessary, until violence of reaction is over.

 

(E)     (Suitable for all fertilizers). Boil gently for 30-45 minutes with 20-30ml. HNO3 in a suitable flask (preferably a Kjeldahl for samples containing large quantities of organic matter to oxidize all easily oxidizable matter) Cool and add 10-20 ml. of 70-72 percent nearly so and transparent dense fumes appear in flask. Do not boil to dryness at any time (danger). (with samples containing large quantities of organic matter temperature should be raised to fuming point approximately 170C over a period of 1 hour at least) Cool slightly, add 50ml. water and boil for few minutes.

(ii)      Gravimetric quinoline, molybdate method for determination of total phosphorus.

(a)      Reagents.

(1)     Citric molybdic acid reagent- Dissolve 54 gm. 100 percent molybdic anhydride (MoO3) and 12gm. NaOH with stirring in 400ml. hot water and cool. Dissolve 60gm. citric acid in mixture of 140 ml. HCL and 300ml. water and cool. Gradually add molybdic solution to citric acid solution with stirring. Cool, filter and dilute to 1litre. (Solution may be green or blue colour depends on exposure to light). If necessary add 0.5 percent KrO3 solution drop by drop until green colour becomes pale. Store in dark in polyethylene bottle.

 

(2)     Quinoline solution -Dissolve 50ml. synthetic quinoline with stirring in mixture of 60ml. HCl and 300ml Water. Cooldilute to 1 litre, and filter. Store in polyethylene bottle.

 

(3)     Quimociac reagent- Dissolve 70gm. of sodium molybdate dihydrate in 150 ml. water Dissolve 60gm citric acid in mixture of 85ml. HNO3 and 150ml. water and cool. Gradually add molybdate solution to citric acid-nitric acid mixture with stirring. Dissolve 5ml. synthetic quionoline in mixture of 35nl. HNO3 and 100ml. water Gradually add this solution to molybdate citric -nitric acid. solution mix and let it stand for 24 hours. Filter add 28 ml. acetone. dilute to 1 litre with water and mix well. Store in polyethylene bottle.

(b)      Procedure.

(1)     Treat 1mg. sample as prescribed in 4(1) and dilute it to 200ml.

(2)     Pipette into 500ml erlenmeyer flask aliquot containing not more than 25mg. P2O5 dilute to approximately 100ml with water.

Proceed with one of the following methods.

A.        Add 30ml. citric molybdic acid reagent and boil gently for 3 minutes. (Solution must be precipitate free at this stage) Remove from heat and swirl carefully. Immediately add from burette 10ml quinoline solution with continuous swirling (Add first 3-4 ml drop wise and remainder in steady steam) or

B.        Add 50ml quimociac reagent, cover with watch glass place on hot plate in well ventilated hood and boil for 1 minute. After treatment with A or B cool to room temperature, swirl carefully 3-4 times during cooling filter into gooch with glass fibre filter paper previously dried at 250 C and weighed, and wash five times with 25ml. portion of water. Dry cruicible andcontents for 30 minutes at 250C. cool in desiccator to constantweight as (C9H7N) 3H3PO4.12 MoO3 subtract weight reagent blank.

Multiply by 0.03207 to obtain weight of P2O5. Report as percent P2O5.

(iii)     Determination of water soluble phosphorus

(a)      Procedure

(1)     Place 1gm sample on 9cm filter paper and wash with small portion of water until filtrate measure approximately 259ml.

 

(2)     Let each portion pass through filter before adding more and use suction if washing would not otherwise be complete within 1 hour.

 

(3)     If the filtrate is turbid, add 1-2 ml. HNO3dilute to 250ml and mix.

 

(4)     Pipette into 500ml. Erlenmeyer flask aliquot containing not more than 25mg. P2O5.

 

(5)     Dilute if necessary to 50ml.

 

(6)     Add 10ml. HNO3 (1plus 1) and boil gently for 10minutes. Cool and dilute to 100ml. and proceed as 4(ii) (b)(2) (B).

(reference- methods of analysis AOAC, 1965)

(iv)    Citrate insoluble phosphorus.

(a)      Reagents.

1.        Ammonium citrate solution - should have specific gravidity of 1.09 at 200C and pH of 7.0 as determined electometrically.

Dissolve 370 gm crystalline citric acid in 1.5 litre distilled water and nearly neutralize by adding 345 ml. NH4OH (28-29% NH3) if concentration of ammonia is less than 28 percent add correspondingly larger volume, and dissolve citric acid in correspondingly smaller volume of water, cool and check pH. Adjust with NH4 OH (1 plus 7) or citric acid solution to pH 7.Dilute solution if necessary to specific gravity of 1.09 at 200 C(Volume will be approximately 2 litres) Keep in tightly stoppered bottles and check pH from time to time. If pH has changed from 7.0 readjust.

2.        Other reagents and solutions as in 4(i) and 4(ii)

(b)      Procedure (acidulated samples and mixed fertilizers)

(1)     After removing water soluble P2O5. in 4(iii) transfer filter and residue within 1 hour to 200or 250 ml flask containing 100ml. ammonium acetate solution previously heated to 650C.

 

(2)     Close flask tightly with smooth rubber stopper.

 

(3)     Shake vigorously until paper is reduced to pulp and relieve pressure by removing stopper momentarily.

 

(4)     continuously agitate contents of stopper flask in apparatus equiped to hold contents of flask at exactly 650C. (Action of apparatus should be such that dispersion of sample in citrate solution is continually maintained and entire inner surface of flask and stopper is continually bathed with solution).

 

(5)     Exactly 1 hour after adding filter and residue, remove flask from apparatus and immediately filter contents by suction as rapidly as possible through Whatman No. 5 paper or equivalent. using buchner or ordinary funnel with platinum or other cone.

 

(6)     Wash with distilled water and at 650C until volume of filtrate is approximately 350ml. allowing time for through draining before adding more water.

 

(7)     If material is one that will yield cloudy filtrate wash with 2 percent NH4 NO3 solution.

 

(8)     Determine P2O5. in citrate insoluble residue by one of the following methods.

A.        Dry paper and contents transfer to crucible ignite until all organic matter is destroyed and digest with 10-15 ml. HCl until all phosphate dissolve or.

B.        Treat wet filter and contents a s in method prescribed in 4(i) (b) (2) (A) (C) (D) or (E) Dilute solution to 250ml. or other suitable volume, mix well filter through dry paper and determine P2O5. as in 4 (ii)

(Reference - methods of Analysis, AOAC, 1965)

(v)      Citrate soluble phosphorus [152][(Available Phosphorus)]

(Reference S.O. 403 (E) dated 23 May, 1990)

Subtract citrate insoluble P2O5. from total P2O5.to obtain citrate soluble P2O5. in fertilizers other than basic slag.

(a)      Reagents.

(1)     Concentrated hydrochloric acid.

 

(2)     Concentrated citric acid.

 

(3)     Calcium carbonate finely ground

 

(4)     5 N Sodium hydroxide solution.

 

(5)     Dilute hydrochloric acid- Dilute 240 ml or concentrated hydrochloric acid with water to 1 litre.

 

(6)     Citric molybdic acid solution- Stir 54 gm of molybdic anhydride (MoO3) with 200ml. of water add 11gm of sodium hydroxide and stir the mixture whilst heating to boiling point until the molybdic whilst heating to boiling point until the molybdic anhydride dissolves. Dissolve 60gm of citric acid in about 250to 300 ml of water and add 140 ml of concentrated hydrochloric acid. Pour the molybdate solution into the acid solution. Which is stirred solution through paper pulp pad. Dilute the solution to 1 litre. If the solution is slightly green or blue in colour add dropwise a dilute (0.5 to 1.0 percent) solution of potassium bromate until the colour is discharged. This reagent should be kept in dark.

 

(7)     Quinoline solution- Measure 60ml of concentrated hydrochloric acid and 300 to 400 ml of water into 1 litre beaker and warm to 700C-800C pour 50ml. of quinoline in a thin stream into the dilute acid while stirring. When quinoline has dissolved. cool the solution dilute acid to 1 litre and if necessary filter through a paper pulp filter.

 

(8)     Sodium hydroxide solution- 0.5 N carbonate free.

 

(9)     Indicator solution- Mix three volumes of thymol blue solution and two volumes of phenolphthalein solution prepared as follows.

A.        Thymol blue solution- Dissolve 250mg. thymol blue in 5.5 ml of 0.1 N sodium hydroxide solution and 125 ml of industrial methylated spirit. Dilute with water to 250ml.

B.        Phenolphthalein solution- Dissolve 250mg. phenolphthalein in 150 ml of industrial methylated spirit and dilute with water to 250ml.

(10)   Hydrochloric acid- 0.5N.

 

(11)   Sodium hydroxide solution- 0.1N.

 

(12)   Hydrochloric acid- 0.1 N.

 

(13)   Surface active agent- 0.5 percent solution of sodium dodecyi benzene sulphonate suitable.

(b)      Preparation of solution.

(1)     Weigh to the nearest mg. about 5gm. of the sample and transfer to a stoppered bottle of about 1 litre capacity.

 

(2)     Dissolve 10gm. of pure crystallized citric acid (monohydrate) in water dilute to 500ml and adjust the temperature to 200C.

 

(3)     Add the solution to the sample in the bottle, shaking so as to avoid the possibility of caking.

 

(4)     Shake the bottle continuously for 30 minutes.

 

(5)     Pour whole of the liquid at once on to a large medium fine filter. and collect the filtrate. If the filtrate is not clear, pass it again through the same filter.

(c)      Procedure.

(1)     Transfer a volume of the solution prepared according to procedure given above containing less than 70mg. of phosphoric acid and preferably about 50mg. to a 500ml stoppered conical flask marked at 150ml.

 

(2)     Dilute the solution with water to 100ml.

 

(3)     If the sample does not contain calcium add 100 to 200mg. of calcium carbonate.

 

(4)     Then add 5 N sodium hydroxide solution dropwise until a faint permanent turbidity or precipitate is formed.

 

(5)     Dissolve the precipitate by the dropwise addition of dilute hydrochloric acid but avoid an excess.

 

(6)     Dilute to 150 ml and add 50ml of the citric-molybdic acid reagent and heat the solution to incipient ebullition, maintain it at this temperature for 3 minutes and then bring it to the boiling point.

 

(7)     From burette slowly add 25ml of the quinoline solution with constant swirling throughout the first few ml. being added dropwise, the rest in slow stream.

 

(8)     Keep the solution gently boiling during the addition.

 

(9)     Immerse the flask in boiling water for 5 minutes, then cool it to 150C in funning water.

 

(10)   Filter with suction the contents of the flask on a paper pulp pad, and wash the flask precipitate and filter with successive small washes of cold water until they are free from acid.

 

(11)   Transfer the filter pad and precipitate to the original flask, rinse the funnel with water and collect the rinsings in the flask.

 

(12)   If necessary, wipe the funnel with small piece of damp filter paper to ensure complete removal of the precipitate and place the paper in the flask.

 

(13)   Add water to a total of about but not exceeding 100ml Stopper the flask and shake it vigorously until the pulp and precipitate are completely dispersed.

 

(14)   Remove the stopper and wash it with water returning the washing of the flask.

 

(15)   Add a measured volume of 0.5 N sodium hydroxide solution sufficient to dissolve the precipitate and leave a few ml. in excess.

 

(16)   Shake the flask vigorously until all the precipitate dissolves. (To facilitate the dispersal of the precipitate, after the addition of 0.5 N sodium hydroxide solution a few drops of the surface active agent may be added if necessary)

 

(17)   Add 0.5 -1.0 ml of the indicate solution and titrate the excess of sodium hydroxide with 0.5 N hydrochloric acid until the indicator changes from violet to green-blue and then very sharply to yellow at the end point.

 

(18)   Deduct the number of ml of 0.5 N hydrochloric acid used from the number of ml. 0.5 N sodium hydroxide equivalent to the phosphoric acid.

 

(19)   Carry out a blank determination on all the reagents. omitting only the sample and using 0.1 N standard alkali and acid instead of 0.5 N for the titration. Calculate the blank in terms of 0.5 N alkali and subtract it from the original result.

 

(20)   Calculate the amount of phosphoric acid in the portion taken for analysis from the factor 1.0ml. of 0.5 N Sodium hydroxide = 1.366 mg P2O5

(Reference -Statutory Instruments 1960 No. 1165 Agriculture, the fertilizer and feeding stuffs Regulations. 1960)

(vi)    Free phosphoric acid as (P2O5)

(a)      Reagents.

(1)     Acetone-conforming to IS:170-1950 specification for acetone.

 

(2)     Standard sodium hydroxide solution-0.1 N

 

(3)     Bromocresol green indicator solution- dissolve 0.1 gm of bromocresol green in 100ml of rectified spirit conforming to IS323-1959specification for rectified spirit (Revised).

(b)      Procedure.

(1)     Weigh accurately about 2.5 mg of the prepared sample and transfer to a soxhlet extract or

 

(2)     Add about 100ml of acetone and extract for three hours.

 

(3)     Cool and distil off the acetone as far as possible.

 

(4)     Take up the residue with water and make up the volume to 250ml.

 

(5)     Pipette out exactly 100ml of this solution and titrate with standard sodium hydroxide solution, using bromocresol green as indicator until colour just changes from yellow to blue.

Calculations: Free phosphoric acid (as P2O5)

Percent by weight = -17.75 x V x N/W

Where

V= Volume in ml of standard sodium hydroxide solution used.

N= normality of standard sodium hydroxide solution and

W= weight in gm of sample taken for the test.

(Reference- IS Specification for superphosphate (revised)

IS 294- 1962)

5. Determination of potassium.

Determination of potassium in all kinds of fertilizers is given in this section. Two alternative methods have been described. Any of these two methods may be used depending upon the availability of reagent and suitability of the method.

(i)       Prechloric acid method.

(This method depends on the insolubility of potassium perchlorate and the solubility of sodium perchlorate in alcohol and is applicable in presence of alkali metals chlorides and nitrates. Sulphates and ammonium salts must be absent on account of the low solubility of sodium sulphate of ammonium perchlorate in alcohol. Phosphates must be removed. Methods are given for the elimination of the effect of interfering substances)

(a)      Reagents.

(1)     Concentrated hydrochloric acid.

 

(2)     Barium chloride solution- Dissolve 100gm of barium chloride in water filter the solution and dilute to 1 litre.

 

(3)     Dilute hydrochloric acid-- Dilute 240 ml of concentrated hydrochloric acid with water to one litre.

 

(4)     Calcium oxide 0-- finely ground.

 

(5)     Ammonium hydroxide solution- sp. gr. 0.88.

 

(6)     Ammonium carborate solution- saturated aqueous solution.

 

(7)     Ammonium oxalate solution saturated aqueous solution.

 

(8)     20 percent perchloric acid solution.

 

(9)     Alcohol industrial methylated spirit 95-96 percent V/V.

 

(10)   Wash solution- Add potassium perchlorate to alcohol and shake until saturated solution is obtained, Keep the solution over solid potassium perchlorate and filter immediately before use.

(b)      Potassium salts free from sulphates and other inferfering substances.

(1)     Dissolve in water a portion of the sample weighed to the nearest mg. equivalent to potassium content to 1.5 to 2.0 mg. of potash.

 

(2)     Cool the solution to 200C dilute to 500 ml in a volumetric flask mix well and filter through a dry filter.

 

(3)     Determine the potash in 50ml of solution by precipitating with perchloric acid as described under procedure.

(c)      Potassium salts with sulphates or other interfering substances.

(The following method is given for eliminating the interference caused by presence of sulphate. If salts contain phosphates, iron, manganese or substances other than sulphate that interfere with the determination of potash the method described for mixed fertilizer should be used.)

(1)     Weigh to the nearest mg a portion of the sample equivalent in potassium content to 1.5 to 2.0 mg of potash into a 500ml beaker. Add about 300ml of water and 20ml concentrated hydrochloric acid and heat the solution to boiling.

 

(2)     To the boiling solution cautiously add, drop by drop barium chloride solution in an amount slightly in excess of that previously determined as necessary to ensure the complete precipitation of sulphate.

 

(3)     Cool the liquid to 200C transfer to a 500 ml volumetric flask, dilute to 500 ml. mix and filter through a dry filter.

 

(4)     Take 50ml of the filtrate and evaporate to dryness in a basin. moisten the residue with concentrated hydrochloric acid.

 

(5)     Again evaporate to dryness, dissolve the residue with 5-10 ml dilute hydrochloric acid and filter, if necessary.

(6)     Determine the potash in solution by the method described under procedure.

(d)      Potassium in mixed fertilizers.

(1)     Weigh to the nearest centigram about 10gm of the sample and if organic matter is present , gently incinerate at temperature not exceeding 5000C.

 

(2)     Transfer the weighed portion of the sample or the incinerated residue to a 500ml breaker with a little water add 10ml concentrated hydrochloric acid and then warm for ten minutes.

 

(3)     Dilute with water to about 300ml and bring gradually to boiling point.

 

(4)     Add 10gm of calcium oxide made into a paste with water.

 

(5)     Bring contents again gently to the boiling point and keep so heated for about half an hour with frequent stirring .

 

(6)     Cool to 200C transfer to a 500ml volumetric flask dilute to 500ml and after thoroughly shaking filter through a dry filter paper.

 

(7)     Transfer 250ml of the filtrate to another 500ml volumetric flask, make just acid with hydrochloric acid and heat to boiling point.

 

(8)     To the boiling solution cautiously add drop by drop, barium chloride solution until there is no further precipitation of barium sulphate.

 

(9)     Render the contents of the flask alkaline with ammonium hydroxide solution and precipitate the calcium and any excess of barium by adding ammonium carbonate solution until no further visible precipitation occurs followed by the addition of about 1ml of ammonium oxalate solution.

 

(10)   Cool to 200C dilute with water to 500ml and after thoroughly shaking filter through a dry filter paper.

 

(11)   Measure 100ml of the filtrate and evaporate to dryness in a basin. Expel the ammonium salts from the residue by gently heating the basin over a low flame, being careful to keep the temperature below that of faint redness.

 

(12)   Cool the residue, moisten with concentrated hydrochloric acid and again evaporate to dryness.

 

(13)   Take up the residue with water and filter if necessary.

 

(14)   Determine the potash in the solution by precipitation with perchloric acid as described under procedure.

(e)      Procedure.

(1)     Transfer the solution obtained as described above into a basin and add about 7ml of perchloric acid solution.

 

(2)     Place the basin on a hot plate or sand bath and evaporate the contents until the transparent fumes are copiously evolved.

 

(3)     Cool and dissolve the precipitate in a little hot water.

 

(4)     Add about 1ml of perchloric acid solution and again concentrates to the fuming stage.

 

(5)     Thoroughly cool the residue in the basin and stir in 20ml. or alcohol.

 

(6)     Allow the precipitate to cool and settle, then pour the clear liquid through a dry filter paper, drain the precipitate in the basin and stir in 20ml or alcohol.

 

(7)     Allow precipitate to cool and settle then pour the clear liquid through a dry filter paper, drain the precipitate in thebasin as completely as possible.

 

(8)     Redissolve the precipitate on the paper and that remaining in the basin with hot water.

 

(9)     Add 2ml of perchloric acid solution to the combined solution and evaporate the whole down to the fuming stage.

 

(10)   Cool the residue in the basin and throughly stir the contents with 20ml. of alcohol.

 

(11)   Allow the precipitate to cool and settle and pour the clear liquid through a weighed gooch or sintered glass crucible, draining the precipitate as completely as possible from the liquid before adding 5mnl of wash solution.

 

(12)   Wash the precipitate by decantation with several similar small portions of the wash solution, pouring the washing through the crucible.

 

(13)   Transfer the precipitate to the crucible and wash it well with the wash solution until free from acid.

 

(14)   Dry the precipitate at 1000c and weight.

 

(15)   Regard the precipitate as potassium perchlorate (KClO4) and calculate its equivalent as potash (K2O) by multiplying its weight by 0.34.

(Reference- Statutory Instruments 1960 No. 1165 Agriculture the Fertilizer and Feeding Stuffs Regulation 1960).

(ii)      Sodium tetraphenyl boron method-This method is applicable to both mixed and straight potassium fertilizers.

(a)      Reagents.

(1)     Sodium hydroxide solution-20 percent. Dissolve 20gm NaOH in 100ml distilled water.

 

(2)     Formaldehyde solution-37 percent.

 

(3)     Sodium tetraphenyl boron (STPB) solution- approximately 1.2 percent. Dissolve .012gm sodium tetraphenyl boron in approximately 800 ml water. Add 20-25 ml Al (OH3 )stir for 5 minutes, and filter (Whatman No. 42 paper or equivalent) into 1 litre volumetric flask, Rinse beaker sparingly with water and add to filter. Collect entire filtrate add 2ml 20 percent NOH solution, dilute to volume with water and mix. Let it stand for 48 hours and standardize. Adjust to that 1ml STPB-1 percent K2O. Store at room temperature.

 

(4)     Quaternary ammonium chloride solution- approximately 0.625 percent. Dilute 50ml of 12.8 percent zephiran chloride to 1litre with water, mix and standardize. Cetyltrimethyl. If other concentration is used, adjust volume.

 

(5)     Clayton yellow- 0.04 percent. Dissolve 40mg in 100ml water.

(b)      Standardization of solutions.

(1)     Zephiran chloride-to 1.0ml STPB solution in 125 ml. Erlenmeyer flask add 20-25 ml water 1ml 20 percent NaOH 2.5 ml HCHO 1.5 ml 4 percent (NH4) 2 C2O4 and 6-8 drops of indicator (5) above.

 

(2)     Titrate to pink end point with zephiran chloride solution, using 10ml semimicro burette, Adjust zephiran chloride solution so that 2.0 ml = 1.0 ml STPB solution.

 

(3)     Sodium tetraphenyl boron solution- Dissolve 2.5 gm of KH2 PO in water in 250 ml volumetric flask, add 50ml 4 percent (NH4) 2C2O4solution, dilute to volume with water and mix.

(It is not necessary to brig to boil) Transfer 15ml aliquot (51.92 mg (K2 O43.10mg K) to 100ml volumetric flask add 2ml 20 percent NaOH, 5ml HCHO and 43 ml STPB reagent. Dilute volume with water, mix throughly, let stand 5-10 minutes and pass throughly dry filter. Transfer 50ml aliquot of filtrate to 125 ml. Erlenmeyer flask add 6-8 drops of indicator

(4)     above and titrate excess reagent with zephiran solution.

Calculate titration values as follows.

F= 34.61 (43 ml-ml zephiran) =% K2 O/ml STPB reagent. factor applies to all fertilizers if 2.5 gm sample is diluted to 250 ml and 15 ml aliquot is taken for analysis, If results are to be expressed as K rather than K2O, substitute 28.73 for 34.61 in calculating the value of F.

(c)      Preparation of solution.

(1)     Mixed fertilizer.

A.        Place 2.5 gm sample or factor weight. 2.430 gm in 250 ml volumetric flask.

 

B.        Add 125 ml water and 50ml saturated (NH4) 2C2O4 solution. Add 1ml of diglycol stearate solution if needed to prevent foaming.

 

C.        Boil for 30 minutes add slight excess of NH4OH and after cooling dilute to 250ml. Mix and pass through dry filter.

(2)     Potassium salts (Potassium chloride sulphate, potassium magnesium sulphate, and kainite)

A.        Dissolve 2.5 gm or factor weight 2.430 gm and dilute to x 250 ml without adding NH4OH and (NH4) 2C2O4

 

B.        When interfering substances such as NH3, Ca, Al, etc. are present proceed as in (1) above.

(d)      Procedure.

(1)     Transfer 15ml aliquot of sample solution to 100ml volumetric flask and add 2ml 20percent NaOH and 5ml HCHO.

 

(2)     Add 1ml standard STPB solution for each 1percent K2O expected in sample plus additional 8ml excess to ensure complete precipitation.

 

(3)     Dilute to volume with water mix thoroughly, let it stand for 5-10 minutes and pass it through dry filter (Whatman 12 or equivalent).

 

(4)     Transfer 50ml filtrate to 125 ml Erlenmeyer flask,. add 6-8 drops of indicator (5) above and titrate excess reagent with standard zephiran solution.

Percent K2O in the sample = (ml STPB added-ml zephiran)X F where F= percent-

K2O/ml STPB reagent. (Reference- Methods of Analysis, AOAC, 1965)-

6. Method of analysis of anhydrous ammonia

(i)       Estimation of water and ammonia.

(a)      Scope

This method is for the determination of water at 200C (or room temperature) (and usually ammonia by difference) of any essentially anhydrous ammonia liquid product. Normally, the water will be low (less than 0.5 percent) or sample of synthetic ammonia.

(b)      Apparatus.

(1)     Ammonia sampling tubes.

 

(2)     Fume hood with exhaust dust.

 

(3)     Sample tube holder rack in hood fabricated as convenient to hold number of tubes desired.

 

(4)     Gloves, protective, elbow length.

(c)      Reagents

Charcoal, reagent, 14-20 mesh.

(d)      Procedure.

(1)     Remove the sample tubes from the sample carrier and place in the provided sample tube holders in the fume hood.

 

(2)     Allow the ammonia sample to boil and to evaporate (approximately 30 minutes) spontaneously in the fume hood. Because of the low temperature of the boiling ammonia atmospheric moisture freezes on the sample container. Exercise care to see that none of this ice contaminates the sample.

 

(3)     When the boiling of the sample ceases, remove the tube from the holder. Wipe the outer surface of the tube dry and read and record the volume of liquid residue in the tube.

 

(4)     From the volume recorded, calculate the weight percent water in the sample. Ignore the small piece of charcoal, if used.

Calculation: Percent water = A x F x 0.890 x 0.684 / V x 0.682 x 100

Where A = Volume of residue in tube (ml)

V = volume of sample taken (ml)

F = Evaporation factor, taken from table 1 corresponding to noted sample pressure when sample was obtained.

0.890=density of residue (gm/ml)

0.684=wight fraction of water in residue.

0.682=density of sample (gm/ml)

Precaution: The evaporation in the fume hood should be conducted with the window lowered to protect personnel from possible spray. Whenever it is necessary to handle the sample tubes, protective gloves should be worn.

Note: Determination of residue on evaporation will not usually be necessary for normal ammonia sample. If sample is clear and water residue is clear and colourless, the residue may be considered to be nil. However, should it become necessary to determine the dissolved solids and suspended solids in anhydrous ammonia, proceed, as follows:

(e)      Sampling

Thoroughly clean and dry the sample tubes, weigh (W1) each selected tube to the nearest milligram with a similar tube as counterpoise. Obtain the sample as desired earlier.

(f)       Apparatus.

(1)     Analytical balance.

 

(2)     Ammonia sampling tubes.

 

(3)     Rubber tubing 1/4" OD length desired.

 

(4)     Reagents

(g)      Air dry, carbondioxide –free

(h)     Procedure

(1)     Start test following elimination of the water content of the sample as given earlier.

 

(2)     Connect one end of a rubber hose to a source of dry, carbon dioxide free air, Insert the other end of the hose into the sample tube and gently force air through the sample tube until all liquid has been evaporated and no ammonia gas remains in the tube.

 

(3)     Wipe a counterpoise and the sample tube containing the residue to substantially the same extent to remove moisture which may have condensed on their outer surfaces.

 

(4)     Weigh the sample tube and residue to nearest milligram.

 

(5)     Calculate the weight percent residue of the sample.

Calculation: percent residue = (W2-W1) x f x 100 / V x 0.682

Where W1 =weight (gm) 0f tube (before sampling).

W2=weight (gm) of tube and residue.

V =Volume of sample taken (ml).

F =Evaporation factor, taken from Table 1 corresponding to noted sample pressure when sample was obtained.

0.682 =density of sample (gm/ml).

(i)       Precaution.

A check of completeness of evaporation may be made by visual inspection and by carefully smelling the air in the tube making sure that no carbon dioxide or moisture from the sample tube.

(j)       percent ammonia content (by difference)

In general, the ammonia content of the sample will be percent ammonia =100 (percent water percent residue, if determined).

(i)      Precaution

The evaporation in the fume hood should be conducted with teh window lowered to protected personnel from possible spray. Whenever it is necessary to handle the sample tubes protective gloves should be worn.

(ii)    Determination of oil content.

(a)      Apparatus.

(1)     500 ml conical flask calibrated to hold 300ml (about 200gms)of sample and with a bunk fitted with glass through which the exit gas. can be led away to a safe place. Ensure the glass tube and exit line are free from constructions.

(2)     Platinum dish 75 mm in diameter.

(b)      Reagent

The reagent use shall be of a recognised analytical reagent quality like petroleum spirit with a boiling range of 400 to 600C.

(c)      Procedure

(1)     Quickly running the sample (as per the sample procedure) upto the calibration mark, insert the bunk.

 

(2)     Immerse the flask in a continuous stream of cold water and allow the ammonia to evaporate slowly.

 

(3)     When the evaporation is complete, remove the bunk and gently blow out the last traces of ammonia with a small jet of filtered air free from carbon dioxide.

 

(4)     Dry the outside of the flask.

 

(5)     Place the flask in an oven at 105+50C for 15 minutes to remove the moisture blowing out the last traces with a gentle stream of filtered air at the end of this period allow to cool.

 

(6)     Add to the flask approximately 100ml of the petroleum spirit and swirl to dissolve the oil.

 

(7)     Filter the solution through a small filter paper (a Whatman No. 31 paper is suitable)direct into the platinum dish previously traced to the nearest 0.1 mg.

 

(8)     Repeat the operation with two more successive 10ml portions of petroleum spirit, filtering through the same paper as before into the same dish.

 

(9)     Evaporate the combined extracts to dryness on a water bath in a fume cup board, taking care to avoid naked lights and finally dry in an oven at 105+50C for 30 minutes.

 

(10)   Allow the dish to cool thoroughly in desicator and weigh again to the nearest 0.1 mg.

 

(11)   At the same time, carry out a blank determination on the petroleum spirit and filter paper.

 

(12)   Make an appropriate correction in the calculation

Calculation: Oil content, parts per million by weight = (W1 W2)-W3 / 0.68 V2 x 106F / 0.68 V2

Where W1= Weight in grams of platinum dish and residue.

W2 = Weight in grams of dish alone.

W3= Weight in grams of oil in blank determination

V2 = Volume in ml of sample taken.

F = Evaporation factor taken from table 1 corresponding to noted sample pressure when sample was obtained.

Table 1- Evaporation factor for different vessels or line pressures

Note : When a sample of liquid ammonia is transferred to an open flask/tube from a container n which the pressure is higher than the atmospheric that environment. some of the liquid ammonia will evaporate and since the ammonia so lost as vapour contains non-volatile constituents present in the original product, the concentration will increase in the liquid sample taken. This may be significant factor the known thermo dynamic properties of ammonia an appropriate correction. This correction is usually known in this context as the evaporation factor of flask factor and is simply that fraction by weight of the original liquid ammonia which remains as liquid in the sample. Multiplication of the determined quantity of a non-volatile constituents (oil, water dissolved or suspended solids, etc) by the evaporation factor given a result which will be closer to the true figure. The Table above presents the evaporation factor for different vessel or line pressure. When a sample is transferred (example by gravity from a container of a cylinder or the sampler at the same pressure, there should be no loss by evaporation and in this case it is not necessary to use evaporation factor.

7. Method of analysis of zinc sulphate (Both Heptahydrate and Monohydrate)*

(i)       Quality of reagents

Pure chemicals and distilled water shall be used in tests.

Note: Pure chemicals shall mean chemicals that do not contain impurities which affect the results of analysis.

(ii)      determination of matter insoluble in water.

(a)      Reagents

Dilute sulphuric acid - 10 percent

(b)      Procedure

Dissolve 25.0 gm of the material in 125 ml of water and add 1ml of dilute sulphuric acid. Heat the solution to boiling, filter through a weighted and prepared Gooch crucible or sintered glass crucibel (G No.4) and wash the residue throughly with hot water. Dry the crucibel at 1100+50C to constant mass.

Calculation: Matter insoluble in water percent by mass weight=4A

Where A= weight in g of the residue.

(iii)     Determination of Zinc in Zinc Sulphate by modified EDTA titration method.

(a)      Reagents

(1)     E.D.T.A. Solution

Dissolve 3.72 g of Di-sodium Ethylene Diamine Tetracetate dihydrate in distilled water and make up the volume to 1litre

(2)     Standard Zinc metal solution:

Weigh about 1.0g of zinc metal and record the weight accurately. Express this as W, Add HCL (1:1) @ 20ml per g of zinc metal keep it for few hours and allow it to dissolve completely. Make up the volume of the solution to exactly 1000ml.

(3)     Ammonium Hydroxide (20%) (m/m)

 

(4)     Ammonium Chloride -AR grade salt

 

(5)     Sodium Cyanide -AR/GR grade salt.

 

(6)     Eriochrome Black (T) indicator mixture Mix thoroughly 1g of Eriochrome Black (T) indicator with 100g of AR grade sodium chloride.

 

(7)     Formaldehyde -Acetic Acid solution (4%)Dissolve 100ml of Formaldehyde (37-40%) in about 100ml of distilled water. Add 40ml glacial Acetic acid and make volume to 1litre with distilled water.

 

(8)     Hydroxylamine HydrochlorideAR Grade solid salt.

(b)      Procedure.

(1)     Standardization of EDTA solution.

(A)     Take 10ml of Zinc metal solution (Standard)

 

(B)     Add about 0.1 g of ammonium chloride and 30ml of ammonium hydroxide solution (20%)

 

(C)     Dilute it by adding about 30ml distilled water.

 

(D)     Add a pinch of eriochrome black (T) indicator mixture.

 

(E)     Titrate in with EDTA solution to obtain clear blue end point Note the volume of EDTA used as V1 ml.

(2)     Estimation of Zinc in samples.

(A)     Weigh accurately 1.0 g of a given zinc sulphate sample and dissolve it in 100ml of distilled water in a volumetric flask

 

(B)     Take 10ml of aliquot in beaker. Add 0.1 g of hydroxylamine hydrochloride and 0.1 g of ammonium chloride

 

(C)     Cautiously add small quantity of sodium cyanide. White precipitate will appear, Continue adding sodium cyanide till transparent precipitate disappears while swirling the beaker with hand. Add about 0.5 excess of sodium cyanide.

 

(D)     Dilute it by adding about 30ml of ammonium hydroxide (20%) and add about 30ml of distilled water.

 

(E)     Add a pinch of eriochrome black (T) indicator mixture. It will give red colour.

 

(F)      Titrate with EDTA solution till there is a sharp change to violet colour. Note the volume of EDTA used as V2 (ml)

 

(G)     Add 20ml of Formaldehyde -acid solution into above titrated solution and mix well. Red colour will reappear.

 

(H)     Titrate it with EDTA solution to get blue end point without red tinge. Note the volume of EDTA used in second titration as V3ml.

Calculation: Zinc % = 10 / V1 X V3 x W

W = Weigh in g of piece of Zinc metal taken for preparation of standard zinc solution

V1 = Volume of EDTA solution (in ml) used for 10ml of Zinc metal

V3 = Volume of EDTA solution (in ml)used for second titration

(iv)    Colorimetric method for determining of copper.

(a)      Reagent-

Outline of the method Sodium diethyldithiocarbamate reacts with slightly acidic or ammonical solution of coper in low concentration to produce a brown colloidal suspension of the cupric diethtyldithiocarbamante. The suspension can be extracted with an organic solvent and the colour extracted determined spectrophotometrically.

