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CHAPTER 226 - AGRICULTURE (FERTILISERS AND FEED) ACT: SUBSIDIARY LEGISLATION

 

INDEX TO SUBSIDIARY LEGISLATION

Agriculture (Fertilisers) Regulations

Agriculture (Farm Feed) Regulations

 

AGRICULTURE (FERTILISERS) REGULATIONS

[Section 52]

[Currency mentioned in this regulation should be re-denominated as stipulated under S 4 of Re-denomination Act, 2012, read with S 29 of Bank of Zambia Act, 1996.]

Arrangement of Regulations

   Regulation

PART I
PRELIMINARY

   1.   Title

   2.   Application

PART II
REGISTRATION OF PLANT

   3.   Registration of plant and fees

   4.   Register of plant

   5.   Requirements of plant

PART III
ANALYSTS AND LABORATORIES

   6.   Approval of analysts

   7.   Approval of laboratories

   8.   Roll of analysts

   9.   Roll of laboratories

PART IV
SEARCHES AND SEIZURES

   10.   Certificates of authority for inspectors

PART V
SALE OF FARMING REQUISITES

   11.   Statements of analysis for sales in bags, containers, etc.

   12.   Statements of analysis for sales in bulk

   13.   Statements of analysis for sales under trade names, etc.

PART VI
SAMPLING, ANALYSIS AND LIMITS OF VARIATION

   14.   Form of report to be used

   15.   Form of certificate to be used

   16.   Method of taking samples

   17.   Methods of analysis

   18.   Limits of variation

      FIRST SCHEDULE

      SECOND SCHEDULE

      THIRD SCHEDULE

      FOURTH SCHEDULE

      FIFTH SCHEDULE

      SIXTH SCHEDULE

[Regulations by the Minister]

Act 13 of 1994,

SI 476 of 1969,

SI 117 of 1970.

 

PART I
PRELIMINARY

 

1.   Title

These Regulations may be cited as the Agriculture (Fertilisers) Regulations.

 

2.   Application

These Regulations shall apply to any fertiliser as defined in section 2 of the Act.

 

PART II
REGISTRATION OF PLANT

 

3.   Registration of plant and fees

   (1) Applications under Part II of the Act for registration, transfer of registration or renewal of registration of plant shall be made in Form FERT. 4 in the First Schedule, and such application shall be accompanied by the appropriate fees shown in the First Schedule and the Second Schedule to the Act, and be given to the Registering Officer.

   (2) The Registering Officer shall issue a certificate of registration in Form FERT. 5 in the First Schedule.

   (3) The Registering Officer shall issue a certificate of provisional registration in Form FERT. 6 in the First Schedule.

 

4.   Register of plant

The Registering Officer shall keep a register of plant as prescribed in Form FERT. 1 in the First Schedule.

 

5.   Requirements of plant

Any plant within the definition in section 2 of the Act shall be so equipped as to permit the adequate performance therein of the activities described in the application for registration of such plant, to the satisfaction of the Registering Officer.

 

PART III
ANALYSTS AND LABORATORIES

 

6.   Approval of analysis

   (1) For the purposes of the Act, an analyst shall furnish proof to the satisfaction of the Minister that he has competent knowledge of chemistry and of chemical analyses, as applied to fertilisers. Such proof shall in every case comprise documentary evidence that such person holds a certificate or diploma attesting his possession of the requisite knowledge and given by a recognised competent body. All such documentary evidence shall be submitted to the Minister when applying for approval. The Minister may call for further evidence if required in any particular case.

   (2) Where the requirements referred to in sub-regulation (1) are satisfied, the Registering Officer shall issue a certificate of approval in Form FERT. 7 in the First Schedule.

 

7.   Approval of laboratories

   (1) An approved laboratory shall be so equipped as to enable approved analysts to perform accurately for the purposes of the Act all the analyses specified under the Third Schedule, and such laboratories shall have been inspected by a duly authorised officer of the Ministry of Agriculture before approval by the Minister and may be inspected from time to time as the Registering Officer may deem necessary:

Provided that, in addition, other laboratories may be approved for certain analyses only, such analyses to be specified by the Registering Officer after inspection by a duly authorised officer of the Ministry of Agriculture.

   (2) Where the Minister approves a laboratory, the Registering Officer shall issue a certificate of approval in Form FERT. 8 in the First Schedule.

 

8.   Roll of analysts

The Registering Officer shall keep a roll of approved analysts in Form FERT. 2 in the First Schedule.

 

9.   Roll of laboratories

The Registering Officer shall keep a roll of approved laboratories in Form FERT. 3 in the First Schedule.

 

PART IV
SEARCHES AND SEIZURES

 

10.   Certificates of authority for inspectors

The certificate of authority to be held by inspectors under section 25 of the Act shall be issued by the Registering Officer and shall be"”

   (a)   in the case of general authorisation, in Form FERT. 11 in the First Schedule; and

   (b)   in the case of limited authorisation, in Form FERT. 12 in the First Schedule.