(b)      Apparatus

Photometer Any suitable photoelectric colorimeter.

(c)      Regents.

1.        Ammonium citrate solution 40percent (m/v)

 

2.        Sodium diethyldithiocarbamate 0.1 percent (m/v)

 

3.        Standard copper solution- Clean the surface of a copper wire with sand paper. Dissolve 100 mg of pur copper in dilute nitric acid. Heat the solution nearly to dryness to drive off the acid. Add about 10 ml of water and heat again nearly to dryness. Take upthe residue in water, add 25 ml of 1 N sulphuric acid and dillute to 1000 ml. One mililitre iof this solution contains 0.1 mg of copper (as Cu)

Alternatively dissolve 3.928g cupric sulphate (CuSO25H2O) in sufficient water containing 1 or 2 ml of concentrated sulphuric acid and dilute to 1000 ml. One ml of the solution contains 1.0 mg of copper (as cu)

(d)      Preparation of sample.

(1)     Weigh 5g sample accurately, dissolve in distilled water and add 1ml of sulphuric acid. Filter the solution and make up to 250 ml with water in a volumetric flask. Take 50 ml or the above solution in a beaker, heat, pass hydrogen sulphide gas or add sodium sulphide solution and ensure complete precipitation. Filter hot and keep the filtrate for subsequent analysis.

 

(2)     Boil the residue with diluter nitric acid and filter , if necessary To the filtered solution add sulphuric acid, evaporate, dilute and filter. Keep the residue for determination of lead.

(e)      Procedure for determination of copper.determine copper in the filtrate from (d) (2) above by diethyldithiocarbamate method as detailed below:-

Transfer an aliquot containing not more than 0.65 mg of copper to a 100ml. separating funnel. Add 2ml of ammonium citrate solution and adjust the pH to 8.5 with ammonium hydroxide. The presence of ammonium ions helps to dionize iron, if present, and to prevent rapid fading of developed colour. Add 10ml of sodium diethyldithiocarbamate solution and develop the colour. Extract the coloured complex with 5-19ml of carbon tetrachloride. Separate the carbon tetrachloride layer from aqueous layer and centrifuge for 5 minutes to separate the water droplets. Transfer the carbon tetrachloride solution to a photometeric cell and measure its absorbance at the wave length of maximum absorption 440 ms relative to reagent blank. Calculate the corrected absorbance by subtracting the reading obtained for the solution containing no copper.

Transfer to a series of 100 ml separating funnels aliquot of standard copper solution corresponding to 0,0.1,0.2,0.5,1.0,2.0 and 2.5 mg of copper and proceed exactly as prescribed above. Plot a graph of corrected, absorbance of solution against their copper contents.

Note: If bismunt is suspected it has to be separated or otherwise accounted for.

Calculation: Calculate the corrected absorbance by subtracting the value obtained for the black from that obtained for the test solution and read from the calibration curve the corresponding mass of copper.

Copper (as Cu), cent by mass = M1 / M2 x 100

Where M1 = mass in g of copper as determined in the given aliquot of the test solution, and M2 = mass in g of the material present in the aliquot of the test solution.

(v)      Determination of lead by colorometric method using dithizone.

(a)      Apparatus

Nessler cylinders - 50ml capacity.

(b)      Reagents.

(1)     standard lead solution- Dissolve 0.40 g of lead nitrate (pb(NO3)2)in water containing 2 or 3ml of concentrated nitric acid and make up the volume to 1000ml with water. Transfer 10ml of this solution to a volumetric flask add 20or 3 ml of concentrated nitric acid and dilute with water to 1000 ml. One milliliter of this solution contains 2.5 mg of lead (as pb.) The diluted solution shall freshly prepared.

 

(2)     Dilute ammonium hydroxide- 1N, approximately.

 

(3)     Reagent A- Dissolve 25g of triammonium citrate or 22 g of citric acid and 4 g of hydroxylamine hydrochloride in about 200ml of water. Add dilute ammonium hydroxide to bring the pH to 8.5 Dilute the solution to 500ml. Purify this solution by extracting with 15ml portions of 0.01 percent dithizone solution until the final colour of the dithizone extract is green. Wash the aqueous remainder portion three times with 25ml portions of chloroform and finally with 25ml portion of carbon tetrachloride.

 

(4)     Dithizone (diphenyl thiocarbazone or phenylazothiomoformic acid ) solution- Dissolve 0.001 g of dithizone in 100ml of carbon tetrachloride, shaking intermittently for 1 hour. Allow to stand overnight and shake once again before using. This shall be kept in a cool and dark place. This gives a 0.01 percent solution. Filter if necessary. Dilute 10ml of this solution to 100ml with carbon tetrachloride in a 100ml volumetric flask. This shall be prepared fresh before determination. This gives a solution of 0.001 percent

Note -1: carbon tetrachloride used should be further purified. One Liter of carbon tetrachloride is extracted with two portions of 25ml dilute ammonium hydroxide and then kept over 100g of activated carbon. Before use, it is decanted and distilled at about

Note -2: Sometimes dithizone solid and its 0.01 percent solution deteriorate on storage. The 0.01 percent solution should, therefore be tested before further dilution, by shaking 2ml of the solution should, therefore be tested before further dilution by shakeing 2ml of the solution with 5ml of 1 percent ammonium hydroxide. If the organic layer is only faintly yellow under these conditions, the solution may be used. If it is deeply coloured it shall be discarded and fresh solution may be used. If it is deeply coloured it shall be discarded and fresh solution be prepared. The solution as well as the reagent should be stored in a refrigerator and exposure to sunlight should be avoided during analytical work. To increase the stability of 0.01 percent solution, it should be covered with a thin aqueouslayer saturated with sulphur dioxide.

(5)     Thymol blue indicator solution- 1 percent (m/v) solution-in rectified spirit.

(c)      Procedure

(1)     Take several aliquots of standard lead solution into a series of separating funnels, add 5ml of the water and 10ml of the reagent A. Then add 2 drops thymol blue indicator and bring the pH of the solution to 8.5 by addition of dilute ammonium hydroxide. Add 5ml of the dithizone solution and shake well for about 10 seconds. Drain the organic layers into stoppered Nessler cylinders.

 

(2)     Dissolve the residue obtained in iv (d)(2) above, in dilute nitric acid and dilute with water. Take a suitable aliquot of the solution and transfer to a separating funnel. Develop the colour as prescribed above. Drain the organic layer into a stoppered Nessler cylinder, add 10ml of dilute ammonium hydroxide and shake for about 10 seconds. Compare the colour developed with those of the standard solution. Note the volume of the standard with which the colour of the test solution matches.

Note: If the colour of the test solution is intermediate between two standard solutions. then the experiment is repeated by taking more number of standard solutions in that range and exact colour matching is arrived at.

Calculation: Heavy metal (as pb) percent by mass = 100 x Y x f /M

where V= Volume in ml of standard lead solution matching with the test solution

f= mass in g of heavy metals (as Pb) equivalent to 1ml of standard lead solution and

M= mass in g of the material in the aliquot taken for the test.

(vi)    Determination of magnesium in the sample material.

(a)      Reagents.

(1)     Eriochrome black T indicators- Dissolve 0.1 g of eriochrome black T in 25ml of methyl alcohol.

 

(2)     Ammonium hydroxide -ammonium chloride buffer solution- Mix 350 ml of ammonium hydroxide (20percent w/w) with 54 g of ammonium chloride, Dilute with water and make up the volume to 1000 ml (the pH of the solution should not be more than 10)

 

(3)     Standard magnesium solution- 0.01 M weigh 2.4640 g of magnesium sulphate (MgSO4.7H2O) and dissolve it in water. Make up the volume to one litre.

 

(4)     Ethylenediamine tetra-acetate (EDTA) solution- Dissolve 3.72 g of disodium ethylenediamine tetra-acetate dihydrate in water and make up the volume to one litre.

(b)      Procedure

Standardization of EDTA solution- Take 10ml of standard magnesium solution in a conical flask. Add 20ml of water, one millilitre of eriochrome black T indicator and 25ml of ammonium hydroxide ammonium chloride buffer solution. Heat at 40 to 50 C and then titrate with EDTA solution, maintaining the temperature between 40 and 50 C until the colour changes form wine red to distinct blue.

Molarity of EDTA Solution = 10M1 / V1

Where M1= Molarity of standard magnesium solution and

V1= Volume in ml of EDTA solution used for titration

(c)      Determination of magnesium in the sample material

Take the filterate from (iv) (d) (1) (after removal of copper) add a few drops of concentrated nitric acid. boil and cool and then add solid ammonium chloride (about 2 grams) boil and cool and ammonium hydroxide till the strong smell of ammonia comes and filter the precipitate through sintered crucible take this filterate and add dilute sulphuric acid till the solution is acidic (test with methyl red) heat the solution to boil and add excess of di-ammonium-hydrogen phosphate with continuous stirring. Add 10 percent ammonia solution with continuous stirring till the solution is just alkaline (test with methyl red) while precipitate of zinc ammonium phosphate will be formed (the optimum pH of r precipitation is 6-7 allow it to stand for 3-4 hours. Filter through whatman filter paper no. 40.collect the filterate in a volumetric flask. Make up the volume (say 100ml) Take a suitable aliquot (say 10ml) for the determination of magnesium. Add 20ml of water, one ml of eriochrome black-T indicator and 20ml of ammonia hydorxide ammonia chloride buffer solution. Heat to 40C to 50C and titrate with standard EDTA solution maintaining the temperature between 40C and 50C until the colour changes from wine red to distinct blue.

1 ml of 0.01 M-EDTA = 0.2432 mg of 'Mg

Mg = X x 0.2432 / 5

Where X = volume of 0.1 M-EDTA use for titration.

The calculation factor 5 is derived presuming that 5g of material is taken for test and the filterate obtained is 100ml out of which 100ml is titrate.

(vii)   Determination of pH

Dissolve 5gm of the material in freshly boiled and cooled water.

Dilute to 100 ml and mix Determination the pH value of the solution a pH meter.

(viii)  Determination of iron in the sample material (Spectro-photometric Method)

(This method is applicable for Iron contents upto 1mg. in the final aliquot)

(a)      Outline of the method - In test solution iron is determined absorption metrically as Ferrous Iron forms red complex with Ortho-phenanthroline.

 

(b)      Appratus- Photo- elecric-- colorimete.

 

(c)      Reagents

(1)     Bromophenol blue indicator solution 0.4 percent solution in 95 percent ethanol.

 

(2)     Sodium citrate solution 25 percent.

 

(3)     Hydroquinone solution- 1 percent in an Acetic acid buffer of pH 4.5 obtained by mixing 65 ml of 0.1 M acetic acid with 35ml of 0.1 M Sodium Acetate solution.

 

(4)     Ortho-phenanthroline solution - 0.25 percent in 25 percent ethanol.

 

(5)     Dilute Hydrochloric acid- 1.3 (v/v)

 

(6)     Standard Iron solution - Dissolve 0.7002 gm. of Ammonium Ferrous Sulphate (AR) in distilled water containing 2ml of perchloric acid and dilute to 100ml with water. One ml of this solution contains 1mg of Iron.

(d)      Preparation of sample solution

Boil 1 gm. sample in 20ml of Hydrochloric Acid (1:1) for 20 minutes and filter through Whatman No. 40 filter paper in 100ml. volumetric flask. Follow with repeated extraction with boiling dilute Hydrochloric acid (1:5) decanting the solution each time through the same filter paper. Dilute the filterate to 100ml.

(e)      Procedure.

(1)     Take 5ml of the sample solution add bromophenol blue indicator solution and titrate with Sodium Citrate solution until yellow colour changes to blue.

 

(2)     Take another 5ml of sample solution in a 25 ml. volumetric flask. Add 1ml of Hydroquinone solution, 3ml of Ortho-phenanthroline solution and an amount of Sodium Citrate solution equivalent to the above titration in step (1) Dilute with distilled water to 25ml. Allow the solution to stand for one hour.

 

(3)     Measure the absorbance of test solution at 510 nm using 1cm. cell and also blank with water.

 

(4)     Place 4,8,12,16 and 20ml of standard Iron solution in a series of 100ml.

 

(5)     Using 5ml. aliquot proceed as for sample solution.

 

(6)     Measure the absorbance of the solution and plot a graph relating to absorbance to number or mgs. of Iron

Calculation: Percent Fe = 2X / W

Where X = concentration (in mg.) of Iron in final sample solution

aliquot as determination from the graph.

W= Weight in gm. of material taken for the preparation of sample

solution"

8. Alternate method of analysis of zinc sulphate (both Heptahydrate) and monohydrate)

(i)       Quality of reagents.

1.        Unless specified otherwise pure chemicals and glass distilled or demineralise water shall be use in test.

Note: Pure chemicals means chemicals that do not contain impurities which affect the results of analysis.

Demineralised water means the water obtained after passing distilled water through a cation and a anion exchange resins or a combined cationation exchange resin.

(ii)      Determination of zinc.

(a)      Reagents.

(1)     Standard zinc solution- Weigh 0.4398 g of zinc sulphate (ZnSO4.7H2O) A.R. grade on a clear watch glass and transfer it to one litre flask through the funnel giving several washings to watch glass and funnel with glass distilled or demineralised water. Add one ml of 10percent sulphuric acid (A.R. grade) and make the volume upto the mark. Stopper the flask and shake the solution well. This is 100 ppm zinc solution herein after called Standard A. This solution should be stored in a clean bottle for further use. Dilute 10ml of 100ppm solution of zinc (Standard A) to 100ml to get 10ppm standard zinc solution designated as Standard B.

 

(2)     Glass distilled or mineralised water of pH 2.5 + 0.5 Dilute 1 ml of 10 percent sulphuric acid to one litre with glass distilled or mineralised water and adjust the pH to 2.5 with a pH meter using H2SO4 or NaOH. This solution is called acidified water and 5 to 10 litres of this solution should be prepared at a time.

 

(3)     Preparation of working standards- Pipette the following volume of Standard B in 50ml numbered volumetric flask and make the volume with acidified water (See Table on page. 93) Stopper the flasks and shake them well. Prepare the standard in duplicate. The same acidified water should be used for preparing the solution of unknown fertilizer samples. Fresh standards should be prepared every time when a fresh lot of acidified water is prepared.

(b)      Procedure.

(1)     Preparation of zinc sulphate fertilizer sample- Weigh 0.25 g of the material on a clean watch glass and transfer it to one litre volumetric flask through the funnel giving repeated washings with glass distilled water and dissolve the material by shaking well. There make the volume upto mark with glass distilled water and shake well.

 

(2)     Take 5ml of the prepared solution in 250ml volumetric flask and make the volume with acidified water. Shake the solution well and filter through Whatman No. 42 filter paper in dry clean flasks. The flasks should be rinsed with a 10 to 15 ml of the filterate and then continue filtration.

 

(3)     Flaming the solutions-- Flame the standards and the filtered samples on atomic absorption spectrophotometer at a wavelength of 213.8 mu (Zn line of the instrument)

Calculations: Prepare a standard curve of know concentrations of zinc solution by plotting the absorbance values on Y-axis against their respective zinc concentration on X-axis Calculate the percentage zinc in zinc fertilizer by multiplying zinc concentration value calculation from standard curve by 20 Example.

Weigh of the fertilizers sample ..................= 0.25 g

Volume made.......................................= 1000ml

Further dilution .................................= 50times

Reading of the samples form atomic absorption.....= Y

Corresponding concentration value of zinc from standard curve against Y absorbance...............= X ppm

Percentage zinc in the fertilizer.................= 20(X)

(c)      Precautions.

(1)     Weighing must be done on a electric balance.

 

(2)     All the glass apparatus to be used should be of corning make and washed with dilute hydrochloric acid (1:4) and washed thoroughly. with distilled and then with demineralise water.

 

(3)     The pipette should be rinsed with the same solution to be measured.

 

(4)     The outside or the pipette should be wiped with filter paper after taking out form the solution to be measured.

 

(5)     After using the pipette, place them on a clean dry filter paper in order to prevent contamination.

 

(6)     To start filtration only a few drops should be added first in order to wet the filter paper and then continue further filtration.

(iii)     Determination of magnesium.

(a)      Reagents.

(1)     Strontium chloride- Dissolve 7.5 g of strontium chloride (SrCl26H2O) in one litre of glass distilled water.

 

(2)     Standard magnesium solution- Weigh 0.507 g of magnesium sulphate (MgSO4.7H2O) on a clean watch glass and transfer it to one litre flask through the funnel giving several washings to watch glass and the funnel with glass distilled or demineralise water. This is 50ppm Mg solution Dilute 10ml of 50 ppm solution of Mg to 100ml to get 5 ppm standard Mg solution.

1.        Preparation of working standards- Pipette the following volume of 5 ppm standard Mg solution in 50ml numbered volumetric flasks. Add 10ml of strontium chloride solution to each flask and make up the volume to 50 ml. Stopper the flask and shake them well prepare fresh standards every for night

(b)      Procedure.

(1)     Pipette 20ml of the solution which was prepared for the determination of zinc by dissolving 0.25 g of the fertilizer sample in one litre flask (Step a-2.2.1) Add 10ml of strontium chloride Make up the volume to 50ml.

(2)     Flame the standards and the samples on atomic absorption spectrophotometer at a wave length of 285.5 mu (Mg line of the instrument)

Calculations: Prepare a standard curve of known concentrations of Mg solutions by plotting the absorbance value on Y-axis against their respective concentration values on X-axis. Percentage magnesium in the zinc fertilizer will correspond to the concentration vales calculated from the standard curve.

Example:

Weight of the fertilizer .............................= 0.25 g

Volume made...........................................= 1000ml.

Further dilution......................................= 2.5 times

Reading of the sample from atomic absorption

spectrophotometer.....................................= Y

Corresponding concentration of Mg from standard

curve against Y absorbance............................= X ppm

Percentage magnesium in the fertilizer...............= X

(iv)    Determination of copper.

(a)      Reagents.

(1)     Standard copper solution- Weigh 0.196 g of copper sulphate (CuSO4.5H2O) on a clean watch glass and transfer it to one litre flask through the funnel giving several washings to watch glass and the funnel with glass distilled water. Add one ml of 10 percent sulphuric acid and make up the volume upto the mark. Stopper the flask and shake the solution well. This is 50 ppm Cu Solution and should be stored in a clean bottle for further use. Dilute 10ml of 50 ppm solution of copper to 100 ml to get 5 ppm standard copper solution.

(2)     Glass distilled or mineralized acidified water of pH 2.5 + 0.5 (same as given in B (ii) (a)(2).

Preparation of working standards- Pipette the following volume of 5 ppm standard copper solution in 50ml numbered volumetric flasks and make the volume with acidified water.

Stopper the flask and shake them well. prepare fresh standard every fortnight.

(b)      Procedure.

(1)     The solution which was prepared for the determination of zinc by dissolving 0.25 g of the fertilizer sample in one litre flask step B(ii) (b)(1) should be used for the determination of copper

(2)     Flame the standards and the samples on an atomic absorption spectro photometer at a wavelength of 324.8 mu (Cu line of  the instrument)

Calculations: Prepare a standard curve of known concentrations of copper

solutions by plotting the absorbance values on Y-axis against their

respective concentration values on X-axis calculate the percentage

copper in the zinc fertilizer by multiplying the copper in the zinc

fertilizer by multiplying the copper concentration value calculated

from the standard curve by 0.4.

Example :-

Weight of the fertilizer sample .........................=0.25 g

Volume made..............................................=1000ml.

Reading of the sample from atomic absorption spectro photometer.............................................=Y

Corresponding concentration of copper from standard

curve against Y absorbance...............................=X ppm

Percentage copper in the fertilizer......................=0.4 x

(v)      Determination of lead.

(a)      Reagents.

(1)     Standard lead solution- Weigh 0.1599 g of lead nitrate (Pb(NO3)2) on a clean watch glass and transfer it to one litre flask through the funnel giving distilled or demineralised water. Add 10ml of concentrated distilled nitric acid and make the volume upto the mark. Stopper the flask and shake the solution well. This is 100ppm lead solution and should be stored in a clean bottle for further use. Dilute 10 ml of 100 ppm solution of lead to 100ml with 1 percent nitric acid solution to get 10 ppm standard lead solution.

 

(2)     1 percent nitric acid solution- Dilute 10ml of concentrated distilled nitric acid to one litre with glass distilled water.

 

(3)     20 percent zinc sulphate solution- Weigh 20g of zinc sulphate (ZnSO4.7H2O) and dilute to 100ml with 1 percent nitric acid solution.

Preparation of working standards- Pipette the following volume of 10 ppm standard lead solution in 50 ml numbered volumetric flasks. Add 5ml of 20 percent zinc sulphate solution to each flask and make the volume with 1 percent nitric acid solution.

Stopper the flasks and shake them well. 

(b)      Procedure.

(1)     Preparation of zinc sulphate fertilizer samples- Weigh 1 g of the material on a clean watch glass and transfer to 50 ml volumetric flask through the funnel giving washings with 1 percent nitric acid solution. Dissolve the material and make the volume with percent nitric acid solution. Samples should be prepared in duplicate.

 

(2)     Flaming the solution-- Flame the standards and the samples on atomic absorption spectrophotometer a a wavelength of 217 m (Lead line of the instrument)

 

(3)     Calculations- Prepare a standard curve of known concentrations of lead solution by plotting the absorbance values on Y - axis against their respective lead concentration on X -axis. Calculate the percentage lead in zinc fertilizer by multiplying lead concentration value calculated from standard curve by 0.005.

(vi)    Determination of pH

(a)      Procedure

Dissolve 5gm of material in freshly boiled water. Dilute to 100ml and mix. Determine the pH value of the solution with pH meter.

(vii)   Determination of matter insoluble in water.

(a)      Procedure

Dissolve 25.0 g of the material in 125 ml of water. Filter through a weighed and prepared Gooch crucible or sintered glass crucible (G.NO.4) and wash the residue thoroughly with water. Dry the crucible at 110+8 to constant mass.

Calculations: Matter insoluble n water percent by weight = 4A Where A= Weight in g of the residue

(viii)  Determination of Iron (Atomic Absorption Spectrophotometric method)

(a)      Reagents

(1)     Standard Iron solution (1000 ppm)- Weigh accurately 1gm. pure Iron wire and put it in approximately 30 ml of 6 N HCL in a beaker and boil. Transfer it to one litre volumetric flask through the funnel giving several washings to the beaker and funnel with glass distilled water. Make the volume upto the mark. Stopper the flask and shake the solution well. This is 1000 ppm Iron solution.

 

(2)     Glass distilled or demineralised water of pH 2.5 + 0.5.

 

(3)     Preparation of working standards- Pipette 10ml. Iron stock solution in 100ml. volumetric flask and dilute to volume. This is 100ppm Iron solution. Pipette the following volumes of 100 ppm Iron solution in 50ml volumetric flask and make the volume with acidified water.

Stopper the flask and shake the solution well

(b)      Procedure.

(1)     Preparation of fertilizer sample solution - weight exactly 1gm of the material on a clean watch glass and transfer it to a one litre volumetric flask through the funnel giving repeated washings with acidified water and dissolve the material by shaking well. Make the volume upto the mark with acidified water and shake well and filter through Whatman No. 42 filter paper in dry clean flask. The flask should be rinsed with a 10-15 ml. of filtrate and then continue filtration.

(2)     Flamming the solution - Flame the standards and the filtered sample on atomic Absorption Spectrophotometer at a wavelength of 248.3 nm using clean air acetylene flame.

Calculations: Prepare a standard cure of known concentrations of iron solution by plotting the absorbance value on Y - axis against the respective Iron concentration on X - axis. Determine the concentration of Iron in the sample solution from the graph.

Total Iron (as Fe) percent = X

Note : In case a sample has been analyzed by both the methods. Viz. indicated under the heading '7' and '8' the result obtained by the method indicated under the heading '8' shall prevail.

9. Method of analysis of manganese sulphate agricultural grade

(i)       Quality of Reagents Unless specified otherwise, pure chemicals and glass distilled or demineralized water shall be used in tests.

Note: 'Pure chemicals' means chemicals that do not contain impurities which affect the result of analysis. 'Demineralized water' means the water obtained after passing distilled water through a cation and a anion exchange resins or a combined cation-anion exchange resins.

(ii)      Determination of manganese.

(a)      Reagents.

(1)     Standard manganese solution: Weigh 3.0763 g of manganese sulphate (MnSO4H2O A. R. grade) on a clear watch glass and transfer it to one litre flask through the funnel giving several washings to watch glass and funnel with acidified water and make the volume up to the mark. This solution will be 1000 ppm Mn. A secondary dilution of 5 ml to 100ml with acidified water gives a 50 ppm working standard.

 

(2)     Glass distilled or demineralised water of pH 2.5+0.2 Dilute 1 ml of 10 percent sulphuric acid to one litre with glass distilled or demineralised water and adjust the pH to 2.5 with a pH meter using 10% H2SO4 or NaOH. This solution is called acidified.

 

(3)     Preparation of working standards: Pipette the following volume of working standard solution in 50 ml numbered volumetric flasks and make the volume with acidified water.

Stopper the flask and shake them well. Prepare the standard in duplicate. The same acidified water should be used for preparing the solution of unknown fertilizer samples. Fresh standards should be prepared every time when a fresh lot of acidified water is prepared.

(b)      Procedure.

(1)     Preparation of manganese sulphate fertilizer samples: Weigh exactly 0.4 g of the material on the clean watch glass and transfer it to a one litre volumetric flask through the funnel giving repeated washings with acidified water and dissolve the material by shaking well. Make the volume up to the mark with acidified water and shake well.

 

(2)     Take 5ml of the prepared solution in 250 ml volumetric flask and make the volume with acidified water. Shake the solution well and filter through Whatman No. 42 filter paper in dry clean flasks. The flasks should be rinsed with a 10 to 15 ml of the filterate and then continue filtration.

 

(3)     Flaming the solutions: Flame the standards and the filtered samples on atomic absorption spectrophotometer at a wavelength of 279.5m (Mn line of the instrument).

Calculation: Prepare a standard curve of known concentration of manganese solution by plotting the absorbance value on Y- axis against their respective manganese concentrations on X -axis Calculate the percentage manganese in manganese fertilizer by multiplying manganese concentration value calculated from the standard curve by 12.5.

(c)      Precaution.

(1)     Weighing must be done accurately with a precision balance.

 

(2)     All the glass apparatus to be used should be corning/pyrex make and washed with dilute hydrochloric acid (1:4) and washed thoroughly wish distilled and then with demineralised water.

 

(3)     The pipette should be rinsed with the same solution to be measured.

 

(4)     The outside of the pipette should be wiped with filter paper after pipetting the solution to be measured.

 

(5)     After using the pipette. place them on a clear dry filter paper in order to prevent contamination.

 

(6)     To start filtration only a few drops should be added first in order to wet the filter paper and then continue further filteration.

10. Alternative method of analysis of manganese sulphate, agricultural grade.

(i)       Quality of reagents

Unless specified otherwise. Pure chemicals and glass distilled or demineralised water shall be used in tests.

Note: Pure Chemicals' mean chemicals that do not contain impurities which affect the results of analysis.

'Demineralised water' means the water obtained after passing distilled water through a cation and anion exchange resins or a combined cation- anion exchange resin.

(ii)      Determination of manganese.

(a)      Reagents

(1)     Hydrogen peroxide (H2O2)- 30 percent.

 

(2)     Nitric acid (HNO3)- concentrated.

 

(3)     Orthophosphoric acid (H3PO4.from steel industry)- 85 percent.

 

(4)     Potassium periodate (KLO4).

 

(5)     Glass distilled or mineralised water of pH 2.5+0.5- Dilute 1 ml of 10percent H2SO4 to one litre with glass distilled or demineralised water and adjust the pH to 2.5 with a pH meter using 10% H2SO4 or NaOH.

 

(6)     Standard manganese solution- Weigh 3.0763 g of manganese sulphate (Mn SO4.H2O- A.R. grade) on a clear watch glass and transfer it to one litre flask through the funnel giving several washins to the watch glass and the funnel with acidified water and make the volume up to the mark. This solution will be 1000 ppm Mn. A secondary dilution of 5 ml to 100 ml with acidified water gives a 50 ppm working standard.

 

(7)     Preparation of working standard- Pipette 0.0, 0.5, 1.0,1.5, 2.0, 2.5, 3.0, 3.5, 4.0, 4.5 and 5.0 ml of standard solution of manganese in a series of 11 different 100 ml beakers. Evaporate the solutions to dryness at low temperature on a hot plate or steam bath. Add 5 ml of HNO3 and 2ml of 30%H2O2 Cover the beakers with watch glass and digest the contents on a steam bath or hot plate for 30 minutes. Remove the glass cover and evaporate the contents to dryness. Cool the beakers add 2ml of HNO3 5ml of phosphoric acid and heat till boiling. Again cool and mix the contents with 10ml of demineralised water. Add 0.3 g of KIO4 and heat the solutions on water bath until pink colour appears. Add about 20ml water and heat for about 40 minutes or until there is no more increase in colour intensity. Cool the beakers to room temperature. transfer the solutions to 50ml volumetric flasks. Make the volume with deionised water and shake throughly. The concentration of manganese ion will be as follows.

Measure the light transmittance at 540 m (green filter). Make the standard curve by plotting percent transmittance against the concentration of manganese.

(b)      Procedure

(1)     Analysis of manganese sulphate fertilizer sample- weigh exactly 0.500 g of the material on a clean watch glass and transfer it to a one litre volumetric flask through the funnel giving repeated washings with acidified water and dissolve the material by shaking well. Make the volume up to the mark with acidified water and shake well. Pipette one ml solution in a 100ml pyrex/corning beaker and proceed further as described above for preparation of standard curve and make the volume to 50ml. The standard and the test samples should be prepared and processed for estimation at the same time.

Calculation: The percentage of manganese in the manganese sulphate fertilizer sample is calculated by multiplying manganese concentration value calculated from standard curve by 10.

11. Method of analysis of Borax (Sodium Tetraborate decahydrate fertilizer)

(i)       Quality of reagents

Unless specified otherwise, pure chemicals and glass distilled water shall be used in tests.

Note: Pure chemicals means chemicals that do not contain impurities which affect the results of analysis.

(ii)      Determination of Boron.

(A)     Atomic Absorption Spectrophotometer Method.

(a)      Reagents

Standard Boron Solution- Weigh 44.095 g of sodium tetraborate decahydrate (Na2B4O710H2O)- AR grade on clean watch glass and transfer it to one litre volumetric flask through the funnel giving several washings to watch glass and funnel with glass distilled water. Make the volume upto the mark. Stopper the flask and shake the solution well. This is 5000 ppm boron solution herein after called standard A. This solution should be stored in clean bottle for further use.

Preparation of working standards- Pipette the following volume of standard A in 50ml numbered volumetric flasks and make the volume with water.

(b)      Procedure.

(1)     Preparation of sample solution:

Weigh 2.500 g of the material on a clean watch glass & transfer it quantitatively in a 250 ml volumetric flask through the funnel giving repeated washing with water. Make up the volume, stopper the flask & shake well.

(2)     Flamming the solution- Flame the standards & the sample solution on atomic absorption spectrophotometer at a wavelength of 249.8 mn using nitrous oxide acetylene flame.

Calculations: Prepare a standard curve of known concentrations of boron solutions by plotting the absorbance value on Y-axis Calculate the percentage boron in the given sample by multiplying boron concentration value obtained from standard curve by 0.01.

Example

Reading of sample from atomic absorption = Y

Corresponding concentration value of boron from standard curve

against Y absorbance = X ppm

Percentage of boron in the sample = 0.01X

(B)     Titrametric method

(a)      Outline of the method: Borax is determined by first converting it to boric acid with hydrochloric acid and then titrating against Sodium hydroxide solution after complexing boric acid with mannitol or sorbitol.

 

(b)      Reagents:

(1)     Standard hydrochloric acid- 0.5N

 

(2)     Standard sodium hydroxide-1.0N

 

(3)     Methyl red indicator- Dissolve 0.1 g of the material in 60 ml of rectified spirit and dilute with water to 100ml.

 

(4)     Phenolphthalein indicator-

Dissolve 1 g of the material in 100ml of rectified spirit.

(5)     Mannitol or sorbitol.

(c)      Procedure:

(1)     Dissolve 2.0 g of the material. accurately weighed in 60 ml of water & titrate with hydrochloric acid. using methyl red solution as indicator.

(2)     Boil & cool the solution.

(3)     Add 20 g of mannitol or sorbitol and titrate with sodium hydroxide, using phenolphthalein solution as indicator.

Calculation: Boron content, percent by weight =1.0819 V.N. /W

V= Volume in ml of standard sodium hydroxide used.

N= Normality of sodium hydroxide and

W= Weight in g of the material taken for the test

(Ref- ISI- 1109-- 1980)

(iii)     Determination of pH

Same as method No. 8 (vii) (a)

(iv)    Determination of pH

Dissolve 3.8 g of the material in water and make it to 100ml. Measure the pH value of the solution with the help of suitable pH meter, using glass electrodes.

(v)      Determination of lead:

Same as method No. 8 (v) substitute Zinc sulphate by borax

12. Method of analysis of Copper Sulphate Fertilizer (CuSO4.5H2O)

(i)       Quantity of Reagents:

Unless specified otherwise pure chemicals and glass distilled or demineralise water shall be used in tests.

Note: Pure chemicals means chemicals which do not contain impurities which affect the results of analysis.

Demineralised water, means the water obtained after passing distilled water through a cation and anion exchange resin or a combined cation anion exchange resin.

(ii)      Determination of Copper:

(A)     Atomic Absorption Spectrophotometer method:

(a)      Reagents: As specified in 8 (iv) (a)(1)(2) and (3)

 

(b)      Procedure:

(1)     Weigh 0.25 g of the material on a clean watch glass an transfer it to one litre volumetric flask through the funnel giving repeated washing with glass distilled water. Add one ml of 10 percent sulphuric acid and make up the volume.

 

(2)     Take 5ml of the prepared solution in 500ml volumetric flask and make up the volume. Shake the solution well and filter through Whatman. No. 42 filter paper in dry clean flask. The flask should be rinsed with a 10 to 15 ml of the filterate and then continue filtration.

 

(3)     Flamming the solutions: Flame the standards and the filtered samples on an stomic absorption spectrophotometer at a wavelength of 324.8 nm using air acetylene flame.

Calculation : Prepare a standard curve of known concentrations of Copper solution by plotting the absorbance values on Y-axis against their respective concentration values on X -axis

Percent, copper in sample =- 10X / W

Where W= Weight in g of the material taken for test.

X= Conc. of copper (in ppm) as

determined from the graph.

(B)     By lodometric Titration method

(a)      Outline of the method

copper is determined with the addition of potassium iodide and titrating the liberated iodine against standard sodium thio-sulphate solution.

(b)      REAGENT:

(1)     Sodium Carbonate.

 

(2)     Potassium Acid--AR—Crystals

 

(3)     Acetic Acid-----AR GRADE

 

(4)     Standard Sodium thiosulphate solution -O.IN

 

(5)     Starch indicator solution-Triturate 5 g of starch and 0.01 g of mercuric iodide with 30 ml of cold water and boiling water .Boil for three minutes. Allow to cool and decent off the supernatant clear liquid.