 

PART V
SALE OF FARMING REQUISITES

 

11.   Statements of analysis for sales in bags, containers, etc.

The statement of analysis for each class of fertiliser as defined in the Fifth Schedule shall appear in English in lettering both durable and legible on the bag or container containing the same or on a label securely attached thereto.

 

12. Statements of analysis for sales in bulk

Where any class of fertiliser as defined in the Fifth Schedule is sold in bulk, the statement of analysis for such class shall appear in English in lettering both durable and legible on a note which shall be given to the purchaser or his agent at the time of delivery of such fertiliser.

 

13.   Statements of analysis for sales under trade names, etc.

Where any class of fertiliser as defined in the Fifth Schedule is sold in a container or a package under a trade name, trade mark, trade label or trade brand, as provided by section 30 of the Act, there shall appear in English in lettering both legible and durable on the container or package or on a label securely attached thereto, a statement of analysis in respect thereof and, in addition, there shall be lodged with the Registering Officer, in respect of such fertiliser, a statement of particulars specified in the Sixth Schedule.

 

PART VI
SAMPLING, ANALYSIS AND LIMITS OF VARIATION

 

14.   Form of report to be used

A report of analysis shall be issued by the analyst performing the analysis in respect of every sample taken under the Act, and any such report shall be in Form FERT. 9 in the First Schedule.

 

15.   Form of certificate to be used

A certificate of analysis shall not be issued unless the sample has been taken in accordance with the Second Schedule and such certificate shall be in Form FERT. 10 in the First Schedule.

 

16.   Method of taking samples

Samples for analysis for the purposes of the Act shall be taken in the manner prescribed in the Second Schedule and certificates of sampling issued in relation thereto shall be in Form FERT. 13 in the First Schedule.

 

17.   Method of analysis

Methods of analysis shall be as prescribed in the Third Schedule.

 

18.   Limits of variation

The limits of variation in respect of any prescribed analysis shall be as prescribed in the Fourth Schedule.

 

FIRST SCHEDULE

CERTIFICATES AND FORMS

 

FORM FERT. 1

REPUBLIC OF ZAMBIA

AGRICULTURE (FERTILISERS AND FEED) ACT

AGRICULTURE (FERTILISERS) REGULATIONS

[Section 4 and Regulation 4]

REGISTER OF PLANT

Certificate Number and Date

Location

Name and Purposes for which Registered

Address of registered owner

Remarks (e.g., if only provisional)

         

 

 

 

FORM FERT. 2

REPUBLIC OF ZAMBIA

AGRICULTURE (FERTILISERS AND FEED) ACT

AGRICULTURE (FERTILISERS) REGULATIONS

[Section 20(a) and Regulation 8]

ROLL OF APPROVED ANALYSTS AND ANALYSTS APPROVED FOR SPECIAL TECHNIQUES

Name

Address

Recognised qualifications

Purposes for which approved (general or special)

Date approved

Certificate Number

Remarks

             

NOTE.-Date of withdrawal of approval shall be noted in "Remarks" column opposite the analyst.

 

FORM FERT. 3

REPUBLIC OF ZAMBIA

AGRICULTURE (FERTILISERS AND FEED) ACT

AGRICULTURE (FERTILISERS) REGULATIONS

[Section 20(b) and Regulation 9]

ROLL OF APPROVED LABORATORIES

Name and address of Laboratory

Names of approved analysts attached to laboratory

Purposes for which approved

Date of withdrawal

Certificate Number

Remarks (e.g. types of analysis)

           

 

 

FORM FERT. 4

REPUBLIC OF ZAMBIA

AGRICULTURE (FERTILISERS AND FEED) ACT

AGRICULTURE (FERTILISERS) REGULATIONS

[Sections 5(1), 11(1), (3), 17(1), (2) and Regulation 3]

APPLICATION FOR REGISTRATION, TRANSFER OF REGISTRATION OR RENEWAL OF REGISTRATION

Name of applicant .................................................................................................................

Address ................................................................................................................................

Address of plant ...................................................................................................................

Nature of activities to be carried out in plant ........................................................................

...............................................................................................................................................

...............................................................................................................................................

Owner of plant ......................................................................................................................

Address of owner .................................................................................................................

Please state whether you are applying for*"”

 

Fee units

   (a)   First registration of plant . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

60

   (b)   Annual renewal of registration of plant . . . . . . . . . . . . . . . . . . . . . . . . .

30

   (c)   Provisional registration of a plant . . . . . . . . . . . . . . . . . . . . . . . . . . . .

30

   (d)   Provisional registration of a transferee from, or successor in interest to a registered owner, as registered owner on the register of plant . . . . . . . . . .

30

   (e)   Full registration of a transferee from, or successor in interest to a registered owner, as registered owner on the register of plant . . . . . . . . . . . . . . . . .

60

NOTE.-Fees should accompany this application.

* Strike out those inapplicable.

FOR OFFICIAL USE ONLY

Ref. No. ............................................................. Date received ............................................

 

Fee units

First registration........................................

60

Renewal.....................................................

30

Transfer (Provisional)...............................

30

Transfer (Full) ...........................................

60

Provisional registration.............................

30

Fee paid ................................................... Date....................................................................

Inspection by .......................................................................................................................

Remarks .............................................................................................................................

Certificate issued by ...........................................................................................................

Certificate No. ........................................ Date ....................................................................

NOTES:

1. This form should be used when applying for registration of any plant or plant ownership.

2. Where a plant is owned by more than one person then one person should be nominated and registered as owner for the purposes of the Act.

3. After this application has been received your plant will be inspected and you will be informed whether or not your plant has been approved for registration with or without conditions.

4. If such an inspection is not immediately practicable your application for registration may be classed as "provisional".

[Am by Act 13 of 1994.]

 

FORM FERT. 5

REPUBLIC OF ZAMBIA

AGRICULTURE (FERTILISERS AND FEED) ACT

AGRICULTURE (FERTILISERS) REGULATIONS

[Section 10(1) and Regulation 3]

CERTIFICATE OF REGISTRATION OF PLANT

This is to certify that the plant situated at .............................................................................

and used for the purpose of ..................................................................................................

and owned by .................................. has been inspected, approved and registered for the purposes of the Act.

This certificate should be displayed in a prominent place in the plant.

..................................................................

Registering Officer

Date ......................................

No. ........................................

Receipt No. ...........................

 

FORM FERT. 6

REPUBLIC OF ZAMBIA

AGRICULTURE (FERTILISERS AND FEED) ACT

AGRICULTURE (FERTILISERS) REGULATIONS

[Sections 8 and 9 and Regulation 3]

CERTIFICATE OF PROVISIONAL REGISTRATION OF PLANT

This is to certify that the plant situated at ................... and used for the purposes of ........................... and owned by ..................... has been provisionally registered for the purposes of the Act.

This certificate should be displayed in a prominent position in the plant.

..................................................................

Registering Officer

Date .......................................

No. .........................................

Receipt No. ............................

 

FORM FERT. 7

REPUBLIC OF ZAMBIA

AGRICULTURE (FERTILISERS AND FEED) ACT

AGRICULTURE (FERTILISERS) REGULATIONS

[Section 18(1) and Regulation 6]

CERTIFICATE OF APPROVAL OF ANALYST

This is to certify that the Minister of Agriculture, Food and Fisheries has approved ................................................

.................................................................... as an analyst for the purposes of the Act.

..................................................................

Registering Officer

Date .................................

No. ...................................

 

FORM FERT. 8

REPUBLIC OF ZAMBIA

AGRICULTURE (FERTILISERS AND FEED) ACT

AGRICULTURE (FERTILISERS) REGULATIONS

[Section 19(1) and Regulation 7]

CERTIFICATE OF APPROVAL OF LABORATORY

This is to certify that the Minister of Agriculture has approved .................................... as a laboratory for the purposes of the Act, subject to the following limitations ...................

..............................................................................................

..............................................................................................

..............................................................................................

..................................................................

Registering Officer

Date ................................

Roll No. ...................................

 

FORM FERT. 9

REPUBLIC OF ZAMBIA

AGRICULTURE (FERTILISERS AND FEED) ACT

AGRICULTURE (FERTILISERS) REGULATIONS

[Section 21 and Regulation 14]

REPORT OF ANALYSIS

I certify that I received on ............................................ 20..........., a sample of ......................................................................... from ..............................................................

The report is as follows:

Laboratory number ....................................................

Sample number .........................................................

...............................................................................................................................................

...............................................................................................................................................

...............................................................................................................................................

...............................................................................................................................................

...............................................................................................................................................

...............................................................................................................................................

Date ....................................................

.................................................

 

Analyst

NOTE.-To be completed in triplicate and copies despatched as follows:

Original - Owner or Seller.

Duplicate - Inspector.

Triplicate - To be retained by Analyst.

 

FORM FERT. 10

REPUBLIC OF ZAMBIA

AGRICULTURE (FERTILISERS AND FEED) ACT

AGRICULTURE (FERTILISERS) REGULATIONS

[Sections 21 and 47 and Regulation 15]

CERTIFICATE OF ANALYSIS

I certify that I received on ..................................., 20............... a sample of ............................................................. from ..................................................... and the analysis of this sample is as declared below.

Laboratory number ...............................................................................................................

Sample number ...................................................................................................................