 

(6)     Potassium thiocyanate crystals.

(c)      Procedure:

(1)     Dissolve about 1 g of the test sample (accurately weighed) in 50 ml of water.

 

(2)     Add a pinch of sodium carbonate till a slight turbidity appears. Then add 5 ml of acetic acid. 3 g of potassium iodide and titrate the liberated iodine with sodium thiosulphate solution, using starch as an indicator until only a faint blue colour remains.

 

(3)     Add about 2 g of potassium thiocynate shake and continue the titration until the blue colour disappears.

Calculations: Copper percent by mass =-6.35 V.N. / M

Where V= Volume in ml of standard sodium thiosulphate solution.

N= Normality of standard thiosulphate solution and

M= mass in g of the sample taken for the test.

(Ref: IS-261 (1982).

(iii)     Determination of Lead (Pb)

same as method No. 8(v)

Substitute Zinc Sulphate by copper sulphate.

(iv)    Determination of Soluble Iron and Aluminum compounds (expressed as Fe)

(a)      Outline k of the method iron and aluminum are determined gravimetrically by precipitation with ammonium hydroxide.

(b)      Reagents:

1.        Concentrated nitric acid-- AR grade.

 

2.        Ammonium Chloride-- AR grade

 

3.        Dilute Ammonium Hydroxide- approximately 15 percent NH3 (m/v)

 

4.        Dilute Hydrochloric acid-33 percent (m/v)

(c)      Procedure:

(1)     Take 10g of the test sample and add 25 ml of water 2ml of nitric acid and 5 g of ammonium chloride.

 

(2)     Make the solution alkaline by adding ammonium hydroxide solution.

 

(3)     Keep it on a water bath until the precipitate has flocculated, keeping the solution alkaline by the addition of more ammonium hydroxide if necessary.

 

(4)     Filter and wash the residue with dilute ammonium hydroxide.

 

(5)     Dissolve the residue in hot dilute hydrochloric acid.

 

(6)     Make the solution again alkaline by adding ammonium hydroxide and allow the precipitate to settle.

 

(7)     Filter and wash the residue with water.

 

(8)     Dry the residue ignite and weigh till a constant mass is obtained.

Calculation: Solution iron and aluminum compounds

70M1

(as Fe) percent by mass = 70 M1 /M2

Where M1 = Mass in g of the residue obtained and

M2= Mass in g of the sample taken for the test

(Ref: IS: 261-1982)

(v)      Determination of matter insoluble in water Reagents:

(a)      Reagents:

(1)     Concentrated sulphuric acid- AR Grade.

(b)      Procedure:

Weigh accurately about 10 g of the test sample and dissolve in 100ml of water. Add 3 ml of sulphate acid and stir thoroughly at room temperature. Filter through a tared filter paper or tared Gooch or Sintered galas crucible (G. No. 4) Wash the residue with water till it is free from acid. Dry the filter paper or crucible in an oven maintained at a temperature of 105 to 110 C till constant mass is obtained.

Calculation: Insoluble matter, percent by mass = M1 x 100 /M2

Where M1 = Mass in g of the residue obtained for the test

M 2= Mass in g of the material taken for the test.

(vi)    Determination of pH.

(a)      Procedure:

Dissolve 5 g of the test sample in water and make up the volume to 100ml. Determine the pH with glass electrodes using a suitable pH meter.

13. Method of Analysis of Ferrous Sulphate (heptahydrate) FeSO47H2O)

(i)       Quality of Reagents

Unless specified otherwise, pure chemicals & glass distilled or demineralised water shall be used in tests.

Note: Pure Chemicals means chemicals that do not contain impurities which affect the results of analysis. Demineralised water means the water obtained after passing distilled water through a cation & an anion exchange resin or a combined cation-anion exchange resin.

(ii)      Determination of Ferrous Iron.

(a)      Outline of the method-Ferrous iron content is determined by titration with standard potassium permanganate solution.

(b)      Reagents:

1.        Dilute Sulphate acid- 4N approximately

 

2.        Standard Potassium permanganate solution- 0.1 N

 

3.        Orthophosphoric acid.

(c)      Procedure.

1.        Weigh accurately about 5 g of the prepared sample and dissolve it in water.

 

2.        Add 1 to 2 ml of dilute sulphuric acid and make up the solution to 250 ml in a volumetric flask.

 

3.        Pipette out exactly 50 ml of the solution in a flask .

 

4.        Add 10 ml of dilute sulphuric acid and 2 ml of Ortho-phosphoric acid and titrate with standard potassium permanganate solution.

Calculation: Ferrous iron percent by weight = 27.92 V.N./W

Where V= Volume of standard potassium permanganate used

N= Normality of standard potassium permanganate solution.

W= Weight in g of the material taken for the test.

(Ref: IS 262 - 1982)

(iii)     Determination of total iron:

(A)     Titrimetric method using potassium dichromate.

(a)      Outline of the method:

Total iron is determined by reducing ferric iron with stannous chloride and then titrating the total ferrous iron with standard potassium dichromate solution.

(b)      Reagents:

(1)     Concentrated hydrochloric acid.

 

(2)     Stannous chloride solution- Dissolve 6.0 g of stannous chloride crystals (SnCl2.2H2O) in 60 ml of concentrated hydrochloric acid and dilute with water to 100ml. Keep this solution in stopped bottle.

 

(3)     Mercuric chloride solution-saturated

 

(4)     Concentrated sulphuric acid.

 

(5)     Diphenylamine indicator- Dissolve 0.1 g of diphenylamine in 100 ml of concentrated sulphuric acid.

 

(6)     Standard potassium dichromate solution-1.0N

(c)      Procedure :

(1)     Weigh accurately about 5 g of the prepared sample and dissolve it in water.

 

(2)     Add 1 to 2 ml of dilute sulphuric acid and make up the volume to 250 ml in a volumetric flask.

 

(3)     Take 50 ml aliquot of this solution and add 10 ml of concentrated hydrochloric acid and heat to boiling.

 

(4)     Reduce the iron by adding stannous chloride solution until the yellow colour of the ferric chloride disappears. Do not add more than 2 to 3 drops of stannous chloride in excess.

 

(5)     Cool the solution, add rapidly murcuric chloride solution and stir so that a transparent precipitate of mercurous chloride forms slowly, indicting that a slight excess of stannous chloride is present.

 

(6)     Allow to stand for 5 to 10 minutes, dilute to 150 to 200 ml and add 5 ml of phosphoric acid and 5 drops of diphenylamine indicator. Titrate with standard potassium dichromate solution until the colour of the solution changes to a deep blue which does not fade on stirring.

Calculation : Total iron, percent by weight = 27.92 V.N. /W

Where V = Volume in ml of potassium dichromate used in titration.

N = Normality of standard potassium dichromate

solution and

W = Weight in g of the material present in the

aliquot

(Ref. IS: 262-1967)

(B)     Atomic Absorption Spectrophotometer Method :

(a)      Regents :

(1)     Standard Iron solution - ( 1000 ppm ) - weigh accurately 1 g pure iron wire and put it in approximately 30 ml. 6 N HCL, in a beaker and boil. Transfer it to one litre volumetric flask through the funnel giving several washings to the beaker & funnel with glass distilled water. Make the volume up to the mark. Stopper the flask and shake the solution well. This is 1000 ppm iron solution.

 

(2)     Glass distilled or mineralised water of pH 2.5 +0.5.

 

(3)     Preparation of working standards - pipette 10 ml iron stock solution in 100 ml volumetric flask and dilute to volume. This is 100 ppm iron solution.Pipette the following volumes of 100 ppm iron solution in 50 ml numbered volumetric flask and make the volume with acidified water.

Stopper the flask and shake the solution well.

(b)      Procedure :

(1)     Preparation of ferrous sulphate fertilizer sample: Weight exactly 1.000 g of the material on a clean watch glass and transfer it to a one litre volumetric flask through the funnel giving repeated washings with acidified water and dissolve the material by shaking well. Make the volume up to the mark with acidified water and shake well.

 

(2)     Take 5 ml of the prepared solution in 100 ml volumetric flask and make up the volume with acidified water. Shake the solution well and filter through Whatman No.42 filter paper in dry clean flasks. The flasks should be rinsed with a 10 to 15 ml of the filtrate and then continue filtration.

 

(3)     Flamming the solutions - Flame the standards and the filtered sample on atomic absorption spectrophotometer at a Wavelenght of 248.3 nm using clean air-acetylene flame.

Calculation : Prepare a standard Curve of known concentrations of iron solutions by plotting the absorbance value on Y axis against their respective iron concentrations on X axis. Determine the concentration of iron in the sample solution from the graph.

Total iron % = 2 X/W

Where X = Concentration of Fe ( in ppm ) obtained from the standard curve.

W = Weight in g of the material taken for the test.

(iv)    Determination of Ferric iron -

Substract the value of Ferrous iron percent from total iron percent to obtain the Ferric iron percent in the sample.

(Ref. IS : 262-1967)

(v)      Determination of pH -Dissolve 5.0 g of the sample in 100 ml of freshly boiled and cooled water and determine the pH by means of pH meter using glass electrode.

(vi)    Determination of matter insoluble in water -

Same as method No.8 (vii)

(vii)   Determination of Lead -

Same as method No.8 (v), Substitute Zinc sulphate by ferrous sulphate.

14. Method of analysis of ammonium molybdate(NH4)6 Mo7O24.4H2O

(i)       Quality of Reagents -

Unless specified otherwise, pure chemicals and glass distilled or demineralised water shall be used in tests :

Note: ' Pure Chemical' means chemicals that do not contain impurities which affect the results of analysis. 'Demineralised Water' means the water obtained after passing distilled water through a cation and anion exchange resins or a combined cation-anion exchange resin.

(ii)      Determination of Molybdenum :

(A)     Atomic Absorption spectrophotometer method :

(a)      Reagents:

(1)     Potassium Sulphate - Dissolve 25 g of AR Potassium sulphate in 1 litre of distilled water.

(2)     Standard molybdenum solution - weigh 1.5 g of molybdenum trioxide (MoO3) and transfer it to one litre volumetric flask through the funnel giving several washing to beaker and funnel with glass distilled water. Make up the volume upto the mark. This is 1000 ppm standard molybdenum solution.

1.        Preparation of working standards - Pipette the following volume of 1000 ppm standard Mo solution in 100 ml numbered volumetric flasks. Add 20 ml of potassium sulphate solution to each flask and make up the volume to 100 ml. Stopper the flask and shake them well.

(b)      Procedure.

1.        Preparation of Ammonium Molybdate fertilizer sample: Weigh exactly 0.1 g of the material on the clean watch glass and transfer it to a 100 ml volumetric flask through funnel giving repeated washings and dissolve the material by shaking well. Make the volume upto the mark.

2.        Take 10 ml of the prepared solution in a 100 ml volumetric flask, add 20 ml of potassium sulphate solution and make the volume upto the mark.

3.        Flamming the solution : Flame the standards and the filtered samples on an atomic absorption spectrophotometer at a wavelength of 313.3 nm using nitrousoxide-acetylene flame.

Calculation : Prepare a standard curve of known concentration of molybdenum solution by plotting the absorbance value on Y-axis against their respective molybdenum concentration on X-axis.

Percent of Mo = X /10 W

Where X = Concentration of molybdenum (ppm)as obtained from the calibration curve.

W = Weight in g of the material taken for the test.

(B)     Colorimetric Method for Determination of Molybdenum.

(a)      Outline of the Method

Molybdenum (vi) in acid solution when treated with stannous chloride (best in the presence of a little ferrous ion) is onverted largely into molybdenum (v). This forms a complex with thiocyanate ion, probably largely Mo(SCN)5, which is red in colour. The latter may be extracted with solvents possessing donor oxygen atoms (3-Methylbutanol is preferred). The colour depends upon the acid concentration (optimum concentration 1 M) and the concentration of thiocyanate ion (<1.0 percent, but colour intensity is constant in the range 2-10 percent): it is little influenced by excess of stannous chloride. The molybdenum complex has maximum absorption at 465 nm.

(b)      Apparatus

(1)     Photometer - Any suitable photoelectric colorimeter.

(c)      Reagents

(1)     Standard molybdenum solution - (0.001 percent molybdenum)- weigh 0.184 of A.R. Ammonium molybdate (NH4)6.Mo7O24.4H2O on a clean watch glass and transfer it to one litre volumetric flask through the funnel giving several washings to watch glass and funnel with glass distilled water. Make the volume upto the mark. Pipette out 10 ml of this solution into 100 ml volumetric flask and make the volume up to the mark. This gives 0.001 percent Mo solution.

(2)     Ferrous Ammonium Sulphate - Dissolve 10 g of AR ferrous ammonium sulphate salt in 100 ml of very dilute H2SO4.

(3)     Stannous chloride solution - Dissolve 10 g of AR stannous chloride dihydrate in 100 ml of 1M - hydrochloride acid.

(4)     Potassium thiocyanate solution - Dissolve 10 g of AR potassium thiocyanate salt in 100 ml of distilled water.

(5)     Iso-amyl alcohol.

(d)      Preparation of Sample Weigh 0.1 g of sample on a clean watch glass and transfer it to one litre volumetric flask, through the funnel giving several washings to watch glass and funnel with glass distilled water. Make the volume up to the mark. Pipette out 5 ml of this solution into a 100 ml of volumetric flask and make up the volume up to the mark.

(e)      Procedure.

(1)     Place 1.0, 2.0, 3.0, 4.0 and 5.0 ml of the 0.001 percent molybdenum solution (containing 0.01 mg. 0.02 mg, 0.03 mg 0.04 mg and 0.05 mg molybdenum) severally in 50 ml capacity separating funnels and diluting each with an equal volume of water.

 

(2)     Add to each funnel 2.0 ml of conc. HCL, 1.0 ml of ammonium ferrous sulphate and 3.0 ml of the potassium thiocyanate solution.

 

(3)     Shake gently and then introduce 3.0 ml of the stannous chloride solution.

 

(4)     Add water to bring the total volume in each separating funnel to 25 ml and mix.

 

(5)     Pipette 10 ml of redistilled 3-methylbutanol (iso-amyl alcohol) into each funnel and shake individually for 30 seconds.

 

(6)     Allow the phases to separate and carefully run out the lower aqueous layer.

 

(7)     Remove the glass stopper and pour the alcoholic extract through small plug of purified glass wool in a small funnel and collect the organic extract in a 1.0 cm absorption cell.

 

(8)     Measure the absorbance at 465 nm in a spectrophotometer against a 3-methylbutanol blank.

 

(9)     Plot absorbance against concentration of standard molybdenum solutions and draw the calibration curve.

 

(10)   Take 10 ml of the sample solution and determine the absorbance of it by subjecting it to the same treatment as the standard solutions, using calibration curve, determine the corresponding concentration of molybdenum in the sample solution.

Calculation: % Mo = 2000.W /. Y.W.

Where X = Concentration of molybdenum (in mg ) of

the test solution.

Y = Volume of sample solution taken for the

test.

W = Wt in g of the material taken for the

preparation of the sample solution.

(Ref. : Vogal's Text Book of Quantitative analysis).

(iii)     Determination of matter insoluble in water

(a)      Procedure

Dissolve 25.0 g of the material in 125 ml of water. Filter through a weighed and prepared Gooch crucible or sintered glass crucible (G.No.4) and wash the residue thoroughly with water. Dry the crucible at 110 degree + 8 degree to constant mass.

(b)      Calculation :

Matter insoluble in water percent by weight = 4A

Where A = Weight in g of the residue.

(iv)    Determination of lead

Same as per method No.8(v). Substitute zinc sulphate by ammonium molybdate.

15. Method of Analysis of Chelated Zinc (As Zn-EDTA)

(i)       Reagents.

(a)      EDTA Solution - (0.05M) Dissolve 18.612 g of disodium

ethylene diamine tetra acetate dihydrate (EDTA) in

distilled water & make up the volume to 1 litre.

(b)      Standard Zinc solution (1000 ppm) - Weigh accurately

1.0 g of zinc metal in a beaker. Add 20 ml HCL (1:1).

Keep it for few hours and allow it to dissolve

completely. Transfer the solution to 1 litre

volumetric flask. Make the volume upto the mark.

(c)      Concentrated Ammonia solution (sp.gr.0.88)

(d)      Ammonium Nitrate - AR grade salt.

(e)      Buffer solution (pH-10) - Dissolve 8.0 g AR grade

ammonium nitrate in 65 ml of water and add 35 ml of

concentrated ammonia solution (sp.gr.-0.88)

(f)       Eriochrome black (T) indicator mixture - mix

thoroughly 1 gm of eriochrome Black (T) indicator with

100 gm of AR grade potassium nitrate.

(g)      Hydroxylamine hydrochloride - AR grade.

(h)     Potassium cyanide - AR grade (to be used with extreme

care) 15% aq. solution.

(i)       Manganese sulphate solution - Dissolve 11.15 g of AR

grade manganese sulphate in 1 litre of distilled water.

(j)       Sodium Fluoride AR grade.

(ii)      Preparation of Sample solution.

Weigh accurately 1.0 g of the sample and transfer it to 100 ml volumetric flask. Make up the volume with distilled water. Keep it overnight.

(iii)     Procedure

(a)      Standardization of EDTA solution

(1)     Take 10 ml of zinc solution (standard)

 

(2)     Dilute it by adding 30 ml distilled water.

 

(3)     Add 10 ml of buffer solution and 30-40 mg of indicator mixture.

 

(4)     Titrate with EDTA solution till clear blue end point is obtained. Note the volume of EDTA used s V1 ml.

(b)      Standardisation of Manganese sulphate solution.

(1)     Take 25 ml of manganese sulphate solution.

 

(2)     Dilute it by adding 100 ml distilled water.

 

(3)     Add 0.25 g of dydroxylamine hydrochloride and 10 ml of buffer solution.

 

(4)     Add 30-40 mg of indicator mixture.

 

(5)     Titrate with EDTA solution till clear blue end point is obtained. Note the volume of EDTA used as V2 ml.

(c)      Determination of EDTA content of Zn-EDTA fertilizer

(1)     Take 10 ml of sample of distilled water.

 

(2)     Dilute it by adding 100 ml of distilled water.

 

(3)     Add 0.25 g of hydroxylamine hydrochloride.

 

(4)     Add 10 ml of buffer solution and 30-40 mg of indicator mixture.

 

(5)     Warm to 40 deg.C. and titrate with standard EDTA solution (preferably stirring magnetically) to clear blue end point.

Note the volume of EDTA used as V3 ml.

(6)     After the end point, add 2.5 g of solution fluoride and stir for one minute.

(7)     Titrate the solution with standard mangenese sulphate solution, slowly, till a permanent red colour is obtained. Note the volume of manganese sulphate added as V4 ml.

(8)     Stir for 1 minute.

(9)     Titrate the excess of manganese ions with EDTA solution until the colour changes to pure blue.

Note the volume of EDTA used as V5 ml.

(10)   After the second end point (step 9) add 4-5 ml of 15% aqueous potassium cyanide solution.

(11)   Titrate it with manganese sulphate solution till colour changes sharply from blue to red.

Note:- The volume of manganese sulphate solution added as V6 ml.

Calculation: Molarity of EDTA solution (M1) =

Molarity of standard zinc solution x volume of

standard zinc solution taken.

Volume of standard manganese sulphate solution taken

Nos of millimoles of EDTA used in titrating Zn + other metals (A) = M1V3

No of millimoles of EDTA liberatedby sodium fluoride (B) = M2V4 - M1V5

Hence Nos of millimoles of EDTA used for titratingzinc (C) = A - B

But nos of millimoles of EDTA liberated by KCN (D) = M2V6

Hence no of millimoles of EDTA contained by Zn-EDTA sample = D - C

EDTA percent = 24.31 x B

Percent of free zinc = 65.38 x C

Percent of Zinc chelated with EDTA = 65.38 (D - C)

(Ref. Vogal's Text Book of Quantitive Inorganic Analysis).

16. Method of Analysis of Chelated Iron (As Fe-EDTA)

(i)       Quantity of reagents

Unless specified otherwise, pure chemicals and glass distilled or demineralised water shall be used in tests.

Note:- 'Pure Chemicals' means chemicals that do not contain impurities which affect the result of analysis. 'Demineralized Water' means the water obtained after passing distilled water through a cation and an anion exchange resins or a combined cation-anion exchange resin.

(ii)      Determination of chelated iron

(a)      Reagents.

(1)     Sodium hydroxide solution - 0.5N, Dissolve 20 g NaOH in water and dilute to 1 litre.

 

(2)     Disodium EDTA solution = 0.66%. Dissolve 0.73 g of Na2H2 EDTA 2H2O in water and dilute to 100 ml.

 

(3)     Iron standard solution -

(A)     Stock solution - (1000 ppm) Dissolve 1.000 g pure Fe wire in approximately 30 ml 6 N HCL withboiling. Dilute to 1 litre in a volumetric flask with distilled water.

 

(B)     Intermediate solution - (100 ppm). Pipette 10 ml iron stock solution and 10 ml Na2H2 EDTA solution in 100 ml volumetric flask and dilute to volume.

 

(C)     Working solution - Pipette the following volumes of 100 ppm intermediate solution in 50 ml numbered volumetric flask and make the volume with 0.5 N HCl.

(b)      Apparatus

Atomic Absorption Spectrophotometer with air/acetylene flame.

(c)      Procedure

(1)     Preparation of sample solution :

(A)     Weigh sample containing approximately 40 mg Fe into 200 ml tall form beaker.

 

(B)     Wet with 2-3 drops of alcohol and dissolve in 100 ml of water.

 

(C)     Add 4 drops of 30% H2O2, mix and adjust pH of solution to 8.5 with 0.5 N NaOH. If pH drifts above 8.8, discard solution and repeat analysis.

 

(D)     Transfer solution to 200 ml volumetric flask, dilute to volume with water and mix.

 

(E)     Filter solution through quantitative paper.

 

(F)      Pipette 10 ml filtrate into 200 ml volumetric flask and dilute to volume with 0.5 N HCl.

(2)     Flaming the Solution

Flame the standard and the sample solution on atomic absorption spectrophotometer at a wavelength of 248.3 nm using air acetylene flame. In same manner determine Fe blank on all reagents used.

Calculation:- Prepare a standard curve of known concentration of Fe solution by plotting the absorbance value on Y axis against their respective Fe concentrations on X axis.

Chelated Iron % = ( ppm Fe in sample---- ppm Fe in blank) x 0.4 / g sample

( Ref. Method of Analysis AOAC, 1984)

(iii)     Determination of pH

As per method No. 8(vi) (a)

17. Determination of Sodium in Potassium Chloride and Potassium Sulphate by Atomic Absorption Spectro-photometric method.

(i)       Quantity of Reagents - Unless Specified otherwise, pure chemicals and glass distilled or demineralised water shall be used in tests.

(ii)      Reagents.

(1)     Ammonium Oxalate Solution - Dissolve 40 g of Ammonium Oxalate in 1 litre of distilled water.

 

(2)     Standard Sodium Solution - (1000 ppm) - Weigh accurately 2.5421 g of dried NaCl on a clean watch glass and transfer it to one litre volumetric flask. Make up the volume upto the mark. Stopper the flask and shake the solution well. This is 1000 ppm sodium solution.

 

(3)     Preparation of working standard - Pipette the following volumes of 1000 ppm standard sodium solution in 100 ml volumetric flask and make up the volume with glass distilled water.

Stopper the flask and shake the solution well

(iii)     Procedure.

(1)     Preparation of sample solution - weigh exactly 2.5 grams sample on a clean watch glass and transfer it to 250 ml volumetric flask through the funnel giving repeated washings with glass distilled water (about 125 ml. of water should be used). Add 50 ml of Ammonium Oxalate solution. Boil for 30 minutes, cool, dilute to volume, mix and pass through dry filter paper (Whatman No.1 of equivalent).

(2)     Flaming the solution - Flame the standard and the filtered sample on Atomic Absorption Spectro-photometer at a wavelength of 330.3 nm using clean air acetylene flame.

Calculations : Prepare a standard curve of known concentrations of Sodium solution by plotting the absorbance value on Y-axis against their respective sodium concentration on X-axis. Determine the concentration of sodium in the sample solution from the graph. Sodium (Na) as Sodium Chloride % = 0.0254 X, where X is the concentration of Sodium in ppm obtained from the standard curve. (Ref. : AOAC, 1984)

18 Determination of Total Chlorides in Potassium Sulphate by Silver Nitrate Volumetric Method.

(i)       Reagents.

(1)     Standard Silver Nitrate (AgNO3) solution - 0.1 N

(2)     Potassium Chromate (K2CrO4) Indicator solution - 5 percent.

(ii)      Procedure

(1)     Weigh accurately about 10 gms of the prepared sample and transfer into 500 ml beaker.

 

(2)     Add about 250 ml of water and warm gently for about 20 minutes.

 

(3)     Cool and dilute the solution to 500 ml in a volumetric flask

 

(4)     Allow to stand to let any insoluble matter settle.

 

(5)     Transfer with a pipette 100 ml of the clear solution into a conical flask.

 

(6)     Titrate with standard AgNO3 solution (0.1 N) using 1 ml of Potassium Chromate Indicator solution.

Calculation : Total Chlorides ( as Cl ), percent by

Weight ( on dry basis ) = 17.73 N V / W

Where, N = Normality of standard AgNo3 solution.

19. Methods of Analysis of Magnesium Sulphate

(i)       Quality of Reagents.

Unless specified otherwise, pure chemicals and glass distilled or demineralised water shall be used in testa.

(ii)      Determination of Magnesium.

(A)     Atomic Absorption Spectrophotometer method

(a)      Reagents.

(1)     Hydrochloric Acid 0.5 N.

 

(2)     Magnesium Standard Solution : Dissolve 1.013 g Magnesium Sulphate (MgSO47H2O) in 0.5 N hydrochloric acid solution and dilute to 100 ml with this acid in a volumetric flask. This is 1000 ppm magnesium stock solution.

 

(3)     Strontium Chloride Solution : Dissolve 15 g strontium chloride (SrCl26H2O) in 0.5 N hydrochloric acid and dilute to 100 ml with the same solvent.

(b)      Preparation of working standards.

(1)     Pipette 8.1 ml of 1000 ppm magnesium stock solution to 100 ml capacity volumetric flask and make up the volume with 0.5 N hydrochloric acid. This is 10 ppm Magnesium Solution.

(2)     Pipette the following volume of 10 ppm magnesium solution in 100 ml numbered volumetric flask. Add 10 ml of strontium chloride solution to each flask and make up the volume to 100 ml with 0.5 N hydrochloric acid.

(c)      Procedure.

(1)     Preparation of sample solution.

(A)     Weight 1 g of the sample and place in a 500 ml volumetric flask. Add about 300 ml water and boil for 30 minutes. Allow to cool, dilute to the mark with water, mix and filter.

 

(B)     Pipette 5 ml of the filtrate (A) into a 100 ml volumetric flask, make up to the mark with water and mix.

 

(C)     Transfer by pipette 5 ml of the diluted filtrate (B) into 100 ml volumetric flask and make up to the mark with 0.5 N HCl.

(2)     Blank solution : Prepare a blank solution from which only the sample has been omitted.

(3)     Flaming of solution : Flame the standard and sample solutions on Atomic Absorption Spectrophotometer at wavelength of 205.2 nm using Air Acetylene flame.

Calculations: Plot the calibration curve using the mean absorbances on Y-axis and the corresponding concentrations of Magnesium (ppm) on X-axis. Determine the concentration of Magnesium in the sample by reference to the calibration curve.

Magnesium percent = 20X

Where X = concentration of Magnesium (in ppm) obtained from the standard curve.

(B)     Titrametric method (EDTA Titrations)

(Applicable to the samples which do not contain phosphate as impurity)

(a)      Reagents

(1)     Buffer solution (pH-10.0) - Dissolve 67.5 g ammonium chloride in 200 ml of distilled water, add 570 ml ammonia solution and dilute to 1 litre.

 

(2)     Potassium hydroxide - Potassium cyanide solution - Dissolve 280 g potassium hydroxide and 66 g potassium cyanide in 1 litre of distilled water.

 

(3)     Potassium cyanide solution (2%) - Dissolve 2 g potassium cyanide in 100 ml of distilled water.

 

(4)     Eriochrome black T indicator solution - Dissolve 0.2 g of indicator in 50 ml of methyl alcohol containing 2 g of hydroxylamine hydrochloride.

 

(5)     Calcium standard solution (1 mg/ml) - Dissolve 2.4973 g calcium carbonate, primary standard grade, previously dried for 2 hours at 2850. in HCl (1+10). Dilute to 1 litre with distilled water.

 

(6)     Calcein indicator mixture - Grind together 1 g calcein indicator (2',7'-bis(bis(Carboxymethyl,) amino)methyl-) fluorescein, sodium derivative sodium salt), 10 g charcoal 100 g potassium chloride.

 

(7)     Disodium dihydrogen ethylene diamine tetra acetic acid standard solution (0.4% - Dissolve 4 g Na2H2-EDTA in 1 litre of distilled water.

 

(8)     Triethanolamine (1 + 1)

 

(9)     Potassium ferrocyanide solution (4%) - Dissolve 4 g potassium ferrocyanide in 100 ml of distilled water.

(b)      Standardization of Calcium Solution :

(1)     Pipette 10 ml calcium standard solution into 250 ml erlenamayer flask.

 

(2)     Add 100 ml of distilled water, 10 ml KOH-KCN solution, 2 drops of triethanolamine solution, 5 drops of potassium ferrocyanide solution and 15+1 mg of calcein indicator.

 

(3)     Immediately place the flask on a magnetic stirrer in front of daylight fluorescent light with transparent background.

 

(4)     While stirring, titrate with EDTA solution to disappearence of all fluorescent green and until solution remains pink. Titrate more than 3 aliquots. From average, calculate calcium titer value.

Calcium Titer (mg/ml) = Volume of calcium standard  (ml) / Volume of EDTA solution used (ml)

From calcium titer, calculate magnesium titer value as follows :

Magnesium titer = Calcium titer x 0.6064

(c)      Preparation of sample solution

(1)     Weight 1 g magnesium sulphate fertilizer sample into 250 ml volumetric flask.

 

(2)     Add 200 ml of distilled water and boil for 30 minutes.

 

(3)     Cool dilute to volume with water and mix.

(d)      Procedure.

(1)     Titration for Ca + Mg

(A)     Pipette 25 ml of aliquot in 250 ml erlenmayer flask.

 

(B)     Dilute with 100 ml of distilled water.

 

(C)     Add 5 ml of buffer solution (pH 10), 2ml potassium cyanide solution, 2 drops of triethapolamine solution, 5 drops of potassium ferrocyanide solution and 8 drops of eriochrome black T indicator solution.

 

(D)     Titrate immediately with EDTA solution, stirring and lighting as in standardisation. Colour changes are wine, red, purple, dark blue, to clear blue end point, becoming green if over titrated.

Note:- The volume of EDTA used as V1 ml.

(2)     Titration for Calcium.

(A)     Pipette 25 ml of aliquot in 250 ml erlenmayer flask.

 

(B)     Dilute with 100 ml of water.

 

(C)     Add 10 ml KOH-KCN solution, 2 drops of triethanolamine solution, 5 drops of potassium ferrocyanide solution and 15+ mg. of calcein indicator.

 

(D)     Titrate immediately with EDTA solution in Standardisation.

Note:- The volume of EDTA used as V2 ml.

Calculation:- Magnesium percent = (V1-V2) x MKg Titer EDTA

(Reference : AOAC, 14th edition, 1984)

20. Determination of Particle size in different Fertilizers

(i)       Apparatus :

(A)     Indian Standard of 20 cms. diameter and 5 cms in height with lid and bottom pan of required sizes.

 

(B)     Sieve shaker or vibrator with automatic timer and variable cycle control.

 

(C)     Balance, top leading with suitable capacity and sensitivity of 0.1 gm.

 

(D)     Weighing pan round suitable for holding sample and approximately 23 cms in diameter.

 

(E)     Brush either soft, fine wire or stiff.

(ii)      Procedure :

(A)     Take the sieve of required sizes and stack them in progressive order. The biggest sieve size should be on the top and the smallest in the bottom. Place the empty pan at the bottom.

 

(B)     Put 200 gms of ungrinded sample on the top sieve and place lid on the top of the stack.

 

(C)     Position and secure sieve stack in shaking apparatus.

 

(D)     Start shaking action for 5 minutes. If automatic timer is used, set timer for 5 minutes. If vibrator is used, also set vibrator control at 3000 cycle per minute.

Note:- If mechanical sieve shaker is not available, use hand sieving. Conduct sieving by appropriate lateral and vertical motions accompanied by jarring action. Continue until no appreciable change is noted in sieve fractions.

(E)     After completion of shaking time, transfer material from each sieve to weighing pan with brush and weight to +/- 0.1 gm.

(F)      Record weight from each sieve (sum of weights from each sieve should agree closely with original sample weight)

Calculations:- Percent weight on sieve = Weight on sieve (gm) /Total weight of sample (gm)

21. Method Of Analysis of Calcium nitrate

(i)       Determination of total nitrogen

By the as specified in 3 (viii)

(ii)      Determination of Ammonical Nitrogen

By the method as specified in 3 (vii)

(iii)     Determination of nitrate

By the method as specified in 3(viii) & vii)

(iv)    Determination of water insoluble matter

By the method of specified in 8(vii)

(v)      Determination of water soluble calcium.

A.        Titrimetric method (EDTA) Titrations.

(a)      Reagents.

(i)       Buffer solution (pH-12.0) - Dissolve 225 gm KOH (AR) in 250 ml water. Add 15 ml triethanolamite and make volume to one litre after cooling the solution.

 

(ii)      Pattan and Reeder's indicator 0.2 gm indicator in 100ml methanol.

 

(iii)     calcium standard solution (mg/ml). - Dissolve 2.4973g calcium carbonate, primary standard grade, previously dried for 2 hours at 2850 c, in Hcl (1 + 10). Dilute to 1 litre with distilled water.

 

(iv)    Disodium dihydrogent ethylene diamine tetra acetic standard solution (0.01 m) - Dissolve 3.7224 gm Na₂H₂-EDTA(AR) previously dried at 105 to 110° c for 1 hr in distilled water and make volume to one litre.

(b)      standardisation of calcium Solution

(i)       Pipette 10m1 calcium standard solution into 250 ml erleninayer flask.

 

(ii)      Add 10-15 ml distilled water and 20 ml Duffer solution [153][in case of Potassium Magnesium Calcium Sulphate add 50 ml distilled water and 20 ml buffer solution].

 

(iii)     Add few drops of indicator's solution. A red rose colour will appear.

 

(iv)    Titrate with EDTA till a blue colour is obtained. Note the volume of EDTA used as V₁ ml Calcium Titer (mg/m1) = Volume of Calcium standard solution (m1)/Volume of EDTA solution use (m1) (v1)

(c)      preparation of sample solution..

(i) weigh 2.5 g calcium nitrate fertiliser sample into 250 Volumetric Flask

(ii) make up the volume with distilled water. shake well.

[154][(iii) In case of Potassium Magnesium Calcium Sulphate "weighed 2.5 gm of fresh sample in 250 ml volumetric flask and add 5 ml concentrated HCl, make up the volume and shake well;]

(d)      Procedure.

(i)       pipette 5 ml of aliquot in 250 ml erlenmayer flask.

 

(ii)      Add 10-15 ml distilled water & 20 ml Buffer solution.

 

(iii)     Add few drops of indicator's solution. A red rose colour will appear.

 

(iv)    Titrate with EDTA till a blue colour is obtained. 

Note the volume of EDTA used as v2 ml

calculation

Calcium per cent = V2 x Calcium Titer x 2

B.        Atomic Absorption spectrophotometric method-

(1)     Reagent:

Unless specified otherwise pure chemicals and Glass distilled or demineralised water shall be used in test.

(a)      Hydrochloric Acid r= 3 N

(b)      preparation of stock solution:-

(i)       Calcium stock solution - Dissolve 2.498 gram CaCO₃ in a minimum amount of 3 N Hcl . Dilute to 1 litre (1000 ppm Ca). Dilute 10 ml to 100 ml. This is 100 ppm stock solution.

(ii)      Lanthanum stock solution:- 50 g La/L.

Dissolve 58.65 gram La₂O₃ in 250 ml Hcl, adding acid slowly. Dilute to 1 litre.

(c)      Preparation of working standard: 

Add 0, 5, 10, 15 and 20 ml of ca stock solution in a 100 ml volumetric flask. Add 20 ml La stock solution and make up the volume to 100 ml with distilled water, This will correspond to 0, 5, 10, 15, and 20 Mg Ca/m1 containing 1% La.

(2)     procedures:

weigh 1.00 gram well grind sample in a 100 ml volumeric flask. Add 25 ml water and shake to dissolve. Then add 20 Lanthanum solution in the flask and make volume to 100 ml with Distilled water. shake well and allow to settle. Filter, if required, before it is aspirated.

(3)     Flaming of the solution:- Flame the standard and sample solution on AAS at wave length of 422.7 nm using Air - Acetylene flame.

(4)     Calculation ;- plot the calibration curve using the mean absorbance on Y axis and the corresponding concentration of ca (ug/m1) at 'X'' axis. Determine the concentration of calcium in the sample by reference to the calibration curve:

% Ca = Concentration (ug/ml) x 10-2

22. Analysis of Micronutrient Fertilisers Mixtures by Atomic Absorption Spectro photometric Method-

(a)      Reagents :

(1)     Acidified water : Dissolve 10 ml of 10% Sulphuric Acid in 10 litre of double distilled water and adjust the pH to 2.5 ( ±0.5) with help of a pH meter using H₂SO₄ or NaOH.

 

(2)     Strontium Chloride Solution : Dissolve 7.5 g of Strontium Chloride (SrC12.6H20) in one litre of distilled water.

 

(3)     Potassium Sulphate Solution : Dissolve 25 gm of AR Potassium Sulphate in one litre of distilled water.

(b)      Procedure:

(i)       Preparation of standard stock solution :

Dissolve the specific quantity of standard material for specific element with the help of suitable solvent as indicated below and make up the volume 1000 ml with distilled water. Further dilute it to suitable flaming range with acidified water in case of Fe, Cu, Mn and Zn. In case of Mg, add 20 ml of Strontium Chloride and in case of Mo, add 20 ml of Potassium Sulphate before make up the volume up to the mark, in 100 ml volumetric flask with acidified water.

(ii)      Preparation of sample solution -

Weigh 1 gm micronutrient fertilizer mixture (Solid or liquid) transfer to 100 ml volumetric flask with the help of acidified water and make up the volume up to the mark. Shake well and keep it stand for at least 4-6 ;hours. Dilute it further to suitable standard working range with acidified water in case of Fe, Cu Mn and Zn. In case of Mg, add 20 ml of Strontium Chloride and in case of Mo, add 20 nil of Potassium Sulphate before making up the volume up to the mark, in 100 ml volumetric flask with acidified water.

(iii)     Flaming of Solutions :

Flame the standard solution of specific element at concentration mode. Then flame the sample solution to observe the concentration (in ppm). of specified element.

Calculation : % Concentration = X x Dilution Factor x 10-4

(X = Concentration in ppm observed by instrument)

23. Determination of Boron in Micronutrient Fertiliser Mixture-Volumetric Method-

(a)      Reagents-

(1)     Mannitol

 

(2)     Bismuth Nitrate Solution : Dissolve 22 gm of Bismuth Nittate [(BiNO3)3 5 H2O] in 8 ml of conch Nitric Acid Warm slightly and dilute to 100 ml with distilled water.

 

(3)     Nitric Acid :- Concentrated AR Grade.

 

(4)     Dilute Nitric Acid :- (1:20)

 

(5)     Sodium Hydroxide Solution :- 109% M/V

 

(6)     Sodium Hydroxide Solution - 0.02 M

 

(7)     Bromothymol Blue Indicator Solutions.

(b)      Procedure :

(1)     Weigh accurately 2.5 gm of prepared sample in to 250 ml beaker.

 

(2)     Add 2 ml of conc. Nitric Acid and 50 ml of water and warm gently and dilute to 100 ml with water.

 

(3)     Warm the solution (but do not boil).

 

(4)     Slowly add 5 ml of Bismuth Nitrate Solution for each 1% of P205 percent in the sample, from a burette with continuous stiffing and maintaining. the liquid hot during addition.

 

(5)     Cool and transfer the contents in to 250 ml volumetric flask and dilute up to the mark with distilled water.

 

(6)     Allow precipitate to settle and dilute up to the mark with distilled Water.

 

(7)     Filter through a dry filter paper (No. 40) rejecting the first few drops in to a beaker.

 

(8)     Pipette 100 ml of the filtrate in 250 ml beaker, add a few drops of indicator solution.

 

(9)     Add few drops of 10% NaOH solution with thorough stirring until the indicator turns blue.

 

(10)   Filter through a dry filter paper (No. 40) into 250 ml beaker and carefully wash the residue several times with cold water. The total volume should be 150 to 200 ml.

 

(11)   Adjust the pH to about 5 by adding diluted HNO₃ . Warm to about 90°C (do. not boil), and stir vigorously to avoid CO2. Cool the solution.

 

(12)   Place in the "solution, the electrodes of pH meter and adjust the pH to exactly 6.3 using NaOH solution.

 

(13)   Add 10 gm of mannitol and again adjust pH to exactly 6.3 with 0.02 N NaOH solution.

 

(14)   Continue adding mannitol in 10 gm portion till pH remains constant at 6.3. Note the total volume of 0.02 N NaOH used for the addition of Mannitol (Step 13).

 

(15)   Carry out a blank determination on fertilizers mixture to which Borate is not added.

(c)      Calculation :

% B = (A-B) x 0.05405/W

Where : A = Volume of 0.02 N NaOH solution used in the sample. 

B = Volume of 0.02 N NaOH solution used in the blank.

Note : In case phosphate is not present in the sample, proceed as follows:-

(i)       Take 2.5 gm of the sample in 250 ml volumetric flask and make up the volume with distilled water.

proceed as given from step (8) onwards.

24. Determination of total sulphur

(The total sulphur includes sum of sulphur present in Sulphate and elemental form).

(A)     Determination of Sulphate Sulphur

Method of determination of sulphur present in the sulphate form in various fertilizers for nitrate free and nitrate containing samples is given below:

Classification of procedures-

Procedure (a) : For nitrate free samples such as ammonium sulphate, potassium sulphate, zinc sulphate , copper sulphate, ferrous sulphate, manganese sulphate , N.P. and NPK complexes and mixtures, 

Procedure (b): Super phosphate

Procedure (c) : For nitrate containing fertilizers such as ammonium phosphate sulphate nitrate 20 :20 :0

(i)       Quality of Reagents-

Unless specified otherwise, pure chemicals, glass, distilled or demineralised water shall he used in tests.

Note :- (1) " pure chemicals" means chemicals which do not contain impurities which affect the results of analysis.

(2) " demineralised water" means water obtained by water passing through a cation and anion exchange resins er a combined cation-anion exchange resins.

(ii)      Reagents-

(1)     Hydrochloric acid-concentrated

 

(2)     Dilute hydrochloric acid - Dilute 250 ml. of concentrated hydrochloric acid to 1000 ml, of water.

 

(3)     Barium chloride solution - 2 percent . Dissolve 20 g of barium chloride in 1000 ml of water.

 

(4)     Silver nitrate solution - 5 percent . Dissolve 5 g silver nitrate in 100 ml water.

(iii)     Procedure (a)-

(1)     Weigh about 2.5 g of sample and transfer to 250 ml capacity volumetric flask with the help of dilute hydrochloric acid.

 

(2)     Make up the volume with dilute hydrochloric acid.

 

(3)     Apply stopper, shake well and filter through Whatman Filter paper No.40 or equivalent part in a dry beaker if the solution is not clear and transparent.

 

(4)     Take 25 ml of the filtered aliquot in a beaker of 250 ml capacity. Add 100 ml of water and heat to boil. While stirring add in a slow stream.1 ml of hot barium Chloride solution for each one percent. Sulphur expected in sample plus additional 10 ml in excess to ensure complete precipitation of sulphur as barium sulphate. Boil for a minute.

 

(5)     Digest the precipitate on a hot plate or water bath for 2 hours at low temperature such that the solution does not boil. Ensure the supernatent liquid to be clear and transparent. Cool to room temperature. Filter into a 30 ml capacity G 4 grade - sintered Gooch crucible previously dried at. 250° C cooled and weighed. - Wash the precipitate 10-12 times with hot water to ensure the precipitate to make it free from barium chloride. The filtrate may be tested with silver nitrate solution to confirm that the precipitate is free from chloride.

 

(6)     Dry the crucible and its content to 250 C for two hours in a furnace by raising the temperature of the furnace slowly from room temperature: After drying, cool to room temperature in a desiccator to a constant weight taken.

Calculations: Sulphate Sulphur (as S) per cent by weight - 137.4 x M

Where M = weight of precipitate

W weight of the sample taken.

Procedure (b): Weigh about 2.5 g of sample and transfer to a beaker of 250 ml capacity. Add 25 ml of concentrated hydrochloric acid and 25 ml of water. Heat to boil the solution gently. Boil for 5 minutes and cool. Add 75 ml of water and transfer quantitatively into a volumetric flask of capacity 250 ml with dilute hydrochloric acid solution and make up the volume. Apply stopper, shake well and filter about 50 ml or prepared solution through Whatman filter paper No.40 or equivalent and proceed as at step (2) of Procedure (a) onward.

Procedure (c): (1) Weigh about 2.5 g of sample and transfer to a beaker of 250 ml capacity. Add 10 ml of concentrated hydrochloric acid and grind the sample with the help of a glass rod. Evaporate to dryness on a hot plate Soak the mass again with few drops of concentrated hydrochloric acid and evaporate to dryness.

(2) Add 100 ml of dilute hydrochloric acid, heat to boil and cool to room temperature. Transfer the content to a 250 ml volumetric flask. Filter a portion of the solution through a Whatman No.40 filter paper or equivalent and proceed as at step (2) of Procedure (a) onwards. 

Note: Based on AOAC 1995.

(B)     Determination of elemental Sulphur

(a)      Reagents.

(1)     Hydrochloric Acid- concentrated(4 N)

 

(2)     Sulphur powder (AR Grade)

 

(3)     Acetone saturated with sulphur- Add 2-3 g of sulphur powder in 250 ml of acetone in stoppered bottle. Shake well and allow it to stand for 1 hour. Filter through whatman filter paper No.42 & collect , filtrate in a stoppered glass bottle.

 

(4)     Carbon di sulphide (AR Grade)

(b)      Procedure.

Take 1 g of prepared sample in a beaker. Add 50 ml of 4 N 1-ICI boil for 5 minutes. Cool and filter through a sintered glass crucible (G 4). Wash thoroughly with distilled water. Wash the residue 5-6 times with 10 ml portion of Acetone saturated with sulphur. Dry at 100°C for 1 hour. Cool in a desiccator and take weight of the crucible. Let the weight be W.

After taking the weight of the crucible (WO wash the crucible 8-10 times with 10 ml portion of carbon disulphide thoroughly under slow suction. Dry the crucible at 100° C for 1 hour. Cool in a desicator and weigh. Let this weight be W2.

Calculation:- Elemental sulphur as (S) % by weight = (W₁- W₂) X 100/W

Where "W" is the weight of the sample taken

(C)     Total sulphur(as 5) per cent by weight = Sulphate sulphur (as per procedure 24)+ elemental Sulphur (as per procedure 24 A).

26. Method of analysis of Zincated Oxide (suspension) :-

[155][(i) Determination of total zinc

Scope: Total extraction of Zinc (Zn), Arsenic (As), Lead (Pb) and Cadmium (Cd) from Zinc Oxide Suspension Concentrate.

Principle: Zinc and heavy metal impurities are extracted from the sample with boiling Aqua Regia.

(a)      Sample preparation:

The details of the procedure for drawl of samples of fertilizers have been provided in Schedule II Part A, Serial No. 9 (Method for sampling of liquid fertilizers (other than anhydrous ammonia), however importance of proper shaking and mixing of contents before withdrawal of sample and before drawing aliquot for analysis is particularly emphasized. Since in suspension formulation insoluble materials might settle down over time, thorough mixing of contents would ensure representative composition along the entire depth of the container.

(b)      Reagents:

All the reagents should be of analytical grade to ensure negligible concentration of the elements to be determined.

(1)     Glass double distilled water (free from micronutrients)

(2)     Hydrochloric acid 37% HCI ((HCI) = 12 mol/l, p = 1.18 g/ml)

(3)     Nitric acid 65% HNO₃   {c(HNO3) = 14.3 mol/l, p = 1.4 g/ml}

(c)      Appartatus:

Apparatus for thermal heating digestion-with reaction vessel and reflux condenser.

The vessel should be at least 5 times the volume of the aqua regia used.

In case reaction vessel with reflux condenser is not available, Erlenmeyer flask or high beakers covered with watch glass can be used for the purpose.

Ash free filter paper is required if filtration is necessary.

(d)      Procedure:

(1)     Weight one gram (1 ± 0.001 g) of the sample and transfer quantitatively to the reaction vessel.

 

(2)     Moisten the sample with about 0.5 to 1.0 ml distilled water

 

(3)     Mix the contents well and 21 ml of HCL) followed by 7 ml of HNO3 (reagent both drop wise to reduce foaming.

 

(4)     Connect the condenser to the reaction vessel and let the mixture stand at laboratory room temperature until effervescence ceases.

 

(5)     Turn on the heating device and slowly raise the temperature of the reaction mixture to reflux condition. Maintain for 2 hours.

 

(6)     Ensure that the condensation zone is lower than half of the height of the condenser.

 

(7)     After 2 hours of reflux, allow to cool and rinse the condenser with 10 ml of distilled water.

 

(8)     Transfer the contents quantitatively into a 500 ml volumetric flask and dilute to the mark with water. The test solution corresponds to a 500 times dilution of the sample.

 

(9)     Test solution can be filtered, if necessary (should not be required for Zinc Oxide Suspension concentrate). If filtered, discard the first 20 ml (approx) portion for analysis.

(10)   Prepare a blank test solution following the same procedure as the sample. This is to be used for background correction of analysis, in case of any possible contamination through reagents.

 

(11)   Measurement can be carried out immediately, or can be stored in tightly closed plastic vessels for up to 15 day.

Note:-Addition of one drop of octanol to the reaction vessel can be used as an antifoaming agent.

(e)      Determination of Zinc in the extracted material:

Process for analysis of Zinc shall be as per the procedure specified at Method no. 7 (iii) (b) (2) step (B) onwards or method No. 8 (ii) (b) step (2) onward.

Note:-Calculation need to be adjusted accordingly, in view of extent of dilution of original sample.]

(ii) Determination of lead

By the method as specified in 8 (v) [156][specified in 8(v) after extraction thorugh aqua regia as specified in sub-item (d) of item (i)]

(iii) Determination of specific gravity

By the method as specified in 21

[157][(iv) For determination of Arsenic

By the method specified as 8 (ix) after extraction thorugh aqua regia as specified in sub-item (d) of item (i).

(v) For determination through Cadmium

By the method specified as 8 (x) after extraction thorugh aqua regia as specified in sub-item (d) of item (i).]

27. Determination of Boron in Colemanite :-

(a)      Reagents:-

(1)     Mannitol

 

(2)     Bismuth nitrate solution: Dissolve 22g of bismuth nitrate {(BiNO3)3.5H20} in 8 ml of conc. Nitric acid. Warm slightly and dilute to 100 ml with distilled water.

 

(3)     Nitric acid - Concentrated AR grade.

 

(4)     Dilute nitric acid - (1:20).

 

(5)     Sodium hydroxide solution - 10% MN.

 

(6)     Sodium hydroxide solution - 0.5M.

 

(7)     Bromothymol blue indicator solutions.

(b)      Procedure:-

(i)       Weigh accurately 2.5g of sample into 250 ml of beaker.

 

(ii)      Add 5m1 of concentrated Nitric acid and 50 ml of water, warm gently and dilute to 100 ml cool and transfer the contents into 250 ml volumetric flask and dilute to the mark with distilled water.

 

(iii)     Filter through a dry filter paper Whatman No.40 rejecting the first few drops into a beaker.

 

(iv)    Pipette 100 ml of the filtrate into 250 ml beaker, add a few drops of indicator solution.

 

(v)      Add few drops of 10% NaOH solution with thorough stirring until the indicator turns blue.

 

(vi)    Filter through a dry filter paper into 250 ml beaker and carefully wash the residue several times with cold water. The total volume should be 150¬200 ml.

 

(vii)   Adjust the pH to about 5 by adding dilute nitric acid. Warm to about 90° C (do not boil) and stir vigorously to avoid carbon dioxide. Cool the solution.

 

(viii)  Adjust the pH to exactly 6.3 using NaOH solution.

 

(ix)    Add 10g of mannitol and again adjust pH to exactly 6.3 with 0.5 NaOH solution.

 

(x)      Continue adding mannitol in 10g portion till pH remains constant at 6.3. Note the total volume 0.5 NaOH use for the first addition of mannitol.

 

(xi)    Carry out a blank determination to which borate is not added.

(c)      Calculation:

Percentage boron = (A-B) x 1.3512/W

Where A is the volume of 0.5 N NaOH solution used in the sample

B is the volume of 0.5 N NaOH solution used in the blank.

28. Method of Analysis of Customized and Fortified Fertilizers:-

(i)       Determination of nitrogen by method 3 (iv) or 3 (v).

 

(ii)      Determination of ammoniacal nitrogen by method 3 (vii).

 

(iii)     Determination of neutral ammonium citrate soluble phosphate by method 4 (v).

 

(iv)    Determination of water soluble phosphate by method 4 (iii).

 

(v)      Determination of water soluble potash by method 5 (i).

 

(vi)    Determination of sulphur by method 24.

 

(vii)   Determination of micronutrients in Customized or Fortified Fertilisers.

(a)      Sample Preparation:-

1.        Weigh accurately 2.5g sample into a 250 ml beaker. Add 50 ml of 1+1 HCI and cover with a glass.

 

2.        Heat to boiling and continue to boil until volume is reduced to about 25 ml.

 

3.        Dilute to about 100 ml with water and bring to boil.

 

4.        Cool, transfer to a 500 ml volumetric flask and dilute to volume with water.

 

5.        Mix thoroughly and allow to stand until a clear solution is obtained or filter a portion through a dry whatman No.40 filter paper.

 

6.        Transfer 25 ml aliquot to 250 ml volumetric flask, dilute to volume and mix thoroughly.

 

7.        Dilute it further to suitable standard working range with acidified water.

 

8.        Prepare a blank solution in the same manner, omitting the sample.

(b)      Preparation of Standard Stock Solution, working standards and Determination:

As given in Method 22 A

(c)      Determination of Boron-Method 23

29.Determination of Plant Available Silicon (Si(OH)4)

CaCl2 extraction of Silicon fertilizer amendment

Analysis with UV

(a)      Reagents: Do not store any reagent in glass containers, and do not expose to glassware any longer than absolutely necessary while making up reagents. e.g. dissolve reagent/prepare solution in plastic beaker with slightly less than the final volume of solvent, and use volumetric glassware only for a short interval at the very end to make up to volume.

1.        Extractant 0.01 M CaCl2: Dissolve 7.35 g CaCl2.2H2O in de-ionised water, and make up to 5L.

 

2.        Tartaric Acid: Dissolve 100 g of tartaric acid and make up to 500 ml with deionized water. Store in polyethylene bottle. Make up fresh solution when appreciable sediment forms. Store in refrigerator.

 

3.        ANSA reducing agent: Dissolve 25 g of sodium bisulphite (NaHSO3) in 200 ml water, and combine with a solution containing 2 g of anhydrous sodium sulfite (Na2SO3) and 0.4 g of 1-amino-2-napthol-4- sulfonic acid in 25 ml of water. Dilute the combined solution to 250 ml and store in a polyethylene bottle in fridge. Discard if solution darkens in colour.

 

4.        Ammonium paramolybdate tetrahydrate: Dissolve 54 g ammonium molybdate (see note 2) in about 800 ml deionised water in a plastic beaker. Adjust pH to 7 with 5 N NaOH or 0.5 M H₂SO₄ depending on whether the pH needs to be raised or lowered. Make up to 1 L, and store in polyethylene bottle in refrigerator.

 

5.        0.5M Sulfuric Acid: 56 ml of conc. sulfuric acid (from plastic bottle) in 2 L deionised water.

 

6.        5NNaOH: 20 g of NaOH pellets in 100 ml of deionised water (Make and store in plastic container.

(b)      Standards:

A minimum of 5 calibration standards must be prepared; covering the core range from 0 to 5.0 mg/L. Higher standards may be included. Suggested standards are: Si Primary standard - 1000 mg/L Si. Commercial Si standard solution is used.

Si Secondary standard - 50 mg/L Si: Dilute 50 ml primary standard to 1 L with deionised water. Store in tightly stoppered polyethylene bottle.

Working standards: Prepare 0, 0.5, 1, 2, 3, 4, 5, and 6 mg/L Si standards equivalent to 0, 5, 10, 20, 30, 40, 50, 60mg/kg in the Silicon Fertiliser. Add 0, 0.5, 1 ,2 ,3 ,4, 5,and 6ml of secondary standard to separate 50 ml volumetric flasks and make up to volume with 0.01 M CaCl2.

0.01 M CaCl2 is the 0 standard.

Method: 1. Dry approximately 2-3 grams of Silicon fertiliser in a 1050C oven overnight. Grind the sample if not already in powder form.

2. Weigh 0.4 g of dried Silicon fertiliser into a 70 ml container, and add 40 ml 0.01 M CaCl2. Lid, and shake in an end over end shaker overnight (16 hours). Centrifuge sample extract at 2000 rpm for 10 minutes. The extract should be clear.

3. Transfer 1 ml of filtrate into a 20 ml capacity test tube (See note 4)

4. Add 2.5ml of 0.5M sulfuric acid

5. Add 2.5ml ammonium molybdate solution

6. Shake well on a vortex stirrer and wait 5minutes.

7. Add1.25ml tartaric acid solution

8. Add 0.25ml ANSA reducing solution. Mix well.

9. Prepare a sample blank for each sample in a similar way, but using water instead of the ammonium molybdate solution. Also prepare a reagent blank, using 0.01M CaCl2 instead of sample and water instead of the ammonium molybdate solution. The reagent blank is used to zero the spectrophotometer prior to calibration.

10. Prepare a standard curve from the working standards by using the samealiquot for the standards as is used for the samples and treat the same way. (See note 5.)

11. The spectrophotometer should be set to 820 nm wavelength. After 30 minutes, transfer reagent blank to spectrophotometer cell, place in machine and zero absorbance. Remove, transfer sample to cell, place in machine and record absorbance reading (ie. colour intensity due to amount of soluble silica Si in sample). Wash cell before next sample with a small amount of the next sample blank.

12. Read the concentration of silica Si in the soil sample, mg/kg Si, directly from a regression equation prepared from the standard curve.

[158][Note:- 1. Discard ANSA solution if it does not completely dissolve, or yields a dark solution immediately. Try again after changing source of de-ionised water.

2. Molybdate compounds are considered as environmental hazard. Waste containing those elements has to be collected and disposed of according to regional requirements.

3. Avoid use of glass whenever possible. All standards and reagents should be kept in polyethylene or other plastic bottles, particularly NaOH to avoid any possibility of it being stored in glass. (NaOH is able to actively dissolve silica in glass)

4. Do not start filling glass test tubes in advances with any of the reagents or sample, at the glass can leach silicon.

5. As the same amount of each reagent is used for both standard solutions and samples, a small amount of Si contamination can be tolerated. The calibration line will allow for minor background contamination. However, if the blue colour in the zero stand becomes too intense, the working range may be pushed beyond the linear range of the calibration line, and all contain solutions must be prepared again. Si Contamination may occur in one or more of the following solutions; de-ionised water (used to make up one or all of the solutions), 0.5 sulfluric acid, ammonium para molybdate, tartaric acid or ANSA. Another de-ionised water supply should be used, if available. If Si is still present, reagents and extractant may need to be prepared in distilled, no de-ionised water.]

[159][30. Method of analysis of Sodium Silicate

(i)       Determination of Silicon

(a)      Chemicals and Glasswares:

(1)     Conc. HCl

 

(2)     Conc. HNO3

 

(3)     Hot Plate

 

(4)     Platinum Crucible

 

(5)     Muffle Furnace (Temp. capacity by 10000C)

 

(6)     Desiccators and other routine laboratory glasswares

(b)      Procedure:

(1)     Take 1 gm of prepared sample in Teflon or corning beaker, add 2-3 ml HCl solution (1:1) and 2-3 ml HNO3 solution (1:1).

 

(2)     Digest the solution on a hot plate till it becomes semi-solid, cool it and again add 3-4 ml HNO3 solution. Dry it completely on hot plate.

 

(3)     Add 2-3 ml HCl solution (1:1) and boil it till yellow fumes cease. Filter it with Filter Paper No. 1, wash with 10 ml HCl solution (1:1) one time and 2-3 washing with hot water .

 

(4)     Transfer the filter paper alongwith residue in pre-weighed platinum crucible, dry for one and half hour in muffle furnace at 250oC temperature and finally ignite the residue at 950oC temperature for 30 minutes.

 

(5)     Cool the crucible in desiccator and re-weigh and calculate

Calculation: (i) Determination of sodium

By the method as specified in serial number 17

(ii) Determination of Specific gravity

By the method as specified in serial number 21]

[160][31. Method of analysis of nano Nitogen

(i)       Determination of Nitrogen-Total Kjeldahl Nitrogen.

(a)      Procedure:

(1)     Liquid Nano Fertilizer sample: Take aliquot quantity (10 ml) of sample in the Kjeldahl flask.

 

(2)     In case of solid Nano Fertilizer Sample: Take one gram of powdered nano-fertilizer sample is transferred to the Kjeldahl flask

 

(3)     Add 15 g K2SO4   or 12 g anhydrous Na2SO4, 0.4g anhydrous CuSO4, or 0.6g CuSO4.5H2O, and approximately 0.8g alundum granules.

 

(4)     Add 37 ml diluted Sulfuric acid with water H2SO4+H2O(1+1, v/v) or 20 ml concentrated Sulfuric acid, if adequate ventilation is available.

 

(5)     Add sufficient test portion mass, precisely 0.1000 to 2.800 g for fertilizers with 30 to 5% nitrogen, respectively. Rinse the inner wall with about 10ml water.

 

(6)     Transfer the flask to a preheated (400oC) Kjeldahl block digestor and digest test portions for 75 minutes.

 

(7)     Remove the flask from the heating block and upon cooling (the reaction mixed must be near room temperature). Wash the inner wall with 20-30 ml water and mix.

 

(8)     Prepare the distillate receiving flask (300ml Erlenmeyer flask) by adding 30ml of 0.25 N standardized Sulfuric acid to trap the expected total Nitrogen in the test portion.

 

(9)     Add 2-3 drops of Methyl purple indicator and install the receiver on the outlet tube of the distillation unit, being sure that the distillate outlet tube end is totally immersed in the standardized acid solution.

 

(10)   Install the digestion tube on the distillation unit. Initiate steam generation and slowly dispense about 80ml (30-35%) Sodium Hydroxide into the flask.

 

(11)   Continue steam distillation until about 250 ml or more of steam condensate has been collected in the receiving flask. This usually requires about 6-8 minutes.

 

(12)   If color changes to green, add more 0.25 N H2SO4   to bring the color back to purple and record the amount of acid added.

 

(13)   Titrate to a grey end point (pH5.7) with 0.25 N Standard NaOH. The color of the distillate depends upon the amount of total nitrogen in the test portion, which is a function of the amount of ammonia trapped in the receiver flask.

 

(14)   A green color indicates that the acid in the trap was neutralized by the Ammonia. At this point, add an additional known amount of standardized H2SO4   to get to the grey end point.

 

(15)   The net volume (in ml) of standardized acid would be equal to the total amount of acid initially added to the receiving flask plus the amount of the acid added, after distillation, to reach the grey end point. A blue or Purple colour indicates that there is still acid in the receiving flask, and back titration with NaOH is required.

 

(16)   The net volume standardized acid would be equal to the amount of acid in the receiving flask minus the amount of base added, after distillation, to reach to the grey end point.

(b)      Calculations:

Weight percent total nitrogen is calculated as follows:

(ii)      Physical Particle Size (as per Transmission Electron Microscope (TEM) Analysis)

(a)      Equipment and Apparatus:

(1)     Transmission Electron Microscope

 

(2)     Sample grid

 

(3)     Tweezers, Petri dish, Ethanol and Deionized water

(b)      Procedure:

(1)     TEM sample grids carbon coated film that is electron transparent supported by copper mesh or equivalent are suitable.

 

(2)     Glassware and apparatus used for sample preparation should be cleaned with filtered, demineralized water and stored dry.

 

(3)     The apparatus used for dispersion and deposition of particles consists of a small glass vial with a screw-on cap, a teflon pillar about 10 mm high that may be inserted into the vial, a petri dish, and a teflon block about 40 mm by 40 mm square.

 

(4)     Hold the grid with tweezers, dip rinse the grid thoroughly with ethanol. Wick the excess liquid off the grid using filter paper. Place the dried grid onto the clean Teflon block.

 

(5)     Place a 10 µL drop of the nanoparticle solution onto the grid.

 

(6)     Cover the grid with a petri dish lid and let stand at room temperature for getting the grid dry, typically from 5 to 30 minutes, depending on solvent type.

 

(7)     Transfer the grid on TEM sample holder. Record enough micrographs to image a minimum of 200 nanoparticles per sample per grid square from a minimum of 2 widely separated regions of the grid using a well-aligned and stable TEM, operated at a fixed magnification that allows a large number of nanoparticles to be visible within the micrograph field of view, while ensuring that each individual nanoparticle is recorded with a large number of image pixels.

(c)      Precautions:

(1)     Transmission Electron Microscope grids (especially thin film membranes) are very fragile and must be held by their edges with fine tweezers so as not to damage or crack the membrane.

 

(2)     Exposure of Transmission Electron Microscope grids to the ambient environment should be minimized to reduce the likelihood of dust contamination. Grids should be stored in suitable boxes in dust-free or desiccating cabinets.

 

(3)     A well-aligned Transmission Electron Microscope is essential to obtain accurate particle size results.

 

(4)     A minimum of 200 discrete particles should be measured from each of at least two widely separated regions of the sample (that is, different grid squares or membrane regions). Foreign debris in a given image (e.g., dust particles or residues from the rinsing and drying process) should be avoided.

 

(5)     Particle size results obtained from Transmission Electron Microscope measurements may not coincide with those obtained from other techniques (e.g., dynamic light scattering). This is due in part to differences in the weighted averages determined in each case (e.g., number for Transmission Electron Microscope versus intensity for dynamic light scattering), as well as differences in the physical property that is actually measured (e.g., projected area versus hydrodynamic diffusion area).

(iii)     Hydrodynamic particle size (as per Dynamic Light Scattering (DLS) Analysis

(a)      Equipment and Apparatus:

(1)     Dynamic Light Scattering Equipment

(2)     Sample Cuvettes of size

(3)     Deionized water

(b)      Procedure:

(1)     For liquid nano-fartilizer sample, 10 ml is sonicated for one minute and used for the analysis. In case for solid nano-fertilizer, fertilizer: distilled water (1:10 ratio) suspension is prepared, sonicated for one minute

 

(2)     Known standard samples (either one of the nano particles such as Ag, Au or TiO2) are used to set the machine

 

(3)     Load sample into the Cuvette

 

(4)     Pre-rinse filter with solvent (at least 1 ml, depending on filter size and dead volume of filter holder or cartridge).

 

(5)     After loading syringe with sample and inserting syringe filter, allow the first 4 drops to go to waste. Use the next 4 drops to pre-rinse the cuvette, and discard. The remainder can be used for the sample measurement.

 

(6)     Load sample into cuvette using minimum amount necessary to ensure liquid level is at least 2 mm above the entrance height of the laser beam for your particular instrument configuration.

 

(7)     Take care not to touch the cuvette windows with your bare hands while loading. Wipe outside of quartz or glass cuvette with lens paper if needed. Cap the cuvette to prevent dust contamination and solvent evaporation.

 

(8)     Inspect the cuvette to ensure that air bubbles are not clinging to the optical window area.

 

(9)     Load the sample into Dynamic Light Scattering machine.

 

(10)   Perform 3 to 10 independent measurements per sample.

(c)      Precautions:

(1)     To measure the size of solid phase nano nitrogen particles, 1 gram of nanoparticles sample should be suspended in 20 ml water followed by 1 minute ultra-sonication before the size measurement carried out by the Dynamic Light Scattering.

 

(2)     Measurement cuvettes should be cleaned with filtered demineralized water and stored dry.

 

(3)     The choice of pore size depends on the maximum dimension of the test particles and their tendency to adhere to the filter membrane.   µ   Suspended medium (such as solvent, dispersant, solution) should be filtered prior to sample preparation using a 0.1 or 0.2.

 

(4)     A typical starting sample concentration is 1 mg/ml.

 

(5)     Use cuvette with quartz or equivalent optical-quality windows.

 

(6)     Pre-rinse cuvette with filtered solvent at least 3 times.

(iv)    Zeta Potential Analysis

(a)      Equipment and Apparatus:

(1)     Dynamic Light Scattering (DLS).

 

(2)     Sample Cuvettes of zeta.

 

(3)     Deionized water.

(b)      Procedure:

(1)     For liquid nano-fertilizer sample, 10 ml is sonicated for one minute and used for the analysis and in case for solid nano-fertilizer, fertilizer: distilled water (1:10 ratio) suspension is prepared, sonicated for one minute.

 

(2)     Known standard samples (either one of the nano particles such as Ag, Au or TiO2) are used to set the machine.

 

(3)     Loading Sample into the Cuvette.

 

(4)     Pre-rinse filter with solvent (at least 1 ml, depending on filter size and dead volume of filter holder or cartridge).

 

(5)     After loading syringe with sample and inserting syringe filter, allow the first 4 drops to go waste. Use the next 4 drops to pre-rinse the cuvette, and discard. The remainder can be used for the sample measurement.

 

(6)     Load sample into cuvette using minimum amount necessary to ensure liquid level is at least 2 mm above the entrance height of the laser beam for your particular instrument configuration.

 

(7)     Take care not to touch the cuvette windows with your bare hands while loading. Wipe outside of quartz or glass cuvette with lens paper if needed.

 

(8)     Cap the cuvette to prevent dust contamination and solvent evaporation.

 

(9)     Inspect the cuvette to ensure that air bubbles are not clinging to the optical window area.

 

(10)   Load the sample into Dynamic Light Scattering machine.

 

(11)   Perform 3 to 10 independent measurements per sample.

(c)      Precautions:

(1)     Measurement cuvettes should be cleaned with filtered demineralized water and stored dry. The choice of pore size depends on the maximum dimension of the test particles and their tendency to adhere to the filter membrane. µ suspending medium (such as solvent, dispersant, solution) should be filtered prior to sample preparation using a 0.1 or 0.2

 

(2)     A typical starting sample concentration is 1 mg/ml.

 

(3)     Use cuvette with quartz or equivalent optical-quality windows.

 

(4)     Pre-rinse cuvette with filtered solvent at least 3 times.

(v)      Viscosity Measurement:

(a)      Equipment and Apparatus:

(1)     Demineralised water.

 

(2)     Viscometer.

 

(3)     Measuring cylinder.

 

(4)     Bottle Adapter.

(b)      Procedure:

(1)     Calibrate the viscometer with distilled water to set the machine as 1 cps.

 

(2)     Viscometer Assembly.

 

(3)     Attach vertical pole to the base using the wrench provided in the case.

 

(4)     Attach the viscometer to the vertical pole.

 

(5)     Connect power cable to the viscometer.

 

(6)     Turn on the viscometer and calibrate.

 

(7)     Starting up-Select and attach required spindle.

 

(8)     Raise the viscometer to the highest level using a screw on the vertical pole.

 

(9)     Place beaker with liquid under the spindle.

 

(10)   Lower the viscometer until the spindle is submerged to the spindle's mark.

 

(11)   Viscometer Operation:-This depend on the software of the instrument make. The analyst should follow the manufacturer's operating instructions for a particular instrument. Set the viscometer using distilled water to measure 1cps at room temperature.

(c)      Precautions:

(1)     Wait for 30-60 sec before reading.

 

(2)     Good results are in range 60%-80% of torque.

 

(3)     Results depend on beaker and volume of liquid so use the same beakers for comparison measurements. Viscosity of a Liquid nano-fertilizer N is measured directly.

 

(4)     For solid nano-fertilizer, fertilizer: water suspension should be in 1:10 ratio with distilled water.

(vi)    Measurement of pH

(a)      Apparatus:

pH meter, vacuum pump, beaker, pipette, glass rod, china dish, spatula etc.

(b)      Reagents:

Buffer solutions of pH 4.0, 7.0 and 9.2: One buffer tablet of the respective pH is dissolved in water and the volume is made to 100 ml.

(c)      Procedure:

(1)     Take 10 ml of liquid sample, homogenise it and take the pH measurement. For solid/powder samples (1 g dry sample/10 ml water) homogenisation or ultrasonic agitation of the sample for 1 minute followed by pH measurement should be taken after settling of the samples.

 

(2)     pH meter is set at room temperature and calibrated by immersing theelectrodes in different buffer solutions of pH 4.0, 7.0 and 9.2.

 

(3)     Take the beaker of homogenised samples and dip the electrodes into it and note the pH reading.

 

(4)     After each determination the electrodes must be washed with distilled water and wiped out by ordinary filter paper.

(d)      Precautions:

(1)     Proper homogenisation/sonication must be done.

 

(2)     The glass and reference electrode of pH meter should always remain dipped in water.

 

(3)     Buffer solutions should be prepared accurately and stored well in glass container.

 

(4)     It is desirable to prepare fresh buffer solutions after few days. Connect the pH meter to the stabilizer to avoid the fluctuations in pH readings. Adjust the temperature knob of pH meter at room temperature for correct pH determination]

[161][32. Method of analysis of Zinc Polyphosphate

(i)      Quality of reagents

Pure chemicals and distilled water shall be used in tests.

Note: Pure chemicals shall mean chemicals that do not contain impurities which affect the results of analysis.

Demineralised water means the water obtained after passing distilled water through a cation and an anion exchange resins or a combined cationation exchange resin. Glass distilled water means distilled water that is redistilled in a glass distillation apparatus.

(ii)    Determination of zinc:

(a)      Reagents

(1)     Standard zinc solution-Weigh accurately 1.0 g of zinc metal A.R. grade in a 250 mL beaker. Add 20 mL HCl (1: 1) to it and cover with a watch glass. Keep it for a few hours and allow it to dissolve completely. Transfer it to one litre flask through a funnel giving at least 10 washings of beaker and funnel with glass distilled water. Make up the volume using glass distilled water. Stopper the flask and shake the solution well. This is 1000 ppm zinc solution herein after called Standard A. This solution should be stored in a clean bottle for further use. Dilute 10 ml of 1000 ppm solution of zinc (Standard A) to 1 litre to get 10ppm standard zinc solution designated as Standard B.

 

(2)     Concentrated hydrochloric acid (HCl).

 

(3)     Glass distilled water of pH 2.5. Dilute 1 ml of concentrated hydrochloric acid to one litre with glass distilled water and adjust the pH to 2.5 with a pH meter using HCl or NaOH. This solution is called acidified water and 5 to 10 litres of this solution should be prepared at a time. Do not use sulphuric acid for preparing this acidified water.

 

(4)     Preparation of working standards-Pipette the following volume of Standard B in 50 ml numbered volumetric flask and make the volume with acidified water (See Table below). Stopper the flasks and shake them well. Prepare the standard in duplicate. The same acidified water should be used for preparing the solution of unknown fertilizer samples. Fresh standards should be prepared every time when a fresh lot of acidified water is prepared.

Flask No.

(b)      Procedure

(1)      Preparation of zinc polyphosphate fertilizer sample-Weigh 250 mg (0.25 g) fertilizer in a clean watch glass. Transfer into a 250 mL Erlenmeyer flask (conical flask) using a funnel. Wash the watch glass and funnel with 10 mL concentrated hydrochloric acid. Do not use sulphuric acid for dissolving the sample. Do not dilute with water. Place a funnel over the mouth of the Erlenmeyer flask and heat over a hot plate till fumes of acid appear. Allow the solution to cool to room temperature. Carefully add 100 mL water and swirl to mix. Then filter through Whatman 1 filter paper into a 1L volumetric flask. Wash the Erlenmeyer flask and filter paper repeatedly (at least ten times with 10 mL portions of water) and then dilute to volume. Prepare these solutions in duplicate.

(2)      Pipette 10 ml of the prepared solution in 500 ml volumetric flask and make the volume with acidified water (hydrochloric acid water).

(3)      Flaming the solutions--Flame the standards and the filtered samples on atomic absorption spectrophotometer at a wavelength of 213.8 mu (Zn line of the instrument).

(c)      Calculations

Prepare a standard curve of known concentrations of zinc solution by plotting the absorbance values on Y-axis against their respective zinc concentration on X-axis Calculate the percentage zinc in zinc fertilizer by multiplying zinc concentration value calculation from standard curve by 20.

Example

Weigh of the fertilizers sample .................. = 0.25 g

Volume made ............................................. = 1000 ml

Further dilution .......................................... = 50 times

Reading of the samples form atomic absorption...= Y

Corresponding concentration value of zinc from standard curve against Y absorbance ................................................ = X ppm

Percentage zinc in the fertilizer ................. = 20X

(d)      Precautions.

(1)     Weighing must be done on an electric or electronic balance.

 

(2)     All the glass apparatus to be used should be of corning or borosil make and washed with dilute hydrochloric acid (1:4), and subsequently washed thoroughly with distilled water and then with glass distilled water.

 

(3)     The pipette should be rinsed thrice with the same solution to be measured.

 

(4)     The outside or the pipette should be wiped with filter paper after taking out from the solution to be measured.

 

(5)     After using the pipettes, wash with distilled water and place them on a clean dry filter paper in order to prevent contamination.

 

(6)     To start filtration only a few drops should be added first in order to wet the filter paper and then continue further filtration.

 

(7)     Do not use sulphuric acid for dissolving the sample or for dilution of solution prior to analysis.

(iii)   Determination of magnesium

(a)      Reagents

(1)     Strontium chloride-Dissolve 7.5 g of strontium chloride (SrCl2.6H2O) in one litre of glass distilled water.

 

(2)     Standard magnesium solution-Weigh 0.507 g of magnesium sulphate (MgSO4.7H2O) on a clean watch glass and transfer it to one litre flask through the funnel giving several washings to watch glass and the funnel with glass distilled water. This is 50ppm Mg solution Dilute 10 ml of 50 ppm solution of Mg to 100 ml to get 5 ppm standard Mg solution.

 

(3)     Preparation of working standards-Pipette the following volume of 5 ppm standard Mg solution in 50 ml numbered volumetric flasks. Add 10 ml of strontium chloride solution to each flask and make up the volume to 50 ml. Stopper the flask and shake them well prepare fresh standards every for night.

(b)      Procedure.

(1)     Pipette 5 ml of the solution which was prepared for the determination of zinc by dissolving 0.25 g of the fertilizer sample in one litre flask [this section (ii) (b) (1)] Add 50 ml of strontium chloride Make up the volume to 250ml.

(2)     Flame the standards and the samples on atomic absorption spectrophotometer at a wave length of 285.5 mu (Mg line of the instrument)

(c)      Calculations

Prepare a standard curve of known concentrations of Mg solutions by plotting the absorbance value on Y-axis against their respective concentration values on X-axis. Percentage magnesium in the fertilizer will correspond to the magnesium concentration value calculated from the standard curve multiplied by 20.

Example: Weight of the fertilizer ............................. = 0.25 g

Volume made ........................................... = 1000 ml.

Further dilution ......................................... = 50 times

Reading of the sample from atomic absorption spectrophotometer ..................................... = Y

Corresponding concentration of Mg from standard curve against Y absorbance ................................ = X ppm

Percentage magnesium in the fertilizer ............... = 20X

(iv)   Determination of lead

(a)      Reagents.

(1)     Standard lead solution-Weigh 0.1599 g of lead nitrate [Pb(NO₃)₂] on a clean watch glass and transfer it to one litre flask through a funnel using glass distilled water. Add 10 ml of concentrated distilled nitric acid and make the volume upto the mark. Stopper the flask and shake the solution well. This is 100 ppm lead solution and should be stored in a clean bottle for further use. Dilute 10 ml of 100 ppm solution of lead to 100 ml with 1 percent nitric acid solution to get 10 ppm standard lead solution.

 

(2)     1 percent nitric acid solution-Dilute 10 ml of concentrated distilled nitric acid to one litre with glass distilled water.

 

(3)     10 percent nitric acid solution-Dilute 10 ml of concentrated distilled nitric acid to 100 ml with glass distilled water.

 

(4)     20 percent zinc sulphate solution-Weigh 20g of zinc sulphate (ZnSO₄.7H₂O) and dilute to 100 ml with 1 percent nitric acid solution.

 

(5)     Preparation of working standards-Pipette the following volume of 10 ppm standard lead solution in 50 ml numbered volumetric flasks. Add 5 ml of 20 percent zinc sulphate solution to each flask and make the volume with 1 percent nitric acid solution.

Stopper the flasks and shake them well.

(b)      Procedure.

(1)     Preparation of zinc polyphosphate fertilizer samples-Weigh 1 g of the material on a clean watch glass and transfer to 100 ml volumetric flask through the funnel using 10 ml of 10 percent nitric acid solution. Let it stand for a few hours till it dissolves. Add 10 mL of 20% zinc sulphate solution to the flask. Make the volume with glass distilled water. Samples should be prepared in duplicate.

(2)     Flaming the solution--Flame the standards and the samples on atomic absorption spectrophotometer at a wavelength of 217 m (Lead line of the instrument)

(c)      Calculations

Prepare a standard curve of known concentrations of lead solution by plotting the absorbance values on Y-axis against their respective lead concentration on X-axis. Calculate the percentage lead in zinc polyphosphate fertilizer by multiplying lead concentration value calculated from standard curve by 0.01.

Example: Weight of the fertilizer ............................. = 1.0 g

Volume made ........................................... = 100 ml.

Further dilution ......................................... = Nil

Reading of the sample from atomic absorption spectrophotometer ..................................... = Y

Corresponding concentration of Pb from standard curve against Y absorbance ................................ = X ppm

Percentage Pb in the fertilizer ............... = 0.01X

(v)     Determination of Arsenic (as As)

The principle and reagents in this case shall substantially be the same as given in Schedule IV, Part D, 12 relating to determination of As in organic fertilizers by Atom Absorption Spectrophotometer (AAS).

(a)      Reagents.

(1)     Standard sodium hydroxide solution--approximately 20 percent.

 

(2)     Standard arsenic trioxide solution-Dissolve 1.320 gm. of resublimed arsenic trioxide (AS₂ O₃) in 25 ml. sodium hydroxide solution and neutralize with dilute sulphuric acid. Dilute with freshly distilled water containing 10 ml of concentrated sulphuric acid per liter and make up the volume to 1 liter. This solution contains 1000 ppm As and is solution A.

 

(3)     Pipette 5 mL of solution A into a 1 L volumetric flask and dilute to volume. This solution contains 5 ppm As and is solution B.

 

(4)     Prepare standards having concentration of 0.05, 0.1 and 0.2 ppm by diluting 1.0, 2.0 and 4.0 ml, respectively of 5 ppm Arsenic solution (solution B) with double distilled water in volumetric flask and make up the volume to 100 ml.

(b)      Procedure.

(1)     Preparation of zinc polyphosphate fertilizer sample-Weigh 1.0 g of fertilizer in a clean watch glass. Transfer into a 250 mL Erlenmeyer flask (conical flask) using a funnel. Wash the watch glass and funnel with 10 mL concentrated hydrochloric acid. Place a funnel over the mouth of the Erlenmeyer flask and heat over a hot plate till fumes of acid appear. Allow the solution to cool to room temperature. Carefully add 100 mL water and swirl to mix. Neutralise the solution with 12 mL I N NaOH solution. Transfer to a 1 L volumetric flask and make up volume.

 

(2)     Estimate Arsenic using vapour generation assembly attached to Atomic Absorption Spectrophotometer as per the procedure given for the instrument. Use the solution of fertilizer directly without further dilution.

(c)      Calculations.

Prepare a standard curve of known concentrations of As solutions by plotting the absorbance value on Y-axis against their respective concentration values on X-axis. Percentage As in the fertilizer will correspond to the As concentration value calculated from the standard curve multiplied by 0.1.

Example: Weight of the fertilizer ............................. = 1.0 g

Volume made ........................................... = 1000 ml.

Further dilution ......................................... = Nil

Reading of the sample from atomic absorption spectrophotometer ..................................... = Y

Corresponding concentration of AS from standard curve against Y absorbance ................................ = X ppm

Percentage As in the fertilizer ............... = 0.1X

(vi)   Determination of cadmium

Same as provided in paragraph (x) under subheading 7.

(a)      Reagents and procedure same as in subheading 7 (x).

(b)      Procedure.

(1)     Preparation of zinc polyphosphate fertilizer sample-Weigh 1.0 g of fertilizer in a clean watch glass. Transfer into a 100 mL beaker with 10 mL 20 percent hydrochloric acid. Heat over a hot plate till dissolved. Allow the solution to cool to room temperature. Neutralise with 4% NaOH solution (1 N NaOH) to pH 2.5. Transfer to a 100 mL volumetric flask and make up volume.

(2)     Aspirate the standards as well as the sample solution for Cd on an atomic absorption spectrophotometer at a wavelength of 228.8 nm using air acetylene flame and note the absorbance for each solution.

(c)      Calculations.

Prepare a standard curve of known concentrations of Cd solutions by plotting the absorbance value on Y-axis against their respective concentration values on X-axis. Percentage As in the fertilizer will correspond to the Cd concentration value calculated from the standard curve multiplied by 0.01.

Example: Weight of the fertilizer ............................. = 1.0 g

Volume made ........................................... = 100 ml.

Further dilution ......................................... = Nil

Reading of the sample from atomic absorption spectrophotometer ..................................... = Y

Corresponding concentration of Cd from standard curve against Y absorbance ................................ = X ppm

Percentage Cd in the fertilizer ............... = 0.01X

(vii)  Determination of pH

(a)      Procedure

Weigh 5 g of fertilizer into a 100 mL beaker. Add 50 mL distilled water, stir and immediately record pH before the suspension sediments.

(viii)    Determination of water soluble zinc.

(a)      Reagents

As described in item (ii) (a) of this serial number relating to "Determination of Zinc".

(b)      Procedure.

(1)     Extraction of water soluble zinc

Weigh 250 mg zinc fertilizer into a 500 mL Erlenmeyer flask (conical flask). Add 100 mL of glass distilled water. Place a stopper at the mouth and shake the solution in a horizontal shaker for 15 min. Filter through a Whatman 1 filter paper into a 500 mL volumetric flask. Wash the Erlenmeyer flask and filter paper repeatedly (at least ten times with 10 mL portions of water). Remove the funnel and filter paper. Add 5 mL concentrated HCl directly to the solution in the volumetric flask and then make up volume. Prepare these solutions in duplicate.

(2)     Pipette 5 ml of the prepared solution in 50 ml volumetric flask and make the volume with acidified water (hydrochloric acid water).

(3)     Flaming the solutions--Flame the standards and the filtered samples on atomic absorption spectrophotometer at a wavelength of 213.8 mu (Zn line of the instrument).

(c)      Calculations

Prepare a standard curve of known concentrations of zinc solution by plotting the absorbance values on Y-axis against their respective zinc concentration on X-axis Calculate the percentage zinc in zinc fertilizer by multiplying zinc concentration value calculation from standard curve by 20.

Example. Weigh of the fertilizers sample .................. = 0.25 g

Volume made ............................................. = 500 ml

Further dilution .......................................... = 10 times

Reading of the samples form atomic absorption...= Y

Corresponding concentration value of zinc from standard curve against Y absorbance ................................................ = X ppm

Percentage water soluble zinc in the fertilizer ................. = 2X

(ix)   Determination of DTPA soluble zinc.

(a)      Reagents

(1)     Prepare a solution of 0.005 M DTPA (diethylenetriaminepentaacetic acid, [(HOOCCH2)2 NCH2CH2]2NCH2COOH; molecular weight 393.35) by weighing 1.97 g DTPA in a 1000 mL volumetric flask. Add 800 mL water and heat till it is completely dissolved. Cool to room temperature and then make up the volume to 1 litre.

(2)     Other reagents as described in item (ii) (a) of this serial number relating to "Determination of Zinc".

(b)      Procedure.

(1)     Extraction of DTPA soluble zinc-Weigh 250 mg zinc fertilizer into a 1 L Erlenmeyer flask (conical flask). Add 250 mL of the DTPA solution. Place a stopper at the mouth and shake the solution in a horizontal shaker for 60 min. Filter through a Whatman 1 filter paper into a 1 L volumetric flask. Wash the Erlenmeyer flask and filter paper repeatedly (at least ten times with 10 mL portions of water). Remove the funnel and filter paper. Add 5 mL concentrated HCl directly to the solution in the volumetric flask and then make up volume. Prepare these solutions in duplicate.

(2)     Pipette 10 mL of the DTPA extracted solution into a 500 mL volumetric flask and make up volume with acidified water (hydrochloric acid water).

(3)     Flaming the solutions--Flame the standards and the filtered samples on atomic absorption spectrophotometer at a wavelength of 213.8 mu (Zn line of the instrument).

(c)      Calculations

Prepare a standard curve of know concentrations of zinc solution by plotting the absorbance values on Y-axis against their respective zinc concentration on X-axis Calculate the percentage zinc in zinc fertilizer by multiplying zinc concentration value calculation from standard curve by 20.

Example. Weigh of the fertilizers sample .................. = 0.25 g

Volume made ............................................. = 1000 ml

Further dilution .......................................... = 50 times

Reading of the samples form atomic absorption...= Y

Corresponding concentration value of zinc from standard curve against Y absorbance ................................................ = X ppm

Percentage DTPA soluble zinc in the fertilizer ................. = 20X

(d)      Precautions.

(1)     Weighing must be done on a electric or electronic balance.

 

(2)     All the glass apparatus to be used should be of corning or borosil make and washed with dilute hydrochloric acid (1:4) and subsequently washed thoroughly with distilled water and then with glass distilled water.

 

(3)     The pipette should be rinsed thrice with the same solution to be measured.

 

(4)     The outside or the pipette should be wiped with filter paper after taking out form the solution to be measured.

 

(5)     After using the pipettes, place them on a clean dry filter paper in order to prevent contamination.

 

(6)     To start filtration only a few drops should be added first in order to wet the filter paper and then continue further filtration.

 

(7)     Do not use sulphuric acid for dilution of solution prior to analysis.]

[162][33. Method of analysis of potassium Thiosulphate and Calcium Thiosulphate (Liquid Fertilizers)

(i)       Determination of potassium by the method as specified in 5 (ii);

 

(ii)      Determination of Specific Gravity by the method as specified in 21 (ii);

 

(iii)     Determination of Calcium by the method as specified in 21 A (v);

 

(iv)    Determination of Arsenic by the method as specified in 8 (ix);

 

(v)      Determination of Lead by the method as specified in 8(v);

 

(vi)    Determination of Sulphur (as S) in potassium thiosulphate and calcium thiosulphate (Liquid Fertiliser).-

(a)      Apparatus.

(i)       Electric hot plate, water bath, muffle furnace, Oven;

 

(ii)      Electronic balance;

 

(iii)     Desiccators;

 

(iv)    Gooch crucible;

 

(v)      Vacuum pump for filtration;

 

(vi)    Electronic balance (0.001g capacity);

 

(vii)   Whatman No. 40 and 50 filter papers;

 

(viii)  Routine laboratory glassware, instruments;

(b)      Reagents.

(i)       Conc. Hydrochloric acid(37% HCL);

 

(ii)      Dilute hydrochloric acid-Take 250 ml of concentrated hydrochloric acid in one litre volumetric flask. Make the volume upto 1000 ml water. Shake and mix it well';

 

(iii)     Barium chloride solution: Dissolve 120 gm barium chloride in 1000 ml of water;

 

(iv)    silver nitrate (5 percent solution): Dissolve 5g of silver nitrate in 100 ml of distilled water;

 

(v)      Hydrogen per oxide 30 percent (fresh) solution: Dilute liquid hydrogen peroxide to bring final concentration 30 percent;

 

(vi)    Sodium hydroxide solution: Dissolve 40g sodium hydroxide salt in 100 ml distilled water;

 

(vii)   Methyl orange indicator: Dissolve 1g methyl orange indicator in 100 ml alcohol. Shake it and store in cool dry Place;

 

(viii)  Sodium Thiosulphate: AR Grade.

(c)      Procedure.

1.        Oxidation of liquid fertilizer test sample;

(a)      Weight 5.0g sample of potassium thiosulphate (or calcium thiosulphate) liquid fertilisers (up to 0.001 g) accurately in a dry, clean 500 ml graduated flask on an electronic balance. Denote "W" to this as weight of sample. Fill the flask to the mark of 500 ml by using double distilled water'.

 

(b)      Add exactly 50 ml (of the diluted sample from (a) to a 500 ml beaker and add approximately 100 ml of water. Add 2 ml of 40% NaOH solution to it. Add now slowly 2 ml of 30% hydrogen per oxide (H2O2) solution. Cover the beaker with watch glass carefully. Heat the solution on low heat on hot plate slowly for about 30 minutes. Cool it and then add slowly 2 ml of hydrogen peroxide 30% solution again. Heat the solution on hot plate slowly. If required add more 1 to 2 ml of hydrogen per oxide solution. Total hydrogen peroxide solution addition should not be more than 6 ml for complete oxidation. Cool the beaker; add 100 ml of water and then mix.

 

(c)      Add a few drops of methyl orange indicator to the solution. Add 2-5 ml of dilute hydrochloric acid and mix it until colour changes to red uniformly. Add a few more drops of acid and mix well with glass rod.

Then, keep the beaker on hot plate (below boiling temperature, <800C) to bring the solution to colorless within 10 minutes.

Note: lf necessary, add a few drops of 30% H2O2 to the beakers to bring the solution to colourless.

2.        Precipitation of sulphur for gravimetric determination of total sulphur,-

(a)      Add slowly 15 ml barium chloride to the oxidized sample to ensure complete precipitation of sulphur as barium sulphate;

 

(b)      Digest the precipitation on a hot plate or water bath for minimum 5 hours at such a temperature that the solution does not boil (around 80oC). Put a watch glass above the beaker to prevent complete evaporation of the solution. Ensure the supernatant liquid to be clear and transparent. Cool it to room temperature and keep it over night to settle precipitates;

 

(c)      Take 30 ml capacity G4 grade Sintered Gooch crucible. Dry it in furnace at 2500C; cool it and record weight of empty crucible(G1);

 

(d)      Pour the sample with precipitate into 30 ml capacity G4 grade Sintered Gooch Crucible previously weighed. Filter it. Wash the precipitate 10-12 times with hot water to ensure the precipitate to make it free from excess barium chloride. The filtrate may be tested with silver nitrate solution to confirm that the precipitate is free from chloride.

 

(e)      Dry the crucible having barium sulphate precipitate at 2500 C for two hours in a furnace by raising the temperature of the furnace slowly from room temperature to constant weight taken and note the weight(G2).

3.        Calculations:-

Total sulphur (as S) percent = 

Whereas

G1= weight of Gooch crucible (+ filter paper if used)

G2 = Weight of Gooch crucible + barium sulphate precipitate (+ filter paper if used)

W= Weight of sample

Factor 13.74= Per cent total sulphur (w/w) in barium sulphate = 32 × 100/233.39

34. Method of analysis of Phospho Gypsum

1.        Determination of calcium as calcium Sulphate Dihydrate in Phospho Gypsum

(i)       Standarisation of calcium solution-as per method specified in 21A (b)

(ii)      Procedure:-

(a)      Take 1 gram of sample in 250 ml dry beaker. Add 50 ml dilute Hydrochloric acid (1:1)

 

(b)      Boil for 5 minutes on slow heater and cool to room temperature. Add 50 ml distilled water.

 

(c)      Transfer the solution in 250 ml volumetric flask and make the volume to 250 ml with distilled water.

 

(d)      Take 25 ml aliquot in 250 ml washed conical flask and 20 ml distilled water and 20 ml buffer solution. Add few drops of indicator and tighted with EDTA solution till blue color is obtained. Note the volume of EDTA used as V2.

Note:- if the solution is not clear after digestion filter it and then take aliquot.

2.        Calculation:-

Calcium (as Calcium Sulphate Dihydrate) per cent.= V2 X Calcium titer X 3. 4 X 1.]

[163][35. Method of analysis of potash Fortified Silicon by Spectrophotometer

I.         Determination of Silicon as Si (OH)4.

A.        Reagents:

(1)     Silicon Standard Solution (1000 ppm):--

Take 7.5534 gm of Na 2SiO₃.5H₂O in 1000 ml of volumetric flask and dissolve in 100 ml distilled water and make the volume to 1000 ml with distilled water. From 1000 ml standard solution take 10 ml in 100 ml volumetric flask and dilute to the mark with distilled water. Prepare 1 ppm, 2 ppm, 3 ppm and 4 ppm working standard solution in 100 ml volumetric flask accordingly.

(2)     Tartaric Acid Solution:-

Dissolve 50 gram tartaric acid in water and dilute to 500 ml. Store in plastic bottle.

(3)     Ammonium Molybdate Solution:-

Dissolve 7.5 gm Ammonium Molybdate (NH₄)₆ M07 O24 4H2O) in 75 ml water, add 10ml H₂SO₄(1:1) and dilute to 100 ml with distilled water and Store in plastic bottle.

(4)     Reducing Solution:-

Dissolve 0.7 gm Na₂SO₃ in 10 ml water and add 0.15 gm 1-Amino-2-Naphthol-4-Sulphonic Acid. Stir until dissolved. Dissolve 9 gm NaHSO₃ in 90 ml distilled water, add to first solution and mix properly. Store in plastic bottle.

B.        Preparation of Sample Solution.

(1)     Grind requisite quantity of Sample and dry at 105-degree C for two hours.

 

(2)     Place 0.2-0.5 gm sample in 75 Nickel Crucible.

 

(3)     Mix 0.3 gm KNO3 with sample and add 1.5 gm NaOH pellets.

 

(4)     Cover the crucible with Nickel cover and heat to 5 minutes at dull redness over gas flame (do not fuse in furnace).

 

(5)     Remove the crucible from flame and swirl melt around sides.

 

(6)     Cool and add 50 ml distilled water and warm to disintegrate fused cake.

 

(7)     Transfer the material to 150 ml plastic beaker containing 15 ml 5N HClO4 (perchloric acid).

 

(8)     Scrub crucible and lid and wash any residue (with warm distilled water) into beaker.

 

(9)     Transfer it into 250 ml volumetric flask and dilute to volume.

 

(10)   Dilute this sample solution for spectrophotometric analysis accordingly.

C.        preparation of Standard Curve.

(1)     Prepare working standard solution of different strength in 100ml volumetric flask as the like 1 ppm, 2ppm, 3 ppm and 4 ppm and blank solution. Add 1 ml Ammonium Molybdate solution with swirling. Mix well and let it stand for 10 minutes then add 4 ml tartaric acid solution with swirling and mix well. Add 1 ml reducing solution with swirling. dilute to volume with distilled water. Mix well let it stand for thirty minutes.

(2)     Take the absorbance of standard Si solution against blank at 650 nm. Follow same procedure for sample solution and calculate the Si percentage in sample.

Calculation:-

(i)       % Si = X x DF x 10-4

X = Concentration of sample in ppm

(ii)      % of Silica as Si (OH)₄ =% Si x CF

Note:- All the plastic wares are to be used during the analysis.

II.       Determination of Potash

Determination of water Soluble K₂O by the method as specified in 5 (ii) under The said order.]

[164][36. Method of analysis Chelated Manganese as Mn-EDTA:-

A.        Reagents:

(i)       Glass distilled water or demineralized water of pH 2.5+/- 0.5:-Dilute l ml of 10% H2SO4 to one litre with glass distilled water or demineralized water and adjust the pH to 2.5 with a pH meter using 10% H2SO4 or NaOH.

(ii)      Di Sodium EDTA solution :- Dissolve 0.73 gm of di sodium EDTA di hydrate indistilled water and make volume to 100 ml.

B.        Preparation of standard Manganese metal stock solution [1000ppm]:

(i)       Dissolve 1.0 gm of Manganese metal in 50 ml of conc. Hydrochloric acid and make volume to 1000 ml with distilled water. This is 1000 ppm Manganese stock solution.

(ii)      Intermediate solution (100 ppm):- Pipette 10 ml of Manganese stock solution and 10 ml of Di sodium EDTA solution in 100 ml of volumetric ?ask and dilute to volume with distilled water.

(Note:- In case the metal stock solution is not exactly 100.0 ppm, the exact titer value of di sodium EDTA required to chelate the metal has to be added.)

(iii)     Working Standard Solution:- Pipette following volumes of 100 ppm intermediate solution in 100 ml Volumetric ?ask and make volume with acidi?ed water.

C.        Preparation of sample solution for Chelated Manganese:

(i)       Weigh 1.0 gm of sample and transfer into 100 ml volumetric ?ask and make volume with distilled water. Pipette out 1.0 ml of sample solution and dilute further to make second dilution of 100 m1 with distilled water, pipette 5 ml from second dilution and make volume to 50 ml with acidi?ed water to get the above flaming range from 1.0-4.0 ppm.

(ii)      Flaming the solutions:- Flame the standards and the sample of Chelated Manganese on atomic absorption spectrophotometer at a wavelength of 279.5nm (Mn line of instrument ) using air-acetylene flame.

(iii)     Prepare a blank solution from which only the sample has been omitted. Flame along with standards and sample.

D.       Calculations:- Prepare a standard curve of 1‹nown concentration of Manganese solutions by plotting the absorbance value on Y-axis against their respective concentrations on X-axis.

Part-I :- Determination of Total Manganese content in Chelated Manganese sample:- Total Mn content = Concentration of Mn in ppm obtained after flaming the solution X 10

Part-II :- Determination of Free Manganese content in Chelated sample:-

Reagents:- 0.02 M Disodium salt of EDTA- 0.7444 gm of Disodium Salt of EDTA in 100 ml of distilled water. Standardize with 0.02 M standard Zinc or Manganese Metal solution.

(i)       Hydroxylamine Hydrochloride - 0.1-0.2 gm;

(i)       Trietanolamine - 1-2 m1

(ii)      Buffer solution of pH - 10.0;and

(iii)     Indicator Eriochrome black T (EBT) powder.

Take 10 ml of aliquot from stock dilution of sample (1.0 g in 100 ml) Add to it 0.1 g Hydroxylamine HCl,  1to 2 ml of triethanolamine, 10 ml bu?er of pH 10.0, EBT indicator and titrate against 0.02 M disodium EDTA solution.

% Free Manganese=Titration value of EDTA x Atomic weight of Mn metal Molarity of EDTA x 1

% Chelated Manganese content = % Total Manganese - % Free Manganesecontent

37. Method of analysis of Chelated Calcium as Ca EDTA:-

A.        Reagents:-

(i)       Glass distilled water or demineralized water of pH 2.5+/- 0.5:-

Dilute l ml of 10% H2SO4 to one litre with glass distilled water or demineralized water and adjust the pH to 2.5 with a pH meter using 10% H2SO4 or NaOH.

(ii)      Di sodium EDTA solution:- Dissolve 0.73 gm of di sodium EDTA di hydrate indistilled water and make volume to 100 ml.

(iii)     Strontium Chloride (SrCl2 .6H2O )- 15.0 gm in 0.5N HCl and dilute to 100 ml.

B.        Preparation of Standard stock solution of Calcium 1000 ppm.-

(i)       Dissolve 2.498 gm CaCO3 in a minimum amount of 3 N HCl. Dilute to 1000 ml with distilled water. This is 1000 ppm calcium stock solution.

(ii)      Intermediate solution [100 ppm].- Pipette 10 ml of Calcium stock solution and 50 ml of Disodium EDTA solution in100 ml volumetric flask and dilute volume with distilled water.

(Note:- In case the metal stock solution is not exactly 100.0ppm, the exacttiter value of disodium EDTA required to chelate the metal has to be added.)

(iii)     Working Standard solution.- Pipette following volumes of 100 ppm intermediate solution in 100 ml Volumetric ?ask and make volume with acidi?ed water.

C.         Preparation of sample solution for Chelated Calcium.

(i)       Weigh 1.0 gm of sample and transfer into 100 ml volumetric ?ask and make volume with distilled water. Pipette out 5.0 ml of sample solution and dilute further to make second dilution of 100 ml with distilled water, pipette 10.0 ml from second dilution and make volume to 100 ml with acidi?ed water to get the above flaming range from 5.0-20.0 ppm.

(ii)      Flaming the solutions.

Flame the standards and the sample of Chelated Calcium on Atomic Absorbption Spectrophotometer at a wavelength of 422.7 nm (Ca line of instrument) using air-acetylene flame.

(iii)     Prepare a blank solution from which only the sample has been omitted. Flame along with standards and sample.

D.       Calculations.- Prepare a standard curve of known concentration of Calcium solutions by plotting the absorbance value on Y-axis against their respective concentrations on X- axis.

Part-I :- Determination of Total Calcium content in Chelated Calcium sample:-

Total Ca content = Concentration of Ca in ppm obtained after flaining the solution X 2

Part-II :- Determination of Free Calcium in Chelated sample:-

(i)       Reagents:- 0.02 M Disodium salt of EDTA- 0.7444 gm of Disodium Salt of EDTA in 100 ml of distilled water. Standardize with 0.02 M standard Zinc and Manganese Metal solution.

(ii)      Buffer solution of pH - 10.0

(iii)     Indicator Eriochrome black T (EBT) powder,

(iv)    Take 10 ml of aliquot from stock dilution of sample (1.0 g in 100 ml) Add to it 0.1 g

Hydroxylamine HCl, 1 to 2 ml of triethanolamine, 10 ml bu?er of pH 10.0, EBT indicator and titrate against 0.02 M disodium EDTA solution.

% Free Calcium = Titration value of EDTA x Atomic weight of Ca metal x Molarity of EDTA x 1

% Chelated Calcium content = % Total Calcium - % Free Calcium content

38. Method of analysis of Chelated Magnesium as Mg-EDTA:-

A.        Reagents.

(i)       Glass distilled water or demineralized water of pH 2.5+/- 0.5. -

Dilute 1ml of 10% H2SO4, to one litre with glass distilled water or demineralized water and adjust the pH to 2.5 with a pH meter using 1 0% H2 SO4 or NaOH.

(ii)      Di sodium EDTA solution:- Dissolve 0.73 gm of di sodium EDTA di hydrate indistilled water and make volume to 100 ml.

B.        Preparation of Standard stock solution of Magnesium 1000 ppm.

(i)       Dissolve 1.0 gm of magnesium metal in 30 ml of 1:1 HCl and dilute to 1000 ml involumetric flask with distilled water. This is 1000 ppm magnesium stock solution.

(ii)      Intermediate solution {100 ppm].

Pipette 10 ml of magnesium stock solution and 20 ml of Disodium EDTA solution in 100 ml volumetric flask and dilute volume with distilled water.

(Note:- In case the metal stock solution is not exactly I 00 ppm, the exact titer value of disodium EDTA required to chelate the metal has to be added.)

(iii)     Working Standard solution :- 

Pipette following volumes of 100 ppm intermediate solution in 100 ml Volumetric flask and make volume with acidified water.

C.        Preparation of sample solution for Chelated Magnesium:

(i)       Weigh 1.0 gm of sample and transfer into 100 ml volumetric ?ask and make volume with distilled water. Pipette out 2.0 ml of sample solution and dilute further to make second dilution of 100 ml with distilled water, pipette 1.0 ml from second dilution and make volume to 100 ml with acidi?ed water to get the above flaming range from 0.1-0.25 ppm.

(ii)      Flaming the solutions:- Flame the standards and the sample of Chelated Magnesium on atomic absorption spectrophotometer at a wavelength of 285.2 rim (Mg line of instrument) using air-acetylene.

(iii)     Prepare a blank solution from which only the sample has been omitted. Flame along with standards and sample.

D.       Calculations:

Prepare a standard curve of known concentration of Magnesium solutions by plotting the absorbance value on Y-axis against their respective concentrations on X-axis.

Part-I :- Determination of Total Magnesium content in Chelated Magnesium sample.-

Total Mg content = Concentration of Mg in ppm obtained after flaming the solution X 50

Part-II - Determination of Free magnesium in Chelated sample:-

(i)       Reagents:- 0.02 M Disodium salt of EDTA- 0.7444 gm of Disodium Salt of EDTA in 100 ml of distilled water. Standardize with 0.02 M standard Zinc and Manganese Metal solution.

(ii)      Buffer solution of pH - 10.0

(iii)     Indicator Eriochrome black T (EBT) powder

(iv)    Take 10 ml of aliquot from stock dilution of sample (1.0 g in 100 ml) Add to it 0.1 gram Hydroxylamine HCl, 1to 2 ml of triethanolamine, 10 ml bu?er of pH 10.0, EBT indicator and titrate against 0.02 M disodium EDTA solution.

% Free Magnesium=Titration value of EDTA x Atomic weight of Mg metal x Molarity of EDTA x 1

% Chelated Magnesium content = % Total Magnesium - % Free Magnesiumcontent

39. Determination of Chelated Copper as Cu-EDTA:-

A.        Reagents:-

(i)       Glass distilled water or demineralized water of pH 2.5+/- 0.5:-

Dilute l mI of 10% H2SO4 to one litre with glass distilled water or demineralized water and adjust the pH to 2.5 with a pH meter using 10% H2SO4 or NaOH.

(ii)      Di sodium EDTA solution:- Dissolve 0.73 gm of di sodium EDTA di hydrate in distilled water and make volume to 100 ml.

B.        Preparation of Standard stock solution of Copper 1000 ppm.

(i)       Dissolve 1.0 gm of Copper turnings in 30 ml of 1:1HNO3 and dilute to 1000 ml in volumetric flask with distilled water. This is 1000 ppm copper stock solution.

(ii)      Intermediate solution [100 ppm].-Pipette 10 ml of Copper stock solution and 10 ml of Disodium EDTA solution in100 ml volumetric flask and dilute volume with distilled water.

(Note:- In case the metal stock solution is not exactly 100.0 ppm, the exact titer value of disodium EDTA required to chelate the metal has to be added.)

(iii)     Working Standard solution :- Pipette following volumes of 100 ppm intermediate solution in 100 ml Volumetric flask and make volume with acidified water.

C.        Preparation of sample solution for Chelated Copper:

(i)       Weigh 1.0 gm of sample and transfer into 200 ml volumetric ?ask and make volume with distilled water. Pipette out 2.0 ml of sample solution and dilute further to make second dilution of 100 m l with distilled water, pipette 10.0 ml from second dilution and make volume to 100 ml with acidi?ed water to get between the above flaming range from 0.5-2.0 ppm.

(ii)      Flaming the solutions:- Flame the standards and the sample of Chelated Copper on atomic absorption spectrophotometer at a wavelength of 324.8 nm (Cu line of instrument ) using air-acetylene flame.

(iii)     Prepare a blank solution from which only the sample has been omitted. Flame along with standards and sample.

D.       Calculations:

Prepare a standard curve of known concentration of Copper solutions by plotting the absorbance value on Y-axis against their respective concentrations on X-axis.

Part-I :- Determination of Total Copper content in Chelated Copper sample:-

Total Cu content = Concentration of Cu in ppm obtained after ?aming the solution X10

Part-II :- Determination of Free Copper in Chelated sample:-

(i)       Reagents:- 0.02 M Disodium salt of EDTA- 0.7444 gm of Disodium Salt of EDTA in 100 ml of distilled water. Standardize with 0.02 M standard Zinc/Manganese Metal solution.

(ii)      Acetate buffer (pH= 2.8) - 4.0 gm of Sodium acetate trihydrate + glacial acetic acid 155 ml make volume to 1000 ml.

(iii)     Methanolic PAN Indicator:- 0.2 gm of PAN indicator in 10 ml of methanol.

Take 20 ml of aliquot from stock dilution of sample (1.0 g in 200 ml). Add 10 ml acetate bu?er of pH

2.8 and PAN indicator solution and titrate against 0.02 M disodium EDTA solution. End point is Magenta red to yellowish green.

% Free Copper=Titration value of EDTA x Atomic weight of Cu metal x Molarity of EDTA x 1

% Chelated Copper content = % Total Copper - % Free Copper content

40. Estimation of Zinc Content in Chelated Zinc as Zinc Glycine by AAS

E. Principle:-

The total Zinc in Zinc-Glycine is extracted by wet digestion (as Zinc) and estimated by using Atomic Absorption Spectrophotometer.

1.        Instruments / Equipments / Glasswares:-

(i)           Atomic Absorption Spectrophotometer;

(ii)         Hot Plate;

(iii)       Analytical Balance weight least count 0.1 mg; and

(iv)       Required Glasswares.

2.        Reagents and Chemicals:

(i)           Zinc Metal (pure);

(ii)         Nitric Acid (AR Grade conc.);

(iii)       Sulphuric Acid (AR Grade conc.);

(iv)       Perchloric Acid (AR Grade - 70%); and

(v)         Tri Acid Mixture (10 part of Nitric Acid + 01 part of Sulphuric Acid + 04 parts of Perchloric Acid).

3.        Procedure:

(a)      Preparation of Standard Solutions:

(i)       Preparation of 1000 ppm Standard Solution of Zinc - Weigh accurately 500 mg of Zinc metal and dissolve in 10 ml conc. Hydrochloric Acid and make the volume to the volume of 500 ml with distilled water; and

(ii)      Preparation of Working Standard Solution - Take 1 ml, 2ml, 5 ml, 8 ml, 10 ml aliquot of 100 ppm standard solution in di?erent 100 ml volumetric ?asks and add 2 ml nitric acid in each volumetric ?ask and dilute to volume using distilled water.

(iii)     These solutions will be of 1.0, 2.0, 5.0, 8.0 and 10.0 ppm respectively.

(b)      Preparation of Sample Solution.

(i)       Take 1.0 gm sample of Zinc Glycine weighed in 250 ml Erlenmeyer (Conical) flask;

(ii)      Add 10 ml of Tri acid mixture (10 part of Nitric acid : 1 part of Sulphuric acid : 4parts of Perchloric acid);

(iii)     Boil the solution at temperature between 150 to 200oC on hot plate till the solution is clear and reduce the volume till transparent fumes appears;

(iv)    Then remove the solution from hot plate, cool it and make up the volume to 250 ml with distilled water;

(v)      Take 5 ml aliquot in 250 ml volumetric ?ask and make the volume with distille dwater; and

(vi)    Run blank solution also to the same level.

(c)      Estimation of Zinc in the sample by AAS. -

Flame the standard solution followed by sample solution at 215.9 nm wavelength.

4.        Calculation:-

Zinc % by weight :-

(S-B) x V x D x 100 / W x 106

Where S = Average of concentration in sample reading in ppm V = Volume of solution

B = Blank reading in ppm D = Dilution

W = Weight of the sample in gm

Note:- Distilled water instead of Milli-Q-Water has been used during analysis of the sample.

41. Estimation of Calcium Content in Chelated Calcium as Calcium Glycine by Atomic Absorption Spectrophotometer.

Principle:-

The total Calcium in Calcium-Glycine is extracted by wet digestion (as Calcium) and estimated by using Atomic Absorption Spectrophotometer.

I.         Instruments / Equipments / Glasswares:

(i)       Atomic Absorption Spectrophotometer;

(ii)      Hot Plate;

(iii)     Analytical Balance weight least count 0.1 mg; and

(iv)    Required Glasswares.

II.       Reagents and Chemicals:

(i)       Calcium Carbonate (Assay 99.5%);

(ii)      Nitric Acid (AR Grade conc.);

(iii)     Hydrochloric Acid (Assay 35.8 - 36.5%);

(iv)    Perchloric Acid (AR Grade - 70%);

(v)      Lanthanum Oxide (Assay 99.0%);

(vi)    Acid Mixture (Nitric Acid 2 parts : Perchloric Acid 1 part) ; and

(vii)   Lanthanum Oxide Solution: 5.86%w/v (58.65 gm of lanthanum oxide, 250 ml Hydrochloric acid and make up the volume 1000 ml with Milli-Q water).

III.     Procedure:

A.        Preparation of Standard Solutions.

(i)       Preparation of 1000 ppm Standard Solution of Calcium - Weigh accurately 2.50 gm of Calcium Carbonate and dissolve in 1000 ml volumetric ?ask and make the volume to 1000 ml with distilled water; and

(ii)      Preparation of Working Standard Solution - Take 0.5 ml, 1.0 ml, 2.0 ml, 3.0 ml, 4.0 ml, 5 ml aliquot of 100 ppm standard solution in di?erent 100 mlvolumetric ?asks and add 10 ml of lanthanum oxide solution in each volumetric ?ask and dilute to volume using distilled water. These solutions will be of 0.5, 1.0,2.0, 3.0, 4.0, 5.0 ppm respectively.

B.        Preparation of Sample Solution.

(i)       Take 1.0 gm sample of Calcium Glycine weighed in 250 ml Conical flask;

(ii)      Add 10 ml of acid mixture;

(iii)     Boil the solution at temperature between 150 to 200°C on hot plate till the solution is clear & reduce the volume till transparent fumes appears;

(iv)    Then remove the solution from hot plate, cool it and add 5 ml Hydrochloric acid and make up the volume to 250 ml with distilled water;

(v)      Take 2 ml aliquot in 250 ml volumetric ?ask and add 25 ml lanthanum oxide solution and make the volume with distilled water; and

(vi)    Run blank solution also to the same level.

C.        ESTIMATION of Calcium in the sample by AAS. -

Flame the standard solution followed by sample solution at 422.67 nm wavelength.

Calculation:- Calcium % by weight :- (S-B) x V x D x 100 / W x 106

Where S = Average of concentration in sample reading in ppm V = Volume of solution

B = Blank reading in ppm D = Dilution

W = Weight of the sample in gm

Note:- Distilled water instead of Milli-Q-Water has been used during analysis of the sample.]

 

FORMS FOR REGISTRATION

EMBLEM

FORM 'A'

[See Clause 8]

FORM OF APPLICATION TO OBTAIN DEALER'S (INDUSTRIAL)*

CERTIFICATE OF REGISTRATION

To,

the Controller (If the application is for industrial dealer's certificate of

registration)

Place ......................... State of .............................

1.        Full name and address of the applicant :

(a)      Name of the concern, and postal address:

(b)      Place of business (Please give exact address):

(i)       for sale

(ii)      for storage

2.        Is it a proprietory/partnership/limited company/Hindu Undivided family concern?

Give the name(s) and address(es) of proprietor/partners/manager/Karta:

3.        In what capacity is this application filed.

(i)       Proprietor

 

(ii)      Partner

 

(iii)     Manager

 

(iv)    Karta

4.        Whether the application is for wholesale or retail or industrial dealership?

5.        Have you ever had a fertiliser dealership registration certificate in the past?

If so, give the following details :

(i)       Registration number

 

(ii)      Place for which granted

 

(iii)     Whether wholesale or retail or industrial dealership.

 

(iv)    Date of grant of registration certificate

 

(v)      Whether the registration certificate is still valid?

 

(vi)    If not, when expired?

 

(vii)   Reasons for non-renewal

 

(viii)  If suspended/cancelled and if so, when

 

(ix)    Quantity of fertilisers handled during last year

 

(x)      Names of products handled

 

(xi)    Name of source of supply of fertilisers.

6.        Was the applicant ever convicted under the Essential Commodities Act, 1955 or any Order issued thereunder including the Fertiliser (Control) Order, 1957 during the last three years preceding the date of application? If so give details.

7.        Give the details of the fertilisers to be handled

SI.No. Name of Fertiliser Source of supply

8.        Please attach certificate(s) of source from the supplier(s) indicated under column 3 of Sl.No.7.

9.        I have deposited the registration fee of Rs...vide Challan No....dated .... in treasury / Bank or enclose the Demand Draft No... datedfor Rs........... drawn on .............................. bank, in favour of..................... payable at........................................................ towards registration fee. (Please strike-out whichever is not applicable).

10.     Declaration :-

(a)      I/we declare that the information given above is true to the best of my/ our knowledge and belief and no part thereof is false.

 

(b)      I/we have carefully read the terms and conditions of the Certificate of Registration given in Form `B' appended to the Fertiliser (Control) Order, 1985 and agree to abide by them.

 

(c)      I/we declare that I/we do not possess a certificate of registration for industrial dealer and that I/we shall not sell fertilisers for industrial use. (Applicable in case a person intends to obtain a wholesale dealer or retail dealer certificate of registration, excepting a State Government, a manufacturer or importer or a pool handling agency).

 

(d)      I/we declare that I/we do not possess a certificate of registration for wholesale dealer or retail dealer and that I/we shall not sell fertilisers for agricultural use. (Applicable in case a person intends to obtain a industrial dealer certificate of registration, excepting a State Government, a manufacturer, importer or a pool handling agency).

Date Signature of the Applicant(s)

Place :

Note :

(1)     Where the business of selling fertilisers is intended to be carried on at more than one place, a separate application should be made for registration in respect of each such place.

 

(2)     Where a person intends to carry on the business of selling fertilisers both in retail and wholesale, separate applications for retail and wholesale business should be made.

 

(3)     Where a person represents or intends to represent more than one State Government, Commodity Board, Manufacturer/Importer or Wholesale dealer, separate certificate of source from each such source should be enclosed.

For use in Office of Controller

Date of receipt : Name and designation of

Officer receiving the Application

EMBLEM

FORM AI

MEMORANDUM OF INTIMATION

[See Clause 8(2)]

1.        Details of the application:

(a) Name of the applicant

(b) Name of the concern

(c) Postal address with telephone number

[165][(d) Mobile number]

2.        Place of business (Please given full address)

(i)       For Sale

(ii)      For Storage

3.        Whether the application is for -

4.        Details of fertiliser and their source in Form 'O'*

(i)       Yes No

(ii)      Yes No

(iii)     Yes No

[Please tick mark whichever is applicable]

5.        I have deposited the registration fee of Rs._______ vide Challan No.__________________ Dated______________________________ in the Bank/ Treasury_________________ or enclose Demand Draft No._____________________________ Dated_____________________________ for Rs._____________________ drawn on in favour of _____________________payable at ______________________________ towards registration fees.

6.        Whether the intimation is for an authorization letter or a renewal thereof. (Note : In case the intimation is for renewal of authorization letter, the acknowledgement in Form A2 should be submitted for necessary endorsement thereon.)

7.        Any other relevant information.

I have read the terms and conditions of eligibility for submission of Memorandum of Intimation and undertake that the same will be complied by me and in token of the same. I have signed the same is enclosed herewith.

Place:

Signature of applicant

Attach a separate sheet if the number exceeds three. Terms and Conditions of authorisation:

(1)     I shall comply with the provisions of the Fertiliser (Control) Order, 1985 and the notification issued thereunder for the time being in force.

 

(2)     I shall from time to time report to the Notified Authority and inform about change in the premises of sale depot and godowns attached to sale depot.

 

(3)     I shall also submit in time all the returns as may be prescribed by the State Government.

 

(4)     I shall not sell fertilisers for industrial use.

 

(5)     I shall file a separate Memorandum of Intimation for, where the storage point is located outside the area jurisdiction of the Notified Authority where the sale depot is located.

 

(6)     I shall file a separate Memorandum of Intimation for each place when the business of selling fertilisers is intended to be carried on at more than one place.

 

(7)     I shall file separate Memorandum of Intimation if I carry on the business of fertilisers both as retail and wholesale dealer.

 

(8)     I confirm that my previous certificate of Registration or Authorisation is not under Suspension or Cancellation or debarred from selling of fertilisers.

DECLARATION

I/we declare that the information given above is true to the best of my/our knowledge and belief and no part thereof is false or no material information has been concealed.

Signature of the Applicant(s)";

Date:

Place:

EMBLEM

FORM `A 2'

ACKNOWLEDGEMENT

[See Clause 8(3)]

1.        Received from M/s _________________ a complete Memorandum of Intimation alongwith Form O, fee of Rs. ________________by Demand Draft bearing number ___________________________ dated __________________ .

2.        this acknowledgement shall be deemed to be the letter of authorisation entitling the applicant to carry on the business as applied for, for a period of 3 years from the date of issue of this Memo of acknowledgement unless suspended or revoked by the competent authority.

Signature of Notified Authority

Dated :

Renewals

Received from M/S. __________________ a complete Memorandum of Intimation alongwith Form O, fee of Rs. _______________by Demand Draft bearing number ___________________________ dated ______________.

2. this acknowledgement shall be deemed to be the letter of authorisation entitling the applicant to carry on the business as applied for, for a period of

3 years from the date of issue of this Memo of acknowledgement unless suspended or revoked by the competent authority.

Dated : Signature of Notified Authority

EMBLEM

FORM 'B'

[See Clause 9]

Book No  Registration No.

Date of Issue

Valid upto

CERTIFICATE OF REGISTRATION TO CARRY ON thE BUSINESS OF SELLING FERTlLISERS AS A *INDUSTRIAL DEALER IN thE STATE OF

, is hereby granted certificate of registration to carry on the business of selling fertilisers in retail/ wholesale/ for industrial use at the place specified below in the State of ____________subject to the terms and conditions specified below and to the provisions of the Fertiliser (Control) Order,

1985.

DESCRIPTION OF thE PLACE AND TYPE OF BUSINESS

Name and style Location of Location Type of Source of by which the sale depot of godowns fertiliser supply business is attached to carried on sale depot

Date : Controller / Registering Authority

Seal : State of

Terms and conditions of certificate of registration:

(1)     this certificate of registration shall be displayed in a prominent and conspicuous place in a part of the business premises open to the public.

(2)     the holder of the certificate shall comply with the provisions of the Fertiliser (Control) Order 1985 and the notification issued thereunder for the time being in force.

(3)     the certificate of registration shall come into force immediately and be valid upto.

Unless previously cancelled or suspended

(4)     the holder of the certificate shall from time to time report to the Registering Authority any change in the premises of sale depot and godowns attached to sale depot.

(5)     the wholesale dealer/retail dealer shall submit a report to the Registering Authority, with a copy to the Block Development Officer or such other officer as the State Government may notify, in whose Jurisdiction the place of business is situated, by the 5th of every month, showing the opening stock, receipts, sales and closing stocks of fertilisers in the preceding month. He shall also submit in time such other returns as may be prescribed by the Registering Authority.

(6)     the Industrial dealer shall submit a report to the Central Government by the 15th of April for the preceding year, showing the opening stocks as on 1st of April of the reporting year, sourcewise receipts during the year, sale and closing stocks of fertilisers alongwith the sourcewise purchase/sale price.

(7)     the wholesale or the retail dealer, except where such a dealer is a State Government, a manufacturer, importer or a pool handling agency, shall not sell fertilisers for industrial use and, as the case may be, an industrial dealer for agricultural use.

Note : (a) the original is meant for the holder of the certificate which will be delivered against his proper and adequate acknowledgement. the original certificate of registration shall be torn off at the place perforated while all duplicates shall be kept intact bound in the registration book by the Registering Authority.

(b) Where the business of selling fertilisers is intended to be carried on at more than one place, a separate registration certificate should be obtained in respect of each such place.

(c) Where a person intends to carry on the business of selling fertilisers both in retail and wholesale and, as the case may be, a State Government, a manufacturer, importer or a pool handling agency, also for industrial use, separate registration certificate should be obtained for retail and wholesale business and for sale for industrial use.

EMBLEM

FORM 'C'

[See Clause 11]

APPLICATION FOR RENEWAL OF thE CERTIFICATE OFREGISTRATION TO CARRY ON thE BUSINESS OF SELLING

FERTlLISERS IN RETAIL/WHOLESALE / FOR INDUSTRIAL USE

To,

the Registering Authority/Controller (if the application is for Industrial dealer's certificate of Registration).

Place :

State :

1.        I/we hereby apply for renewal of the certificate of registration to carry on the business of selling fertilisers in retail/wholesale/ for industrial use under the name and style of ___________________________the Certificate of registration desired to be renewed was granted by Registering Authority for the____________________________(mention place and state) and allotted registration certificate No____________________ on the _______________Day of __________ 20________ .

2.        (i) I/we hereby declare that the situation of my/our premises where fertilisers are (a) stored and (b) sold is as stated below:

(ii) I/we hereby declare that the fertiliser(s) in which I/we am/are carrying on the business of selling and the name(s) of manufacturer(s) /importer(s), Commodity Board(s), State Govemment(s) and Wholesale Dealer(s) whom I/we represent are as stated below:

3.        I/we enclose a certificate of source from the manufacturer(s), importer(s), Commodity Board(s), State Government(s), Wholesale Dealer(s) whom I/we represent or intend to represent and from whom fertiliser(s) will be obtained by me/us.

4.        I have deposited the renewal fee of Rs. ___________vide challan No. ____________ dated ___________ in Treasury/Bank ______________ or I enclose the Demand Draft No. ______________dated ___________for Rs. ______________ drawn on _____________ Bank, in favour of __________ payable at _____________________ towards renewal fee (Please strike out whichever not applicable).

Full Name and address of the Signature of applicant(s)

applicant(s) (in block letters)

Date :

Place:

Certified that the certificate of registration bearing number ________________granted on_________ for the period from ___________________to ________________ to carry on the business of selling fertilisers in retail/wholesale/ for Industrial use at the premises situated at ________________is hereby renewed till the ___________ unless previously suspended or cancelled under the provisions of the Fertiliser (Control) Order 1985.

 

EMBLEM

FORM D

[See Clause 14(2), 14(2) (b) and 18(1)]

FORM OF APPLICATION TO OBTAIN A CERTIFICATE OF MANUFACTURE OF PHYSICAL/GRANULATED /SPECIAL MIXTURE OF FERTILISER OR ORGANIC

FERTILISER/BIOFERTILISER

To

The Registering Authority

Place___________________

State of_______________

(1)     Full name and address of the applicant:

 

(2)     Does applicant possess the qualification prescribed by the State Government under sub-clause(1) of clause 14 of the Fertiliser(Control) Order 1985.

 

(3)     Is the applicant a new comer? (say 'Yes' or 'No')

 

(4)     Situation of the applicant's premises where physical/granulated/special mixture of fertilisers/organic fertiliser/biofertiliser will be prepared.

 

(5)     Full particulars regarding specifications of the physical/granulated/special mixture of fertilisers/organic fertiliser/biofertiliser for which the certificate is required and the raw materials used in making the mixture.

 

(6)     Full particulars of any other certificate of manufacture, if any, issued by any other Registering Authority;

 

(7)     How long has the applicant been carrying on the business of preparing physical/granulated/special mixture of fertilisers/organic fertiliser/iofertiliser/mixture of micronutrient fertilisers?

 

(8)     Quantities of each physical /granulated/special mixture of fertilisers/ mixture of micronutrient fertilisers/ organic fertilisers/bio fertilisers (in tonnes) in my/our possession on the date of the application and held at different addresses noted against each;

 

(9)     (i) If the applicant has been carrying on the business of preparing physical/granulated/special mixtures of fertilisers/mixture of micronutrient fertilisers/organic fertiliser/biofertiliser, give all particulars of such mixtures handled, the period and the place (s) at which the mixing of fertilisers was done;

(ii) Also give the quantities of physical/granulated/special mixture of fertiliser/organic fertiliser/ biofertiliser handled during the past calendar year;

(10)   If the application is for renewal, indicate briefly why the original certificate could not be acted on within the period of its validity.

(11)   In case of special mixture of fertilisers

Name and address of the person requiring the special mixture of fertilisers;

Declaration

(a)      I have deposited the prescribed registration certificate fee/renewal fee.

 

(b)      I/we declare that the information given above is true and correct to the best of my/our knowledge and belief, and no part there is false.

 

(c)      I/we have carefully read the terms and conditions of the certificate of manufacture given in Form F appended to the Fertiliser (Control) Order, 1985 and agree to abide by them.

 

(d)      I/we declare that the physical/granulated /special mixture of fertilisers/organic fertiliser/bio fertiliser for which certificate of manufacture is applied for shall be prepared by me/us or by a person having such qualifications as may be prescribed by the State Government from time to time or by any other person under my/our direction, supervision and control or under the direction, supervision and control or person having the said qualification.

 

(e)      I/we declare that the requisite laboratory facility specified by the Controller, under this Order is possessed by me/us.

 

(f)       In case of special mixture of fertilisers:

I am enclosing an attested copy of the requisition made by the purchaser of the special mixture of fertilisers;

Name and address of applicant in block letters:

Date:

Place:

Signature of applicant(s)";

EMBLEM

FORM 'E'

[See Clause 14(2) (b)]

FORM OF APPLICATION TO OBTAIN A CERTIFICATE OF MANUFACTURE FOR SPECIAL MIXTURE OF FERTILISERS

To,

the Registering Authority

Place_______________ State ________________

(1)     Full name and address of the applicant:

 

(2)     Does the applicant possess qualifications prescribed by the State Government under sub-clause (1) of 14 of the Fertiliser (Control) Order, 1985.

 

(3)     Name and address of the person requiring the special mixture of fertilisers:

 

(4)     Particulars of certificate(s) of manufacture already obtained from the same Registering Authority:

 

(5)     Situation of the applicants premises where fertilisers are/will be mixed:

 

(6)     Full particulars regarding specifications of the special mixture of fertilisers required to be manufactured and the materials used in making the special mixture:

 

(7)     I am enclosing an attested copy of the requisition made by the purchaser of the special mixture of fertilisers:

 

(8)     I have deposited the prescribed registration certificate fee:

Declaration :

(a)      I/We declare that the information given above is true and correct to the best of my/our knowledge and belief, and no part thereof is false.

 

(b)      I/we have carefully read the terms and conditions of the certificate of manufacture given in Form "G' appended to the Fertiliser (Control) Order 1985 and agree to abide by them.

 

(c)      I/we declare that the special mixture for which a certificate of manufacture is applied for, shall be prepared by me/us or by a person having such qualifications as may be prescribed by the State Government from time to time or by any other person under my/our direction, supervision and control or under the direction, supervision and control of a person having the said qualifications.

 

(d)      I/we declare that the requisite laboratory facility specified by the Controller under this Order is possessed by me/us.

Name and Address of the applicant(s) Signature of the applicant(s)

in block letters:

Date:

Place:

EMBLEM

FORM F

[See clause 15(2) and 18(2)]

Book No. Certificate No.

Date of issue

Valid upto

CERTIFICATE OF MANUFACTURE IN RESPECT OF PHYSICAL/GRANULATED/SPECIAL

MIXTURE/ORGANIC FERTILISER/BIOFERTILISER

(Name of Manufacture) is hereby given the certificate for manufacture of physical/ granulated/special mixture of fertilizers/organic fertilizer/biofertiliser specified below subject to the terms and conditions of this certificate and to the provisions of the Fertiliser (Control) Order, 1985.

Terms and conditions of this certificate:

(1)     The holder of this certificate shall display the original thereof in a conspicuous place open to the public in a part of the principal's premises in which business of making the physical/ granulated /special mixture of fertilizers/organic fertilizer/biofertiliser is carried on and also a copy of such certificate in similar manner in every other premises in which that business is carried on. The required number of copies of the certificate shall be obtained on payment of the fee thereof.

 

(2)     The holder of this certificate shall not keep in the premises in which he carried on the business of making physical/ granulated/special mixture of fertilizers/organic fertilizer/biofertiliser in respect of which a certificate of registration has not been obtained under the Fertiliser (Control) Order, 1985.

 

(3)     The holder of the certificate shall comply with the provisions of the Fertiliser (Control) Order, 1985 and the notification order and direction, issued there under for the time being in force.

 

(4)     The holder of the certificate shall report forth with to the Registering authority any change in the premises specified in the certificate or any new premises in which he carried on the business of making physical /granulated/special mixture of fertilizers/organic fertilizer/biofertiliser and shall produce before the authority the original certificate and copies thereof so that necessary correction may be made therein by that authority.

 

(5)     The holder of this certificate shall ensure that the physical/granulated/special mixture of fertilizers/organic fertilizer/biofertiliser in respect of which a certificate of registration has been obtained in prepared by him or by a person having such qualifications as may be prescribed by the State Government, from time to time or by any other person under the direction, supervision land control of the holder or the person having the said qualifications.

 

(6)     The certificate and copies thereof, if any, will be machine numbered and delivered against the signature of the holder thereof or his agent on the carbon copy of the certificate which will be kept intact bound in the "Certificate Book" by each Registering Authority.

EMBLEM

[166][FORM-G

[See clause 20C(3)]

APPLICATION FOR INCLUSION OF BIOSTIMULANTS IN SCHEDULE VI

To,

The Controller of Fertiliser

-------------------------

------------------------

(i)       Name of manufacturer along with address of unit where it is located:

 

(ii)      Address of the Registered office of the company:

 

(iii)     Location and full address of storage/godown(s):

 

(iv)    Name and address of the applicant along with his designation, contact number and email ID:

 

(v)      PAN and Adhaar number of the authorized person:

 

(vi)    Name of biostimulant (indicate the category of biostimulant as specified in sub-clause (2) of clause 20C):

 

(vii)   Brand Name:

 

(viii)  In case of importer, following additional information shall be provided:

(a)      country of origin:

(b)      is biostimulant registered under country of origin (provide the copy):

(c)      whether the agronomic efficacy trials and toxicity trials are conducted in the country of origin:

(ix)    Technical details of product:

(x)      Labels and leaflet details:

(xi)    Quantity manufactured and sold during last three years (attach sale document):

Verification:-

I do hereby solemnly verify that to the best of my knowledge and belief the statement given above is correct and complete.

I clearly understand that the certificate of registration is liable to be canceled if any information or data, submitted with application is found incorrect or false at any stage.

Signature of the applicant

FORM-G-1

[See clause 20C(5)]

APPLICATION FOR PROVISIONAL REGISTRATION OF BIOSTIMULANTS

To,

The Controller of Fertiliser

-------------------------

------------------------

(i)       Name of manufacturer [167][or importer] along with address of unit where it is located:

 

(ii)      Address of the Registered office of the company:

 

(iii)     Location and full address of storage/godown(s):

 

(iv)    Name and address of the applicant along with his designation, contact number and email ID:

 

(v)      PAN and Adhaar number of the authorized person:

 

(vi)    Name of biostimulant (indicate the category of biostimulant as specified in sub-clause (2) of clause 20C):

 

(vii)   Brand Name:

 

(viii)  In case of importer, following additional information shall be provided:

(a)      country of origin:

 

(b)      is biostimulant registered under country of origin (provide the copy):

 

(c)      whether the agronomic efficacy trials and toxicity trials are conducted in the country of origin:

(ix)    Technical details of product:

(x)      Labels and leaflet details:

 

(xi)    Quantity manufactured and sold during last three years (attach sale document):

 

(xii)   Date and year when introduced in market:

 

(xiii)  State(s) in which product is sold:

Verification:-

I do hereby solemnly verify that to the best of my knowledge and belief the statement given above is correct and complete.

I clearly understand that the certificate of registration is liable to be canceled if any information or data, submitted with application is found incorrect or false at any stage.

Signature of the applicant

FORM-G-2

[See clause 20C(5)(b)]

(To be issued by the State Government(s))

This is to certify that M/s. is selling biostimulant (Name) brand name prior to the (date of publication of notification) and during last three years,-----metric ton/litre of biostimulant were sold in the state.

This is further certified that no complaint has so far been reported of ill effects or hazardous effects of the said biostimulant on humans as well as on animals or environment.

Director of Agriculture

FORM G-3

[See clause 20C(6)]

(To be issued by Controller)

Certificate of Provisional Registration

M/s. ....... (name) and (address) is hereby given the Certificate of Provisional Registration to manufacture [168][or importer] the biostimulant (Name) under sub-clause (6) of clause 20C of the Fertiliser (Inorganic, Organic or Mixed) (Control) Order, 1985, details of which are as under:--

1.        Name of the bio-stimulant:

 

2.        Brand Name of the bio-stimulant:

 

3.        Location of manufacturing unit:

 

4.        Place of storage:

 

5.        Certificate Registration Number:

The provisional registration shall be valid [169][upto 22nd day of February, [170][2025]].

The provisional registration shall be subject to the following terms and conditions:--

1.        The holder shall manufacture [171][or importer] only the biostimulant for which the registration is provided.

 

2.        The heavy metal content and Pesticide content shall not exceed the limit prescribed under the Order.

 

3.        The holder shall comply with the provisions of the said Order and notification issued thereunder.

 

4.        For selling of biostimulant, the authorization letter shall be obtained from the Notified Authority of the concerned State Government.

 

5.        Any information provided in Form G-1 if found incorrect, or on violation of any terms and conditions, the Controller of Fertiliser shall cancel the provisional registration.]

(Controller)

[172][FORM-G-4

[See clause 20D(3)]

APPLICATION FOR OBTAINING APPROVAL OF NANO FERTILISER UNDER THE FERTILISER

(INORGANIC, ORGANIC OR MIXED) (CONTROL) ORDER, 1985

To,

The Controller of Fertiliser

-------------------------

------------------------

1.        Name of manufacturer:

 

2.        Name of the nano fertiliser:

 

3.        Specifications:

 

4.        Details of Multi locational bio-efficacy trials:

(i)       Name of State Agricultural University/Institute of Indian Council of Agricultural Research:

 

(ii)      Crops:

 

(iii)     Details of locations:

5.        Details of Bio safety/Toxicology trials:

(i)       Whether trials have been conducted as per Department of Bio technology Guidelines on nano technology:

(ii)      Type of trial (as per Department of Bio technology guidelines on nano technology:

(iii)     Name of the NABL accredited laboratory where the trials are conducted:

List of documents attached:

(i)       Agronomic efficacy trials report:

(ii)      Bio-safety/Toxicology trials report:

Authorised Signature
On/or behalf of the ...........

EMBLEM

FORM H

[See Clause 23(1)(b)]

APPLICATION FOR GRANT OF PERMISSION TO SELL NON-STANDARD FERTILISERS

To,

The Notified Authority

State of ___________________________

(1)     Full name and address of the applicant:

(2)     The name of fertilisers in which the applicant has been authorized to carry on business:

(3)     Number and date of authorisation letter granted in favour of the applicant:

(4)     (i) Analysis Report by notified fertiliser control laboratory attached - Yes/No

(ii) The source from which the fertilisers were originally purchased and the period during which they have been held by the applicant.

I enclose a copy of the authorisation letter for dealing in fertilisers already granted to me and I have deposited the prescribed fee for permission to sell non-standard fertilisers.

I certify, that I will comply with the requirements of sub-clause (a) of clause 23 of the Fertiliser (Control) Order, 1985.

Signature of the applicant";

Name and address of applicant in block letters

Date : Place:

EMBLEM

FORM 'I'

[See Clause 23(1)(b)]

AUTHORISATION FOR THE SALE OF NON-STANDARD FERTILISERS

M/s. _______________________________________________is/are hereby permitted to sell the non-standard fertilisers described below subject to the terms and conditions noted hereunder.

Particulars of non-standard fertiliser

(1)     Name of the fertiliser:

(2)     Place of location of the non-standard fertiliser.

Terms and conditions:

(1)     The seller of the non-standard fertiliser described above shall comply with the provisions of sub-clause (a) of Clause 23 of the Fertiliser (Control) Order, 1985.

(2)     The non-standard fertilisers described above shall be sold at a price not exceeding Rs. per metric tonne.

[173][Form 'I-1'

[See clause 23 A]

APPLICATION TO GRANT CERTIFICATE FOR REPROCESSING OF DAMAGED FERTILIZER

To,

The Notified Authority

State of _______

1.        Full name and address of the applicant:

 

2.        The name of fertilizers which is damaged:

 

3.        Whether the material is indigenously manufactured or imported:

 

4.        Name of the Manufacturer/Importer:

 

5.        Name of the dealer with whom the material is stored or location of godown or warehouse where the material is stored:

 

6.        If the material is stored with dealer (wholesaler/retail dealer), provide the number and date of authorisation letter granted in favour of the dealer:

 

7.        Approximate quantity of damaged fertiliser and their number of bags:

 

8.        Address of the plant where the material is to be reprocessed:

 

9.        Whether the damaged material has been segregated:

 

10.     Whether the damaged material is conspicuously superscribed with the word 'Non-Standard' and also whether the "X' mark was marked on the bags of the material.

I enclose a copy of the authorization letter for the dealing in fertilizers already granted to me and I have deposited the prescribed fee for permission to reprocess the fertilizer damaged during storage.

I certify, that I have complied with the requirements of clause 23A of the Fertilizers (Control) Order, 1985 and no subsidy/assistance is availed on this material.

Signature of the applicant

Name and address of applicant in block letters

Form 'I-2'

[See clause 23 A]

CERTIFICATE FOR REPROCESSING OF FERTILISER DAMAGED DURING STORAGE

M/s. (Name of manufacturer/importer)________________ is/are hereby permitted to reprocess the fertiliser damaged during storage described below subject to the terms and conditions noted hereunder:-

1.        Name of the fertiliser:

 

2.        Name of the manufacturer/importer:

 

3.        Name and address of the dealer or godown or warehouse where the material is stored:

 

4.        Quantity of damaged fertiliser permitted to be reprocessed:

 

5.        Address/location of the plant where the material is to be reprocessed:

Terms and Conditions:

(1)     The material shall be moved within one week from the date permission is granted.

 

(2)     The company shall inform the Department of Fertiliser, Ministry of Chemical and Fertilisers/Government of India about reprocessing of fertiliser damaged during storage.

 

(3)     Before selling the same, the company shall ensure its quality/standards.

Date:

Notified Authority.
State of __________

Seal:]

EMBLEM

FORM J

[174][See clause 28(1)(b), 28(1)(ba), 28(1) (bb), 28(1)(bc) and 28(1)(bd)]

FORM INDICATING PARTICULARS OF FERTILISERS/ORGANIC FERTILISERS/BIO-FERTILSIERS SAMPLED

(1)     Name and address of dealer/manufacturer/importer [175][or Marketer]

(1A) Letter of authorisation number

(2)     Date of sampling

(3)     Details of markings on bags from where sample has been taken:

(i)       Type and grade of fertilizer

 

(ii)      Name of dealer/manufacturer/importer

 

(iii)     Batch No. (if applicable) and date of manufacture/import

 

(iv)    Composition

(4)     Date of receipt of the stock by the dealer/manufacture/importer/pool handling agency.

(5)     Code No. of sample

(6)     Stock position of the lot

(7)     Physical condition of fertilizer

(8)     Where samples drawn from open bags or stitched bags

(9)     Name & Address of Fertiliser Inspector drawing sample

Signature & Metallic Seal Impression of Fert. Inspector

Receipt of the dealer

Certified that the sample of fertilizer has been drawn in accordance with the procedure laid down in the Fertilizer (control) Order, 1985 from the stock of my possession and I have signed the test samples in the time of wax sealing. I have also received one test sample out of the three test samples prepared.

EMBLEM

FORM 'J-1'

[See clause 28 (bb)]

FORM INDICATING PARTICULARS OF

ORGANIC FERTILISER/ BIOFERTILISERS SAMPLED

(1)     Name and address of dealer/manufacturer/importer ______________

(1A) Certificate of Registration Number____________________

(2)     Date of sampling_______________________________

(3)     Details of markings of bags from where sample has been taken _________ ________________________________________________________

(i)       Type of organic fertiliser/biofertiliser ______________________

 

(ii)      Name of manufacturer/importer____________________________

 

(iii)     Batch No. (if applicable) and date of manufacture/import________

 

(iv)    Composition ___________________________

(4)     Date of receipt of the stock by the dealer/manufacturer/importer/pool handling agency_______________________________________

(5)     Code No. of sample_____________________________________

(6)     Stock position of the lot__________________________________

(7)     Physical condition of organic fertiliser/biofertiliser ________________

(8)     Whether samples drawn from open bags or stitched bags/with sealed packet_____________________

(9)     Name and Address of organic fertiliser/biofertiliser Inspector drawing sample______________________

For organic fertiliser

Signature and Metallic Seal

impression of Fertiliser Inspector

Receipt of the dealer

Certified that the sample of organic fertiliser/biofertiliser has been drawn in

accordance with the procedure laid down in the Fertiliser (Control) Order, 1985

from the stock in my possession, and I have signed the test samples at the time

of wax sealing. I have also received one test sample out of the three test samples

prepared.

Signature and Seal of

Fertiliser Inspector

Signature of dealer/manufacturer/

importer/pool handling agency

with address

EMBLEM

FORM K

[See clause 30(1)]

MEMORANDUM TO ACCOMPANY FERTILISER/ORGANIC FERTILISER/BIO-FERTILISER SAMPLE FOR

ANALYSIS

No.

From______________________

___________________________

To

Incharge

Fertiliser/ Organic Fertiliser/Bio-fertiliser Quality Control Laboratory

1.        The fertilizer samples as per details given below are sent for analysis:

(1)     Type of the fertilizer, Grade

(2)     Date of sampling__________________

(3)     Physical condition of fertilizer

(4)     Code number of sample

2.        The analysis report may please be forwarded to______________________________________

__________________________________________________________________________________________________________

Signature & Metallic Sea l Impression of Fert. Inspector

Place:

Date:

EMBLEM

FORM 'K-1'

[See clause 30]

MEMORANDUM TO ACCOMPANY ORGANIC FERTILISER/BIOFERTILISER

SAMPLE FOR ANALYSIS

No.

From

________________________________

________________________________

To,

Incharge

Organic fertiliser/Biofertiliser Quality Control Laboratory

1.        the biofertiliser samples as per details given below are sent for analysis:-

(1)     Name of organic fertiliser/biofertiliser _____________________

(2)     Date of sampling______________________________________

(3)     Physical condition of organic fertiliser/biofertiliser ____________

(4)     Code number of sample_________________________________

2.        the analysis report may be forwarded to__________________________

____________________________________________________________

Place:

Date:

Signature and metallic seal

impression of Fertiliser Inspector

EMBLEM

FORM 'L'

[See Clause 30(2)]

ANALYSIS REPORT OF FERTILISER SAMPLE

No.

Government of

(Name of the Laboratory)

Date

To,

the Fertiliser Inspector

………………………..

………………………..

the analysis report of the fertiliser sample forwarded vide your reference

No. …………………….... Dated ………………… is as per details given below :

(1)     Name of fertiliser, grade

 

(2)     Date of sampling

 

(3)     Omitted vide S.O. 49(E) dt.16.01.03

 

(4)     Code No. of sample as indicated by the Inspector

 

(5)     Date of receipt of the sample in the laboratory

 

(6)     Laboratory sample No

 

(7)     Date of analysis of sample

 

(8)     Chemical analysis of fertiliser (on fresh weight basis except in the case of Urea on dry weight basis)

____________________________________________________________________________________

Remarks :- the sample is/is not according to specifications and fails in......................

Signature of the Incharge

Fertiliser Quality Control Laboratory

Copy to :-

Director of Agriculture

EMBLEM

FORM 'L - 1'

(See clause 30 )

ANALYSIS REPORT OF ORGANIC FERTILISER SAMPLE

No.____________________

Government of _________________________

_____________________________________

_____________________________________

(Name of the Laboratory)

Date_____________________

To

the Fertiliser Inspector

____________________________________

____________________________________

the analysis report of the organic fertiliser sample forwarded vide your reference No.______________________________Dated_________________is as per details given below:

(1)     Name of Organic fertilizer

 

(2)     Date of Sampling

 

(3)     Code No. of sample as indicated by the Inspector

 

(4)     Date of receipt of the sample in the Laboratory

 

(5)     Laboratory sample No.

 

(6)     Date of analysis of sample

 

(7)     Analysis of Organic Fertiliser (on fresh weight basis)

(A)     Physical Characteristics -

(i)       Moisture content

 

(ii)      Bulk density

 

(iii)     Particle size

(B)     Chemical Characteristics -

(i)       Total Organic Carbon

 

(ii)      Total Nitrogen

 

(iii)     C:N

 

(iv)    Phosphorus

 

(v)      Potassium

 

(vi)    pH

 

(vii)   Conductivity

(C)     Heavy Metal

(i)       Cadmium

 

(ii)      Chromium

 

(iii)     Copper

 

(iv)    Mercury

 

(v)      Nickel

 

(vi)    Lead

 

(vii)   Zinc

Remarks : the sample is/is not according to specification and fails in__________

Signature of the Incharge

(Testing Laboratory

Copy to:-

Director of Agriculture

EMBLEM

FORM 'L - 2'

[See clause 30]

ANALYSIS REPORT OF BIOFERTILISER SAMPLE

No.

Government of

(Name of the Laboratory)

Date

To

the Fertiliser Inspector

the analysis report of the biofertiliser sample forwarded vide your reference

No.__________________________Dated_________________is as per details given below:

(1)     Name of Biofertiliser

 

(2)     Date of Sampling

 

(3)     Code No. of sample as indicated by by the Inspector

 

(4)     Date of receipt of the sample in the Laboratory

 

(5)     Laboratory sample No.

 

(6)     Date of analysis of sample

 

(7)     Analysis of biofertiliser (on fresh weight basis)

(A)     Physical Characteristics.

(i)       Moisture content

(ii)      Particle size

____________________________________________________________________________________

(B)     Chemical Characteristics

(i)       pH

____________________________________________________________________________________

(C)     Microbial Characteristics

(i)       Viable Cell Count

(ii)      Contamination Level

____________________________________________________________________________________

(D)     Efficiency Characteristics

(i)       Nodulation Test

(ii)      Nitrogen fixed (mg)/g of sucrose consumed

(iii)     Formation of transparent pellicle in semi solid Nitrogen free bromothymol blue media

(iv)    (a) Solubilization zone (mm)

(b) P- phosphorus (%) Spectro-photometer.

____________________________________________________________________________________

Rhizobium, ** Azotobacter, *** Azospirillum, + PSM

Remarks : the sample is/is not according to specification and fails in ___

___________________________________________________________

___________________________________________________________

Signature of the Incharge

(Testing Laboratory)

Copy to:-Director of Agriculture

EMBLEM

FORM 'L - 3'

[See clause 30]

ANALYSIS REPORT OF NON-EDIBLE DE-OILED CAKE FERTILISER SAMPLE

No.

Government of

(Name of the laboratory)

Date

To

the Fertiliser Inspector

the analysis report of the non-edible de-oiled cake fertiliser sample forwarded

vide your reference No. -------------dated---------------------- is as per details given below :

(1)     Name of Non-edible de-oiled cake fertilizer

 

(2)     Date of sampling

 

(3)     Code no. of sample as indicated by the inspector.

 

(4)     Date of receipt of the sample in the laboratory

 

(5)     Laboratory sample No.

 

(6)     Date of analysis of sample

 

(7)     Analysis of non-edible de-oiled cake fertilizer (on fresh weight basis

(A)     Physical Characteristics :

(i)       Moisture content ............................

(ii)      Particle size ...............................

(B)     Chemical Characteristics :

(i)       Total organic carbon

 

(ii)      Total nitrogen

 

(iii)     C:N

 

(iv)    Phosphorus

 

(v)      Potassium

 

(vi)    pH

 

(vii)   Conductivity

 

(viii)  Total ash

 

(ix)    Others

Remarks : the sample is/is not according to specification and fails in Signature of the incharge

(Testing Laboratory)

Copy to :

Director of Agriculture

EMBLEM

FORM 'M'

[See Clause 5]

FORM FOR CASH/CREDIT MEMORANDUM TO BE ISSUED BY thE DEALER/MANUFACTURER/IMPORTER/POOL

HANDLING AGENCY TO thE PURCHASER OF FERTILISERS

ST/CST No……………………….

Sl.No……………………… Date ………………………......

Certificate Registration No. …...........................………………..........…….

Name and Address of Firm : …...………………………………................…

Name and Address of Purchaser : …………………………….……........….

Total :

ST/CST @

G. Total

_______________________________________________________________________

Signature of purchaser

Signature of dealer, etc.

EMBLEM

FORM 'N'

[See Clause 35(1) (a)]

FORM FOR STOCK REGISTER TO BE MAINTAINED BY thE DEALER/ MANUFACTURER/IMPORTER/POOL

HANDLING AGENCY

Page Number : ___________

Name of the Fertiliser :_________________________________________

Date	Opening balance	Receipts During the day	Total	Sales During the day	Closing balance	Remarks	Signature of dealer
1	2	3	4	5	6	7	8

1.        Mention source of supply with bill No. and date

2.        Sl. No. of first and last cash/ credit memo issued

______________________________________________________________________________

Note : the pages of the stock register should be numbered. A Certificate should be recorded by the inspecting authority confirming the pages in the register.

EMBLEM

FORM 'O'

[See Clause 8 and 11]

CERTIFICATE OF SOURCE FOR CARRYING ON thE BUSINESS OF SELLING FERTILISERS IN

WHOLESALE/RETAIL FOR INDUSTRIAL USE

No. __________________ Date of issue ____________________

1.        Particulars of the concern issuing the certificate of source.

(a)      Name and full address

(b)      Status :

(i)       State Government

(ii)      Manufacturer

 

(iii)     Pool handling agency

 

(iv)    Wholesale dealer

 

(v)      Importer

(c)      If manufacturer of mixture of fertilisers, the details of certificate of manufacture of mixture of fertilisers possessed :

(i)       Number

 

(ii)      Date of issue

 

(iii)     Date of expiry

 

(iv)    Grades of mixturers of fertilisers allowed to be manufactured

 

(v)      Authority by whom issued

(d)      Details of certificate of registration :

(i)       Number

 

(ii)      Date of issue

 

(iii)     Date of expiry

 

(iv)    Authority by whom issued

2.        Particulars of the person to whom the certificate of source is being issued

(a)      Name and full address

(b)      Status :

(i)       Wholesale dealer

 

(ii)      Retail dealer

 

(iii)     Industrial dealer

(c)      If holds a valid certificate of registration, the details thereof :

(i)       Number

 

(ii)      Date of issue

 

(iii)     Date of expiry

 

(iv)    Authority by whom issued

(d)      Purpose of obtaining the certificate of source :

(i)       For obtaining a fresh certificate of registration

(ii)      For renewal of the certificate of registration

1.        Details of fertiliser(s) to be supplied :

S.No	Name of fertilisers	Trade mark/Brand name
1	2	3

_________________________________________________________________________________

4.    Declaration : Declared that the fertilisers mentioned above will be supplied conforming to the standards laid down under the Fertiliser (Control) Order, 1985 and, as the case may be, grades/formulations (of mixtures of fertilisers) notified by the Central/State Government and packed and marked in container as provided under clause 21 of the Fertiliser (Control) Order, 1985.

Signature with stamp of the

Authorised Officer

EMBLEM

FORM 'P'

[See Clause 28(1)(b)]

PARTICULARS OF SAMPLE DRAWN

1.        Name and Grade of Fertiliser :

 

2.        Composition :

 

3.        Physical Condition of Fertiliser :

 

4.        Code No. :

 

5.        Date of Sampling :

 

6.        Name & Address of Fertiliser Inspector drawing sample :

Signature and Metallic Seal

Impression of Fertiliser Inspector

Schedule III

[177][See clause (q)]

[178][Part A

SPECIFICATION OF BIOFERTILISER

1.        Rhizobium

2.        Azotobacter

3.        Azospirillum

4.        Phosphate Solubilising Bacteria

5.        Mycorrhizal Biofertilisers

6.        Potassium Mobilising Biofertilisers (KMB)

7.        Zinc Solubilising Bacteria

8.        Acetobacter

9.        Carrier Based Consortia

10.     Liquid Consortia

11.     Phosphate Solubilising Fungal biofertilisers

Part B

TOLERENCE LIMITS OF BIOFERTILIZER

1.        In case of Rhizobium, Azotobacter, Azospirillum Phosphate Solubilising Bacteria, Potash Mobilising Bacteria, Zinc Solubilising Bacteria, the total viable count shall not be less than 1x107   CFU/gm of carrier material in the form of powder or granules or 5x107   CFU/ml in case of liquid formulations.

2.        In case of Consortia, the total viable count shall not be less than 1x107   in case of carrier based and 1x108   in case of liquid formulations.

3.        In case of Mycorrhizal biofertilizers, total viable spores shall not be less than 8/gm of finished product.]

[186][PART C

'PROCEDURE FOR DRAWAL OF SAMPLE OF BIOFERTILISERS -

PROCEDURE FOR SAMPLING OF BIOFERTILIZERS', -

"1. General Requirements of Sampling -

1.0 In drawing, preparing and handling the samples, the following precautions and directions shall be observed.

1.1 Sampling shall be carried out by a trained and experienced person as it is essential that the sample should be representative of the lot to be examined.

1.2 Samples in their original unopened packets should be drawn and sent to the laboratory to prevent possible contamination of sample during handling and to help in revealing the true condition of the material.

1.3 Intact packets shall be drawn from a protected place not exposed to dampness, air, light, dust or soot."

2. Scale of Sampling -

2.1 Lot -

All units (containers in a single consignment of type of material belonging to the same batch of manufacture) shall constitute a lot. If a consignment consists of different batches of the manufacture the containers of the same batch shall be separated and shall constitute a separate lot.

2.2 Batch -

All inoculant prepared from a batch fermentor or a group of flasks (containers) constitute a batch.

2.3 For ascertaining conformity of the material to the requirements of the specification, samples shall be tested from each lot separately.

2.4 The number of packets to be selected from a lot shall depend on the size of the lot and these packets shall be selected at random and in order to ensure the randomness of selection procedure given in IS 4905 may be followed."

"3. Drawal of Samples

3.1 The Inspector shall take three packets as sample from the same batch. Each sample constitutes a test sample.

[187][3.2 Of the sample of biofertilisers drawn by the Inspector, the label affixed therein shall be defaced and a label containing generic name of bio fertilizers or organic fertilisers, expiry date, code number and date of sampling shall be pasted on the upper margin of sample packet/container. The sample shall be kept in cloth bag and be sealed with Inspector seal. The sealed cloth bag containing sample along with form 'P' shall be kept in another cloth bag and be sealed with inspector seal. The identifiable detail such as code number, date of sampling name of biofertiliser shall be put on cloth bag containing biofertiliser with form 'P'.

3.3 Out of three samples collected one sample so sealed shall be sent to Incharge of the laboratory notified by the State Government under clause 29 or the Director, National Centre of Organic Farming at Ghaziabad. In case where the sample is sent to Director National Centre of Organic Farming at Ghaziabad, or his authorized officer shall recode the sample and forward to any of the Regional Centre of Organic Farming at Bengaluru, Bhubaneshwar, Ghaziabad, Imphal, Jabalpur, Nagpur, and Panchkula for analysis. Another sample shall be given to manufacturer or dealer as the case may be. The third sample shall be sent by the inspector to the next higher authority for safe custody. The appellate authority shall be sent any of the latter two samples for referee analysis under sub-clause (2) of clause 29 B.]

3.4 The number of samples to be drawn from the lot

PART D

Method of Analysis of Biofertilisers

[188][1.C. Method of Analysis of Azospirillum Biofertilisers. 

1.        Apparatus: same as Rhizobium

2.        Reagents

3.        Medium

Use N-free semisolid medium (Nfb) of the following composition for preparation of MPN tubes

2.1.1 Trace element solution (g/litre)

 

2.2 Sterilization and preparation of MPN tubes -

2 2.1 Prepare Nitrogen free Bromothymol Blue malate medium as mentioned at paragraph 2.1. Boil to dissolve agar. Quickly dispense 10 ml molten media in 15 x 150 ml test tubes or screw capped culture tubes and close either with cotton plugs or screw caps. Minimum of 25 such tubes shall be needed for each sample.

2.2.2 Sterilize the tubes by autoclaving at 121°C for 20 minutes, as in Rhizobium at paragraph 2.3.2.

3. Preparation of serial dilution for MPN count -

Dispense 30 g of Azospirillum biofertilizers in 270 ml of sterile water and shake for 10 minutes on a reciprocal shaker. Make serial dilutions up to 10-8 dilution. Pipette out 1 ml aliquots of 10-4 to 10-8 dilution and deliver it to screw cap tubes or test tubes containing N-free semi solid Nfb media.

4. Incubation of tubes -

Label the tubes and incubate at 36 ± 1°C for 3-4 days in vertical position in a test tubes stand. Do not disturb the medium during the entire period of incubation.

5. Counting

5.1 Count the tubes which have turned blue and have developed typical transparent sub-surface pellicle.

5.2 Count the tubes as +ve or -ve for the presence of sub-surface pellicle and consider for the purpose of calculation.

5.3 Method for Estimating MPN Count

5.3.1 To calculate the most probable number of organisms in the original sample, select as P1 the number of positive tubes in the least concentrated dilution in which all tubes are positive or in which the greatest number of tubes is +ve, and let P2 and P3 represent the numbers of positive tubes in the next two higher dilutions.

5.3.2 Then find the row of numbers in Table 1 in which P1 and P2 correspond to the values observed experimentally. Follow that row of numbers across the table to the column headed by the observed value of P.

5.3.3 The figure at the point of intersection is the most probable number of organisms in the quantity of original sample represented in the inoculum added in the second dilution. Multiply this figure by the appropriate dilution factor to obtain the MPN value.

5.3.4 Azospirillum count/g of carrier = Value from MPN table* x Dilution level

  ___________________________________

   Dry mass of product

Table 1

*Most Probable Numbers for use with 10 fold dilution and 5 tubes per dilution (Cochran, 1950)

1D. Method of Analysis of Phosphate Solubilising Bacterial Biofertiliser

Determination of Soluble Phosphorus Using Ascorbic Acid

[189][5.33 Procedure

"(i) Preparation of Sample -

Pure culture medium same as at 2.1 above excluding agar.

Prepare broth medium in 100 ml aliquots in 6 no., 250 ml conical flasks and sterilize in autoclave at 121°C for 20 min.

(ii) Inoculation of Medium -

Select one PSB colony of the type that has been counted as PSB (showing sufficient zone of solubilization) and streak on set medium as described at 2.1 in a Petri dish. Use this pure culture for inoculating the broth. Inoculate 3 flasks and keep 3 flasks as uninoculated control. Incubate the flasks over rotary shaker for 12 days at 28 +.1°C. After 12 days, filter the contents of each flask separately through Whatman No. 42 filter paper or centrifuge at 10,000 rpm for 15 min.

(iii) Add 10 ml of filtrate/ centrifugate to 50 ml of olsen extractant and shake for 30 min over rotary shaker.

(iv) Filter the suspension through Whatman filter paper No. 40. If the filtrate is coloured then add a tea spoon of Dacro-60 (activated phosphorous free carbon), reshake and filter.

(v)   Take a known aliquot (5 to 25 ml) of the extract in a 50 ml volumetric flask.

(vi)   Add 5 drops of p-nitrophenol indicator (1.5 per cent solution in water) and adjust the pH of the extract between 2 and 3 with the help of 4NH2SO4. The yellow colour will disappear when the pH of the solution becomes 3. Swirl gently to avoid loss of the solution along with the evolution of CO2.

(vii)  When the CO2 evolution has subsided, wash down the neck of the flask and dilute the solution to about 40 ml.

(viii) Add 5 ml of the sulphomolybdic acid mixed reagent containing ascorbic acid, swirl the content and make up the volume.

(ix)   Measure the transmission after 30 min at 880 nm using red filter. The blue colour developed remains stable upto 60 minutes.

(x)   Record the concentration of phosphorous (P) in the extract form from the standard curve and calculate the concentration of soluble phosphorous as follows:]

1(E). Method of Analysis for Mycorhizal Biofertilisers

[190][(b) Procedure

(i)       Mix 100 gram Mycorrhizal biofertiliser in a substantial volume of water and decant through a series of sieves arranged in descending order of mesh size;

(ii)      Vigorous washing with water is necessary to free spores from aggregates of clay carrier material or organic materials;

(iii)     Roots and coarse debris are collected on coarse sieves (1mm and 450 micron), while spores are captured on all the respective finer sieves (250micron, 100 micron and 40/50 micron);

(iv)    Collect the sieving in jars and view the aliquots for spore count during continuous stirring on magnetic stirrer so that proper separation of spores and carrier could occur (as per suggestions from TERI experts);

(v)      Transfer aliquots from all the finer sieves (250 micron 100 micron and40/50micron) are mixed and observed properly on the gridded Petri dishes or plate under stereomicroscope for total viable spore count; and

(vi)    Count the number of spores in plate/dish and express it as spores or gram of the sample.]

[191][1F. Method of analysis for [192][Potash Mobilising Biofertilisers] (KSB)

Estimation of total viable count and contamination

1.        Apparatus -

1.1 Pippettes graduated 1 ml and 10 ml

1.2 Dilution bottles or flasks

1.3 Petri dishes clear, uniform, flat-bottomed

1.4 Hot -air oven

Capable of giving uniform and adequate temperature, equipped with a thermometer, calibrated to read upto 250øC and with venus suitably located to assure prompt and uniform heating.

1.5 Autoclave

1.6 Incubator

1.7 Hand tally or mechanical counting device

1.8 pH meter

2.        Reagents

2.1 Medium

Use plating medium of the following composition for total viable count and contamination

Medium for analysis of total viable count and contamination (Ingredients g/lit)

Medium for studying zone of solubilization in KSB(Ingredients g/lit)

2.2 Sterilizing and preparation procedure for plates

2.2.1 Sterlize the sampling and plating equipment with dry heat in a hot air oven at less than 160øC for not less than 2 hours;

2.2.2 Sterilize the media by autoclaving at 120øC for 20 min. To permit passage of steam into and from closed containers when auto claved, keep stoppers slightly lossened or plugged with cotton. Air from within the chamber of the sterilizer should be ejected allowing steam pressure to rise.

2.3 Preparation of plating medium and pouring

2.3.1 Prepare growth medium in accordance with the composition of the specific biofertiliser.

2.3.2 Melt the required amount of medium in boiling water or by exposure to flowing steam in partially closed container but avoid prolonged exposure to unnecessarily high temperature during and after melting. Melt enough medium which will be used within 3 h. Re-sterlisation of the medium may cause partial precipitation of ingredients.

2.3.3 When holding time is less than 30 min. promptly cool the molten medium to about 45øC, and store until used, in a water bath or incubator at 43 to 45øC. Introduce 12 to 15 ml of liquefied medium or appropriate quantity depending on size of the petri dish at 42 to 44øC into each plate. Gently lift the cover of the dish just enough to pour in the medium. Sterlise the lips of the medium containers by exposure to flame.

(a)      Immediately before pouring.

(b)      Periodically during pouring, and

(c)      When pouring is complete for each batch of plates, if portions of molten medium remain in containers and are to be used without subsequent sterilization for pouring additional plates. As each plate is poured thoroughly mix the medium with test portions in the petri dish.

2.3.4 By rotating and tilting the dish and without splashing the medium over edge, spread the medium evenly over the bottom of the plate. Provide conditions so that the medium solidifies with reasonable promptness (5-10 min) before removing the plates from level surface.

3.        Preparation of Serial Dilution for Plate Counts:

3.1. Dispense 10 g of inoculants to 90 ml of sterile distilled demineralized water and shake for 10 min on a reciprocal shaker or homogenizer. Make serial dilutions upto 10 Take 1:0 ml or suitable aliquots of 106 to 109 dilutions using sterile pipettes and deliver to petri dishes containing set medium as given in 2.1 and spread it uniformly with a spreader or use droplet method. Invert the plates and promptly place them in the incubator.

4.        Incubation of Plates:

4.1 Label the plates and incubate at 28 N2øC for 4 to 6 days.

4.2 Colony counting aids:

Count the colonies with the aid of magnifying lens under uniform and properly controlled, artificial illumination. Use a colony counter, equipped with a guide plate and rules in centimeter square. Record the total number of colonies with the hand tally. To distinguish colonies from dirt, specks and other foreign matter, examine doubtful objects carefully.

4.3 Count all plates but consider for the purpose of calculation plates showing more than 30 and less than 300 colonies per plate. Disregard colonies which absorb congo red and stand out as reddish colonies. Fraturia aurentia (KMB) stand out as transparent-opaque glistening and domed colonies. Count such colony numbers and calculate figures in terms of per litre, of carrier. Also check for freedom from contamination at 105 dilution.

5.        Counting

Count the total number of colonies on the plates including colonies with solubilisation zone with the help of a colony counter.

6.        Method for estimation of K solubilization zones

6.1 Take 10 g of KSB in 90 ml sterile distilled water

6.2 Make a tenfold dilution series up to 107.

6.3 Take 1.0 ml aliquot of 105 to 107 dilutions using sterile pipettes and deliver to petri dishes containing K-solubilization zone media.

6.4 Spread it uniformly, Invert the plates and incubate for up to 2 weeks at 28 N2øC.

6.5 Count the colonies showing solubilization zones and measure the diameter of solubilization zone. Calculate average zone of solubilization in mm.

[193][7. Method of Analysis for estimation of Potassium solubilisation:

Determination of soluble potash using Flame Photometer

1.        Preparation of Sample

Prepare Aleksandrov broth media comprising of 5.0g glucose; 0.5g MgSO4.7H2O; 0.1g CaCO3; 0.006g FeCl3; 2.0g Ca3(PO4)2; 3.0g potassium aluminium silicate in 1: 1 of distilled water. The pH of this media is adjusted to 7.2+0.2 by using 1 N NaOH. Prepare broth media in 100 ml aliquots in 6 no., 250 ml conical flasks and sterilize in autoclave at 121oC for 20 min.

2.        Inoculation of Media

Select one Potash Mobilising Biofertilisers colony of the type that has been counted as KSB (showing sufficient zone of solubilization) and streak on Aleksandrov agar medium as described above in a Petri dish. Use this pure culture for inoculating the broth. Inoculate 3 flasks and keep 3 flasks as uninoculated control. Incubate the flasks over rotary shaker for 7 days at 30+1oC.

3.        Determination of Soluble K.

(1)     After 7 days, centrifuge the broth at 10,000 rpm for 15 min. Collect the supernatant for estimation of potassium by Flame Photometer.

(2)     Add 1 ml of filtrate/supernatant to 50 ml volumetric flask and make up the volume to 50 ml. Estimate K content by feeding the solution to Flame Photometer. The amount of potassium solubilized is calculated from the standard curve by multiplying the observed value with dilution factor.

4.        Preparation of Standard curve.

(1)     Make a stock solution of 1000 ppm K by dissolving 1.909g. of AR grade potassium chloride (dried at 60oC for 1 h) in distilled water in a 1000 ml volumetric flask; and make up to 1 litre with distilled water. Prepare 100 ppm standard by diluting 100 ml of 1000 ppm stock solution to 1 litre with distilled water.

(2)     Pipette 0.5, 1.0, 1.5 and 2.0 ml of 100 ppm solution into 100 ml volumetric flasks and make up the volume up to the mark. These solutions contain 0.5, 1.0, 1.5 & 2.0 ppm K (mg/Kg) respectively. Plot standard curve using concentrations against flame photometer values.

Express K solubilized as mg/lit of broth]

[194][1G. Method of analysis for Zinc Solubilizing Biofertilizers

2. Estimation of total viable count and contamination

1.        Apparatus -

1.1 Pippettes graduated 1 ml and 10 ml

1.2 Dilution bottles or flasks

1.3 Petri dishes clear, uniform, flat-bottomed

1.4 Hot-air oven - Capable of giving uniform and adequate temperature, equipped with a thermometer, calibrated to read upto 250øC and with venus suitably located to assure prompt and uniform heating.

1.5 Autoclave

1.6 Incubator

1.7 Hand tally or mechanical counting device

1.8 pH meter

2.        Reagents -

2.1 Medium

Use plating medium of the following composition for total viable count and contamination

Medium for analysis of Total Viable Count, Contamination and zone of solubilisation for Zn solubilizing biofertilizer (Ingredients g/lit)

2.2 Sterilizing and preparation procedure for plates:

2.2.1 Sterlize the sampling and plating equipment with dry heat in a hot air oven at less than 160øC for not less than 2 hours;

2.2.2 Sterilize the media by autoclaving at 120øC for 20 min. To permit passage of steam into and from closed containers when auto claved, keep stoppers slightly lossened or plugged with cotton. Air from within the chamber of the sterilizer should be ejected allowing steam pressure to rise.

2.3 Preparation of plating medium and pouring

2.3.1 Prepare growth medium in accordance with the composition of the specific Biofertiliser.

2.3.2 Melt the required amount of medium in boiling water or by exposure to flowing steam in partially closed container but avoid prolonged exposure to unnecessarily high temperature during and after melting. Melt enough medium which will be used within 3 hours. Re-sterlization of the medium may cause partial precipitation of ingredients.

2.3.3 When holding time is less than 30 min. promptly cool the molten medium to about 45øC, and store until used, in a water bath or incubator at 43 to 45øC. Introduce 12 to 15 ml of liquefied medium or appropriate quantity depending on size of the petri dish at 42 to 44øC into each plate. Gently lift the cover of the dish just enough to pour in the medium. Sterlise the lips of the medium containers by exposure to flame.

a.        Immediately before pouring.

b.        Periodically during pouring, and

c.        When pouring is complete for each batch of plates, if portions of molten medium remain in containers and are to be used without subsequent sterilization for pouring additional plates. As each plate is poured thoroughly mix the medium with test portions in the petri dish.

2.3.4 By rotating and tilting the dish and without splashing the medium over edge, spread the medium evenly over the bottom of the plate. Provide conditions so that the medium solidifies with reasonable promptness (5-10 min) before removing the plates from level surface.

3.        Preparation of Serial Dilution for Plate Counts:

3.1 Dispense 10 g of inoculants to 90 ml of sterile distilled de-mineralized water and shake for 10 min on a reciprocal shaker or homogenizer. Make serial dilutions upto 1010 Take 1.0 ml or suitable aliquots of 106 to 109 dilutions using sterile pipettes and deliver to petri dishes containing set medium as given in 2.1 and spread it uniformly with a spreader or used droplet method. Invert the plates and promptly place them in the incubator.

4.        Incubation of Plates:

4.1 Label the plates and incubate-at 28 N2øC for 4 to 6 days.

4.2 Colony counting aids:

Count the colonies with the aid of magnifying lens under uniform and properly controlled, artificial illumination. Use a colony counter, equipped with a guide plate and rules in centimeter square. Record the total number of colonies with the hand tally.

4.3 Count all plates but consider for the purpose of calculation plates showing more than 30 and less than 300 colonies per plate. Disregard colonies which absorb congo red and stand out as reddish colonies. Zinc solubilising biofertilisers stands out as transparent, translucent, glistening and elevated colonies. Count such colony numbers and calculate figures in terms of per litre, of carrier. Also check for freedom from contamination at 105 dilution.

5.        Counting -

Count the total number of colonies on the plates including colonies with solubilization zone with the help of a colony counter.

6.        Method for estimation of Zinc solubilisation zones.

6.1 Take 10 g of ZSB in 90 ml sterile distilled water

6.2 Make a tenfold dilution series up to 107.

6.3 1.0 ml aliquot of 105 to 107 dilutions using sterile pipettes and deliver to petri dishes containing Zinc - solubilization zone media.

6.4 Spread it uniformly, Invert the plates and incubate for up to 2 weeks at 28 N2øC.

6.5 Count the colonies showing solubilization zones and measure the diameter of solubilization zone. Calculate average zone of solubilization in mm.]

[195][7. Determination of soluble Zinc using Atomic Absorption Spectrophotometer

(1)     Preparation of Sample

Prepare Zinc solubilizing broth media comprising of glucose-10.0g; ammonium sulphate-1.0g; potassium chloride-0.2g, dipotassium hydrogen phosphate-0.1g, magnesium sulphate-0.2g and zinc carbonate/zinc oxide 1gm in 1:1 of distilled water. The pH of this media is adjusted to 7.0 by using 1 N NaOH. Prepare broth media in 100 ml aliquots in 6 no., 250 ml conical flasks and sterilize in autoclave at 121oC for 20 min.

(2)     Inoculation of Media

Select one ZnSB colony of the type that has been counted as ZnSB (showing sufficient zone of solubilization) and streak on ZnSB agar media as described above in a Petri dish. Use this pure culture for inoculating the broth. Inoculate 3 flasks and keep 3 flasks as uninoculated control. Incubate the flasks over rotary shaker for 7 days at 30+1oC.

(3)     Determination of Soluble Zinc.

(a)  After 7 days, centrifuge the broth at 10,000 rpm for 15 min. Collect the supernatant for estimation of solubilized Zinc.

(b)  Add 1 ml of filtrate/supernatant to 50 ml volumetric flask and make up the volume to 50 ml. Estimate Zn content by feeding the solution to Atomic Absorption Spectrophotometer. The amount of zinc solubilized was estimated by subtracting the soluble zinc of the inoculated sample from the uninoculated control.

(c)  Standard curve should be made by diluting 0.5, 1.0, 1.5, 2.0 and 3.0 ml of 100ppm standard stock solution (commercially available) of Zinc Sulphate with doubled distilled water in volumetric flasks and make up the volume to 100ml to obtain standards having concentrations of 0.5, 1.0, 1.5, 2.0, 3.0 ppm.

(d)  The amount of zinc solubilized is calculated from the standard curve by multiplying the observed value with dilution factor (50).

Express Zn solubilized as mg/lit of broth.]

[196][1 H Methods of analysis for Acetobacter (spp).

1.        Appartus-As specified in the Method of Analysis of Rhizobium at serial number 1. A.

2.        Reagents.

2.1 Medium: Use plating medium of the following composition for total viable count and contamination:-

Medium for analysis of total viable count and contamination (ingredients gram/litre)

3.        Sterilising and preparation procedure for plates

(Same as specified in the Method of Analysis of Rhizobium)

3.1 Preparation of plating medium and pouring

(Same as specified in the Method of Analysis of Rhizobium.)

4.        Preparation of serial dilutions for plate counts

(Same as specified in the Method of Analysis of Rhizobium)

5.        Incubation of plates

(Same as specified in the Method of Analysis of Rhizobium)

5.1 Colony counting Aids

Count the' colonies with the aid of magnifying lens under uniform and properely controlled, artifical illumination. Use a colony counter, equipped with guide plate and rules in centimeter square. Record the total number of colonies with hand tally. Avoid mistaking particles of undissolved medium or precipitated matter in plates for pin point colonies. To distinguish colonies from dirt, specks and foreign matter, examine doubtful objects carefully

5.2 Count all plates but consider for the purpose of calculation only those plates showing more than 30 and less than 300 colonies per plate. Acetobacter a nitrogen fixing bacteria stand out as irregular 2-3 mm diameter, smooth flat with bright yellow or yellow with orange centre colour. Count such colony numbers and calculate figures in terms of per litre, of carrier. Also check freedom from contamination at 105.

6.        Test for confirmation.

1.        Appartus (same as specified in the Method of Analysis of Azospirillum at serial number 1C).

2.        Reagent.

2.1 Medium (semi solid for pellicle formation) (ingredients gm per liter)

3.        Sterilization and preparation of MPN tubes

(Same as specified in the Method of Analysis of Azospirillum at serial number 1C)

4.        Preparation of serial dilution for MPN count

(Same as specified in the Method of Analysis of Azospirillum at serial number 1C)

5.        Incubation of tubes

(Same as specified in the Method of Analysis of Azospirillum at serial number 1C)

6.        Counting-Yellowish pellicle formation below 1 mm of upper surface of nitrogen free semi solid media. Counting the tubes or plates which have turned yellowish in colour after inoculation and ascertained the presence of pellicle in undistributed medium. To determine usual contamination on the same examine doubtful objects carefully.

7.        Method for Estimating MPN count

Count all tubes which have turned yellowish and consider them for the purpose of calculation. Count such type of tubes and tally this count with MPN table (as specified in the Method of Analysis of Azospirillum at serial number 1C in Table 1) to get the number of cells per gram of carrier or number of cells per ml of liquid.]

[197][1.I. Method of analysis of carrier based Consortia of Biofertiliser and liquid consortia of Biofertiliser

(I)      Methods of Analysis of Rhizobium Biofertiliser - Same as specified for Rhizobium at Serial number 1.A.

(II)     Methods of Analysis of Azotobacter - Same as specified for Azotobacter at serial number 1B

(III)   Methods of Analysis Azospirillum - Same as specified for Azospirillum at serial number 1C

(IV)   Methods of Analysis of Phosphate Solubilising Bacteria PSB - Same as specified for Phosphate Solubilising Bacteria at serial number 1 D

(V)     Methods of Analysis of Potash Mobilising Bacteria (KMB) - Same as specified for Phosphate Solubilising Bacteria at serial number 1 F]

 

SCHEDULE IV

[see clause 2(h) and (q)]

[198][PART - A

1.        City compost:

 

2.        Vermicompost:

3.        [205][Phosphate Rich Organic Manure (PROM)

4.        [206][Organic Manure

Note: The source of organic manure is any of the plant biomass/animal biomass/animal Excreta.]

5.        [210][Bio-enriched Organic Manure

6.        [213][Bone meal, raw

7.        Bone meal, steamed

8.        [214][Potash derived from Rhodophytes

9.        [215][Fermented Organic Manure

[220][Note:- Every manufacturer shall categorically indicate on bags that Fermented Organic Manure shall be added 15-25 days prior to sowing of crop in the field.']

10.    [221][Liquid Fermented Organic manure

[225][Note:-Every manufacturer shall categorically indicate on container that Liquid Fermented Organic Manure shall be added 15-25 days prior to sowing of crop in the field.]

Part- B

TOLERANCE LIMIT OF ORGANIC FERTILISER

[226][A sum total of nitrogen, phosphorus and potassium nutrients shall not be less than 1.5% in City Compost and shall be not less than 2.5% in case of vermicom post]

GRANT OF PERMISSION FOR USE OF FERTILISIER FOR INDUSTRIAL PURPOSE.

The manufacturer of industrial product who intend to use fertilizer as raw material for manufacturing the product may apply to the Central Government in the Proforma I (appended below) along with the recommendation from the State Government/Central Government/ District Industry Centre of the concern State.

PROFORMA - I

Signature of Authorized Signatory

Document to be attached

1.        Application in prescribed proforma.

2.        Certificate from the Chartered Accountant of fertilizer purchase/consum for industrial use.

3.        Recommendation from the State Government/ Central Government/ District Industry Centre of the concerned State Government.

4.        GRANT OF CERTIFICATE OF REGISTRATION FOR SALE OF FERTILISER FOR INDUSTRIAL PURPOSE-

Under Clause 8 of Fertiliser (Control) Order, 1985 for Certificate of Registration is granted for carrying on the business of selling of Fertiliser for industrial purpose.

For this purpose the application is required to be made to Controller of fertilizer in prescribed Form 'A' (appended below) together with fee of Rs. 1500/- and certificate of source in Form 'O' issued by the manufacture of fertilizer.

Currently, the Government of India is granting industrial dealership for sale of Urea only.

[227][PART D

METHODS OF ANALYSIS OF ORGANIC FERTILISERS

1.        Estimation of pH

Make 25 g of compost into a suspension in 50ml of distitled water and shake on a rotary shaker for 2 hours.

Filter through Whatman No. 1 or equivalent filter paper under vacuum using a Buchner funnel.

Determine pH of the filtrate by pH meter.

2.        Estimation of Moisture

Method :

Weigh to the nearest mg about 5 gm of the prepared sample in a weighed clean, dry Petri dish. Heat in an oven for about 5 hours at 65° +. 1° c to constant weigh, Cool in a desicator and weigh. Report percentage loss in weight as moisture content.

Calculation

A = Weight of the Petri dish

B = Weight of the Petri dish plus material before drying

C = Weight of the Petri dish plus material after drying

3.        Estimation of Bulk density

Method

Weigh a dry 100ml cylinder (W 1 gill)

Cylinder is filled with the sample upto the 100 ml mark. Note the volume (VI ml)

Weigh the cylinder along with the sample (W2gm)

Tap the cylinder for two minutes.

Measure the compact volume (V2 ml).

4.        Estimation of Electrical Conductivity

Method

Pass fresh sample of organic fertilizer through a 2-4 mm sieve.

Take 20gm of the sample and add 100ml of distitled water to it to give a ratio of 1:5.

Stir for about an hour at regular intervals.

Calibrate the conductivity meter by using 0.01M potassium chloride solution.

Measure the conductivity of the unfiltered organic fertilizer suspension.

Calculation

Express the results as millimho's or ds/cm at 25°C specifying the dilution of the organic fertilizer suspension viz., 1:5 organic fertilizer suspension.

5.        Estimation of Organic Carbon

Apparatus

(i)       Silica/Platinum crucible 25 g cap.

(ii)      Muffle Furnace

Procedure

Accurately weigh 10 gm of sample dried in oven at 105°C for 6 hrs, in a pre weighed crucible and ignite the material in a Muffle furnace at 650 - 700°C for 6-8 hrs. Cool to room temperature and keep in Desiccator for 12 hrs.

Weigh the contents with crucible

Calculation

Calculate the total organic carbon by the following formulae:-

6.        Estimation of total Nitrogen

As mentioned under Schedule - II, Part-B, 3 (v) of FCO, 1985.

7.        Estimation of C: N Ratio

Method

Calculate the C:N ratio by dividing the organic carbon value with the total nitrogen value.

8.        Estimation of phosphate

Preparation of sample - Accurately weigh 10 gm oven dried sample in 50 g cap. silica crucible and ignite it to 650° - 700°C for 6-8 hrs to obtain ash. Cool and keep in a Dessicator.

Transfer the contents to a 100 ml beaker. Add 30 ml 25% HCl. Wash the crucible with 10 ml 25% HCl twice and transfer the contents to Beaker. Heat over hot plate for 10-15 min. Keep for 4 hrs. Filter through Whatman No. 1 filter paper. Wash with distilled water 4-5 times (till acid free).

Make up the volume of filtrate to 250 ml in a volumetric flask.

Estimate total P by gravimetric quinoline molybdate method as described under Schedule -II, Part B,4(ii)of FCO 1985.

9.        Estimation of Potassium

Flame photometry method:- Total Potassium are usually determined by dry ashing at 650-700 Degree Centigrade and dissolving in concentrated hydrochloric acid. Reagent and Standard curve

(1)     Potassium chloride standard solution: Make a stock solution of 1000 ppm K by dissolving 1.909 g. of AR grade potassium chloride (dried at 60 Degree C. for 1 h) in distilled water 1; and diluting up to 1 litre. Prepare 100 ppm standard by diluting 100 ml of 1000 ppm stock solution to 1 litre with extracting solution.

(2)     Standard curve: Pipette 0,5, 10,15 and 20 ml of 100 ppm solution into 100 ml volumetric flasks and make up the volume upto the mark. The solution contain 0,5, 15 & 20 ppm K respectively.

Procedure:

Take 5g sample in a porceline crucible and ignite the material to ash at 650-700 C in a muffle furnace.

Cool it and dissolve in 5 ml concentrated hydrochloric acid, transfer in a 250 ml beaker with several washing of distilled water and heat it. Again transfer it to a 100 ml volumetric flask and make up the volume.

Filter the solution and dilute the filtrate with distilled water so that the concentration of K in the working solution remains in the range of 0 to 20 ppm, if required.

Determine K by flame photometer using the K- filter after necessary setting and calibration of the instrument.

Read similarly the different concentration of K of the standard solution in flame photometer and prepare the standard curve by plotting the reading against the different concentration of the K.

Calculation: Potash (K) %by weight = R X 20 X diluting factor, where R= ppm of K in the sample solution (obtained by extra plotting from stand curve).

10.    Estimation of Cadmium, Copper, Chromium, Lead, Nickel and Zinc

Material Required

1.        Triacid mixture: Mix 10 parts of HNO3 (Nitric acid), 1 part of H2SO4
(Sulphuric Acid) and 4 parts of HClO3 (Perchloric Acid)

2.        Conical flask, 250ml

3.        Hot plate

4.        Whatman filter paper No. 42

5.        Atomic Absorption Spectrophotometer

Processing of sample

Take 5.0 g or suitable quantity of oven dried (105°C) sample thoroughly ground and sieved through 0.2 mm sieve in a conical flask.

Add 30 ml triacid mixture, cover it with a small glass funnel for refluxing. Digest the sample at 200°C on a hot plate till the volume is significantly reduced with a whitish residue.

After cooling, filter the sample with Whatman No. 42 filter paper, make up to 100 ml in a volumetric flask.

Preparation of working standards

Cadmium - As mentioned under Schedule - II, Part B, 8(x) of FCO (1985)

Copper - As mentioned under Schedule - II, Part B, 8(iv) of FCO (1985)

Chromium - Dilute 1, 2, 3 and 4 ml of standard 199 ppm Chromium standard solution with doubled distilled water in volumetric flasks and make up the volume to 100 ml to obtain standards having concentrations of 1, 2, 3, 4 ppm

Lead - As mentioned under Schedule - II, Part B, 8(v) of FCO (1985) Nickel - Dilute 1,2,3 and 4 ml of standard 100 ppm Nickel standard solution with doubled distilled water in volumetric flasks and make up the volume to 100ml to obtain standards having concentrations of 1,2,3,4 ppm

Zinc - As mentioned under Schedule - II, Part B, 8(ii) of FCO (1985)

Measurement of Result

Estimate the metal concentrations of Cd, Cu, Cr, Fe, Pb, Ni, Zn by flaming the standard solution and samples using atomic absorption spectrophotometer (AAS) as per the method given for instrument at recommended wavelength for each element. Run a blank following the same procedure.

Expression of Result

Express the metal concentration as mg/g on oven dry weight basis in 3 decimal units.

(Reference: Manual for Analysis of Municipal Solid Waste (compost): Central Pollution Control Board)."

11.    'Estimation of Mercury

Reagents:

(a)      Concentrated Nitric acid (HNO3)

(b)      Concentrated Sulphuric acid (H2SO4)

(c)      Potassium persulphate (5% solution): Dissolve 50g of K2S2O8 in 1 litre of distilled water.

(d)      Potassium permagnate (5% solution): Dissolve 50g of KMnO4 in 1 litre of distilled water.

(e)      Hydroxylamine sodium chloride solution: Dissolve 120 g of Hydroxyl amine salt and 120 g of sodium chloride (NaCI) in 1 litre distilled water.

(f)       Stannous chloride (20%): Dissolve 20 g of SnCI2 in 100 ml distilled water.

Materials required

(a)      Water bath

(b)      Flameless atomic absorption spectrophotometer or cold vapour mercury analyzer.

(c)      BOD bottle, 300 ml

Processing of sample:

(a)      Take 5g (finely ground but not dried) sample in an oven at a temperature of 105°C for 8 hours for moisture estimation.

(b)      Take another 5g sample (finaly ground but not dried) in a BOD bottle, add to it 2.5 ml of conc. HNO3, 5ml of cone. H2SO4 and 15 ml of 5% KMnO4.

(c)      After 15 minutes add 8 ml of 5% K2S2O8.

(d)      Close the bottle with the lid and digest it on a water bath at 95°C for 2 hours.

(e)      After cooling to room temperature add 5 ml hydroxylamine sodium chloride soln.

Measurement:

Reduction of the digested sample is brought out with 5 ml of 20% SnCl2 immediately before taking the reading, using a cold vapour mercury analyzer.

Expression of results:

Express the mercury concentration as mg/g on oven dry weight basis in 3 decimal units.

(Reference: Manual for Analysis of Municipal Solid Waste (compost). Central Pollution Control Board).

12.    Estimation of Arsenic

Processing of sample - Suspend 10 gm finely ground sample in 30 ml aquaregia (HNO3 + HCl in a ratio of 1:3) in a beaker. Keep on hot plate till moist black residue is obtained (do not dry). Add 5 ml aquaregia and allow to dry on hot plate till residue is moist. Dissolve the residue in 30 ml conc. HCl and filter through Whatman No.1 filter paper in 100 ml volumetric flask. Wash filter paper 3-4 times with double distilled water. Make up the volume to 100 ml. Take 1 ml of this solution in 100 ml volumetric flask, add 5ml conc. HCl and 2 gm KI and make up the volume to 100 ml.

Prepare standards having concentration of 0.05, 0.1 and 0.2 ppm by diluting 0.05, 0.1 and 0.2 ml, respectively of standard Arsenic solution with double distilled water in volumetric flask and make up the volume to 100 ml

Measurement - Estimate Arsenic using vapour generation assembly attached to Atomic Absorption Spectrophotometer as per the procedure given for the instrument.

13.    Pathogenicity Test

Apparatus

1.        Samples of Compost

2.        Lactose Broth of Single and Double Strength

3.        Culture Tubes

4.        Durham Tubes

5.        Bunsen Burner

6.        Sterile Pipettes

7.        Incubator, Autoclaves,

8.        Petri-Plates

9.        Inoculation Loops

Preparation of Culture Media

A.       For Presumptive Test

1.        Lactose Broth

B.       For Confirmative Test

1. Eosine Methylene Blue Agar Media (EMB Media)

C.        For Completed Test

1. Nutrient Agar

Procedures

A.       Presumptive Test

1.        Prepare 12 tubes of lactose broth for each sample and close the tube with cotton plugs/caps and autoclave at 121°C for 20 min.

2.        Fill Durham tubes with sterilized distilled water and keep in beaker and autoclave at 121°C for 20 min.

3.        Suspend 30g of compost sample in 270 ml of sterile distilled water and serially dilute upto 10-4 dilution as per Schedule III, Part D, serial number 3 of FCO (1985)

4.        Suspend 1 ml suspension from 10-1 to 10-4 in 3 tubes for each dilution

5.        Insert distilled water filled Durham tube in inverted position in each tube and close the tube again

6.        Inoculate tubes at 36°C for 24h in incubator

Result

B.       Confirmative Test

Confirmative test is for differentiating the coliforms from non-coliforms as well as Gram negative and Gram positive bacteria. In this test, the EMB agar plates are inoculated with sample from positive tubes producing gas. Emergence of small colonies with dark centres confirms the presence of Gram negative, lactose fermenting coliform bacteria. Sometimes some of the non-coliforms also produce gas, therefore, this test is necessary.

1.        Prepare EMB agar plates with the composition as per the method at Schedule III, Part D, paragraphs 2.3.3 to 2.3.6

2.        Inoculate plates with the help of inoculation loop with streaking of samples showing positive/doubtful tests in the presumptive test

3.        Incubate plates at 30 ± 1°C for 12 h in incubator

4.        Dark centred or nucleated colonies appear which may differentiate between E. coli and E. aerogenes based on size of colonies and metallic sheen

Result

E. coli colonies on this medium are small with metallic sheen, where as E. aerogenes colonies are usually large and lack the sheen.

C. Completed Test

This test is required for further confirmation. Procedure

1.        Pick up a single colony from EMB agar plate

2.        Inoculate it into lactose broth and streak on a nutrient agar slant

3.        Incubate the slants

4.        Perform Gram reaction after attaining the growth

Result

Gram-negative nature of bacteria is indicative of a positive completed test.]

14.    [228][Method of analysis of Bone Meal Raw and Bone Meal Steamed

(i)       Acid insoluble matter:

(a)      Reagent

Dilute Nitric Acid-1:1 (v/v)

(b)      Procedure

Weigh accurately about 2 to 3g of the sample into a crucible and ignite gently until all organic matter is burnt away, leaving behind grey or transparent ash. Cool and extract the residue twice with warm dilute nitric acid. Filter through a filter paper (Whatman No. 40 or equivalent) and wash the residue on the filter paper with water. Dry the residue in an air-oven at 150 + 2oC for one hour. Incinerate the filter paper with the residue to constant weight in a previously weighed crucible, cool in a desiccator and weigh.

(c)      Calculation

Acid-insoluble matter, percent by weight = 

where

W1 = weight in g of the residue, and

W2 = weight in g of the prepared sample taken for the test.

Note: Indian Standard Specification for Bone Meal Raw (Revised), Fourth Reprint April 1998, by Bureau of Indian Standards

(ii)      Total Phosphorus:

(a)      Preparation of sample

Accurately weigh 1g sample and transfer it to 100 ml beaker. Add 30 ml HNO3 and 10 ml concentrated HCl. Heat over hot plate for 10-15 mins or till the brown fumes disappears. Keep for 4 hrs. Filter through Whatman No. 42 filter paper. Wash with distilled water 4-5 times (till acid free). Make up volume of filtrate to 250 ml in a volumetric flask.

(b)      Estimate total P by gravimetric quinoline molybdate method as described under Schedule-II, Part B, 4(ii) of Order, 1985.

(iii)     Citric acid soluble phosphorus:

(a)      Reagents

Citric Acid solution: To dissolve 20g of citric acid in water and make up the volume to 1 litre.

(b)      Preparation of sample

(a)      Accurately weigh 5g of the sample into a 500-ml dry flask. Make up the volume to 500-ml mark with citric acid solution. Close the flask with a suitable stopper, place it at once in rotary shaking apparatus and shake the flask at the rate of 30 to 40 rev/min for 30 minutes. At the end of this period, remove the flask, filter the solution through a dry filter paper (Whatman No. 42) into a clean dry container.

(b)      Estimate P by gravimetric quinoline molybdate method as described under Schedule-II, Part B, 4(ii) of Order, 1985.

(iv)    Nitrogen content of water insoluble portion:

Preparation of sample

Accurately weigh 1g sample into a clean beaker. Stir well with water for a few minutes and filter through a filter paper (Whatman No. 2 or equivalent). Complete the washing until filtrate measures 200-250 ml. Carefully put the filter paper containing the residue into a 500-ml Kjeldahl flask.

Note: Determine N as Schedule-II, Part B, 3 (iv) of Order, 1985.

15.     Potash Derived from Rhodophytes

(i)       Water soluble Potash:

As mentioned for mixed fertilisers under Schedule-II, Part-B, paragraph 5 of Order, 1985.

(ii)      Determination of Sulphate Sulphur

As mentioned under Schedule-II, Part-B, paragraph 24 (A) Procedure (a) of Order, 1985.

(iii)     Determination of elemental sulphur

As mentioned under Schedule-II, Part-B, paragraph 24 (B) of Order, 1985.

(iv)    Total sulphur (as S) (It is the sum of sulphur present in sulphate and elemental form)

As mentioned under Schedule-II, Part-B, paragraph 24 (C) of Order, 1985.]

[229][SCHEDULE V

See clause 2 (h) and (q)

Part -A

Specification of Non-edible De-oiled Cake Fertilizers

[230][Note.-A company can sell the deoiled cake under its source name as Castor, Neem, Karanj (Pongamiapinnata), Mahua (madhucalongifolia) and Jatropha deoiled cake and can also print any specification of nutrient content over and above the minimum specification of nutrient prescribed under the general specifications of Non edible deoiled cake specified in FCO.]

Part-B

TOLERANCE LIMIT OF NON-EDIBLE DE-OILED

CAKE FERTILISERS

0.5 Unit for Nitrogen, Phosphorous and Potassium nutrients combined.

Part- C

PROCEDURE FOR DRAWL OF SAMPLE OF NON-EDIBLE DE-OILED CAKE FERTILISER

The Inspector shall draw any sample of Non-edible de-oiled cake fertilizer in accordance with the procedure of drawl mentioned under Schedule-II, Part-A.

Part- D

METHODS OF ANALYSIS FOR NON-EDIBLE DE-01LED CAKE FERTILIZERS

1.        Estimation of pH

As mentioned in Schedule IV Part D at serial number 1.

2.        Estimation of moisture

As mentioned in Schedule IV Part D at serial number 2.

3.        Estimation of ash Content

(a)      Apparatus

(i)       Silica/Platinum crucible 25 g cap.

 

(ii)      Muffle Furnace

 

(iii)     Desiccator

Weigh to the nearest mg about 5 gm of oven dried powdered sample in a weighed clean, dry Petri Dish. Incinerate in a muffle furnace for about 6-8 hours at 650-700 °C to constant weight. Cool in a dessicator and weigh. Report percentage of ash content obtained.

(b)      Calculation :

Ash content in per cent by weight = 100 x (C-A)/B - A

A = Weight of the empty crucible

B = Weight of the empty crucible plus material before ashing

C = Weight of the empty crucible plus material after ashing

4.        Estimation of conductivity-

As mentioned in Schedule IV Part D at serial number 4.

5.        Estimation of organic carbon-

As mentioned in Schedule IV Part D at serial number 5.

6.        Estimation of total nitrogen

(a)      Apparatus

1.        Suitable Kjeldahl assembly consisting of 500-800 ml round bottom, digestion flask and Kjeldahl distillation assembly consisting of 500-800 ml distillation flask, splash head tube and condenser, all with appropriate glass joints. The length of the condenser's delivery tube should be long enough to keep immersed in a flask for ammonia absorption.

2.        Kjeldahl digestion unit with heating control, suitable for 500-800 ml flasks.

(b)      Reagents

(a)      Sulphuric acid -- 93-98% H₂SO₄, N-free

 

(b)      Salicylic acid, reagent grade, N-free

 

(c)      Sodium thiosulphate (Na₂S₂O₃ 5H₂0), reagent grade

 

(d)      Zinc dust--impalpable powder

 

(e)      Copper sulphate

 

(f)       Potassium or sodium sulphate

 

(g)      Selanium powder

 

(h)     Red Mercury oxide (HgO)

 

(i)       45% NaOH solution. Dissolve 450 gm of Sodium hydroxide pellets in distilled water and make up the volume to 1000 ml

 

(j)       Methyl red indicator -Dissolve 1 gm methyl red in 200 ml alcohol

 

(k)      Hydrochloric or sulphuric acid standard solution -- 0.1 N or as per requirement

 

(l)       Sodium hydroxide standard solution 0.1 N or as per requirement.

(c)      Procedure.

(1)     Place weighed finely powdered sample (0.5 1.0 gm) in digestion flask,

 

(2)     Add 1 gm digestion mixture (20 g CuSO4 + 3 gm selenium dust + 1 gm HgO).

 

(3)     Add 50 ml conc H₂SO₄.

 

(4)     Shake the flask and let it stand for five minutes then heat over low flame until frothing ceases.

 

(5)     Turn off heat, add 15 --20 gm powdered K,SO4 (or anhydrous Na2SO4 ), and boil briskly until solution clears.

 

(6)     Add 5 gm Sodium thiosulphate, continue boiling for another at least 2-3 hours.

 

(7)     Remove from burner and cool, add 200 ml of water and swirl the flask to dissolve all the contents.

 

(8)     Transfer to 500 ml volumetric flask, giving several washings with water to the digestion flask. Make up the volume to 500 ml.

 

(9)     Take 25 ml aliquot in the distillation flask, add 300 ml water and a pinch of zinc dust.

 

(10)   Take 20 ml of standard acid solution (N,10 H2SO4) in the receiving conical flask, add 4 drops of methyl red indicator and keep the flask at the lower end of the condenser in such a way that the lower tip of the condenser is hilly immersed in acid solution.

 

(11)   Add 40 ml of45%NaOH to the distillation flask gently so that the contents do not mix,

 

(12)   Immediately connect the flask to distillation assembly and swirl to mix the contents. Heat until all the ammonia is distilled (at least 150 ml distillate).

 

(13)   Remove from receiving flask. Rinse outlet tube into receiving flask with a small amount of distilled water.

 

(14)   Titrate the contents in the receiver conical flask with standard NaOH solution.

 

(15)   Determine blank on reagents using same quantity of standard acid in receiving conical flask.

(d)      Calculation

Nitrogen % by weight = 1.401(V₁-N₁-V₂N₂)-(V₃N₁-V₄N₂) X df/W

where

V1- Volume in ml of standard acid taken in receiver flask for sample

V2= Volume in ml of standard NaOH used in titrating standard acid in receiver flask after distillation of test sample

V₃= Volume in ml of standard acid taken in receiver flask for blank

V4= Volume in ml of standard NaOH used in titrating standard acid in receiver flask after distillation in blank

N₁ = Normality of standard acid

N₂ = Normality of standard NaOH

W = Weight in gm of sample taken 

df= Dilution factor of sample

7.        Estimation of C:N ratio

Calculate the C:N ratio by dividing the organic carbon value with the total nitrogen value

8.        Estimation of Phosphate

As mentioned in Schedule IV Part D at serial number 8.

9.        Estimation of Potassium

As mentioned in Schedule IV Part D at serial number 9.]

[231][Schedule VI

[See clause 2(ab) and (q) and clause 20C]

Part-A

SPECIFICATIONS OF BIOSTIMULANTS

Part-B

TOLERANCE LIMIT

Part-C

PROCEDURE FOR DRAWAL OF SAMPLES OF BIOSTIMULANTS

1.        General Requirements of Sampling

1.0 In drawing, preparing and handling of samples, the following precautions and directions shall be observed:

1.1 Sampling shall be carried out by a trained and experienced person as it is essential that the sample should be representative of the lot to be examined.

1.2 Samples in their original unopened packets should be drawn and sent to the laboratory to prevent possible contamination of sample during handling and to help in revealing the true condition of the material.

1.3 Intact packets shall be drawn from a protected place not exposed to dampness, air, light, dust or soot.

2.        Scale of Sampling

2.1 Lot;

All units (containers in a single consignment of type of material belonging to the same batch of manufacture) shall constitute a lot. If a consignment consists of different batches of the manufacture, the containers of the same batch shall be separated and shall constitute a separate lot.

2.2 Batch:-All biostimulants prepared simultaneously in the same process constitute a batch.

2.3 For ascertaining conformity of the material to the requirements of the specification, samples shall be tested from each lot separately.

2.4 The number of packets to be selected from a lot shall depend on the size of the lot and these packets shall be selected at random.

3.        Drawal of Samples

3.1 The Inspector shall take three packets as samples from the same batch. Each sample constitutes a test sample.

3.2 Each sample shall be sealed in a cloth bag and be sealed with the Inspector's seal. The sealed cloth bag containing the sample and Form-P shall be kept in another cloth bag which shall also be sealed with the Inspector's seal. Identifiable details such as sample number, code number or any other details shall be put on the cloth bag containing sample and Form-P which enable its identification.

3.3 Out of the three samples collected, one sample so sealed shall be sent to in-charge of the laboratory notified by the State Government under the sub-clause (1C) of clause 29 or any laboratory notified by the Central Government. Another sample shall be given to the manufacturer or importer or dealer, as the case may be. The third sample shall be sent by the Inspector to his next higher authority for keeping in safe custody. Any of the latter two samples shall be sent for reference analysis under sub-clause (2) of clause 29B.

3.4 The number of samples to be drawn from the lot;

Part-D

METHODOLOGY OF TESTING.]

[232][Schedule VII

[(See clause 20D(1)]

GENERAL SPECIFICATIONS OF NANO FERTILISER

1.        Nano Nitrogen

2.        [237][Nano Nitrogen and Phosphorus fertilizer

3.        [238][Nano Phosphorus fertilizer

4.        [239][Nano Zinc

5.        Nano Copper