Constituent

Declared Analysis

Actual Analysis

     
     
     
     
     

Date ....................................................

.................................................

 

Analyst

NOTE.- To be completed in triplicate and copies dispatched as follows:

Original - Owner or Seller.

Duplicate - Inspector.

Triplicate - To be retained by Analyst.

 

FORM FERT. 11

REPUBLIC OF ZAMBIA

THE AGRICULTURE (FERTILISERS AND FEED) ACT

THE AGRICULTURE (FERTILISERS) REGULATIONS

[Sections 24(2) and 25(2) and Regulation 10]

CERTIFICATE OF AUTHORITY FOR INSPECTOR

This is to certify that .................................................................................................. has been duly authorised as an Inspector of farming requisites for the purposes of the Act and is empowered to exercise all the powers therein described anywhere in Zambia.

 

Certificate number ......................................

 
 

..................................................
Inspector

Date ................................................................

.................................................
Registering Officer

 

 


{mprestriction ids="2,3,5"}

FORM FERT. 12

REPUBLIC OF ZAMBIA

AGRICULTURE (FERTILISERS AND FEED) ACT

AGRICULTURE (FERTILISERS) REGULATIONS

[Section 24 and Regulation 10]

CERTIFICATE OF LIMITED AUTHORITY FOR INSPECTOR

This is to certify that ............................................................................................................. has been granted limited authorisation to act as an Inspector of farming requisites for the purposes of the Act and is empowered to exercise all the powers therein described except as stated below.

...............................................................................................................................................

...............................................................................................................................................

...............................................................................................................................................

...............................................................................................................................................

...............................................................................................................................................

Signature of Inspector ...............................................................

Certificate number .....................................................................

Date ...........................................................................................

 

..................................................................

 

Registering Officer

 

 

FORM FERT. 13

REPUBLIC OF ZAMBIA

AGRICULTURE (FERTILISERS AND FEED) ACT

AGRICULTURE (FERTILISERS) REGULATIONS

[Section 52(h) and Regulation 16]

CERTIFICATE OF SAMPLING

I certify that the accompanying is/are sample(s) of ............................................ taken by me on ..................................., 20.........., at .................................. from stock in charge of .......................................................................................................... in the presence of ..................................................................................................................

....................................................

(name and address of witness)

The following particulars are given in connection with this/these sample(s).

Sample No.

Description of goods represented by this sample

Quantity of goods represented by this sample

     

Other particulars ..................................................................................................................

..............................................................................................................................................

Declared analysis as set out in the Fifth Schedule and trade name, trade brand or trade mark, etc., under which sold

..............................................................................................................................................

Signature of witness ......................................

Signature of Inspector ...................................

Date ...............................................................

NOTE.- This form is to be completed in triplicate and should be despatched as follows:

Original - Analyst.

Duplicate - Owner or Seller.

Triplicate - To be retained by Inspector.

 

SECOND SCHEDULE

[Section 25(1)(a), (1)(b) and Regulation 16]

METHOD OF TAKING SAMPLES

NOTE.- In this regulation "metric ton" is defined as 1,000 kg.

1. Where the fertiliser is contained in packages the samples shall be taken from different parts of the whole quantity as follows:

   (a)   if the quantity does not exceed two and a half metric tons, from not less than two unopened packages per ton or part thereof;

   (b)   if the quantity exceeds two and a half metric tons, from one additional unopened package for every additional ton or part thereof:

Provided that in no case need samples be taken from more than 20 packages.

2. Where the fertiliser is not contained in packages, not less than two samples per ton or part thereof shall be taken from different parts of the whole quantity:

Provided that not less than six shall be taken and not more than 50 need be taken.

3. The samples shall be taken by means of a suitable sampling probe or by such other means as will ensure, as far as is practicable, the taking of a representative sample.

4. The samples thus taken shall be thoroughly mixed and reduced in size to give a final sample not exceeding six pounds in weight. This final sample shall be mixed and divided into three parts and each of these parts shall be transferred to a clean, dry, non-corrodible container capable of being closed in such a manner as to preserve the contents of the container in their original condition. These three containers shall be so sealed so that they cannot be opened without breaking the seal. Each of these three parts shall be marked with the name of the fertiliser, date and place of sampling and the sample number together with the name of the inspector taking the sample.

5. The first part shall be given to the owner or seller of the fertiliser or his agent, the second part shall be delivered to an approved analyst for analysis, and the third part shall be retained by the inspector for a period of not less than six months after the date on which the Report or Certificate of Analysis is issued.

6. A Certificate of Sampling (Form FERT. 13 in the First Schedule) shall be made out in triplicate at the time of sampling and the relevant copies as detailed in Form FERT. 13 in the First Schedule should accompany each part of the sample.

[Am by SI 117 of 1970.]

 

THIRD SCHEDULE

[Section 52(i) and Regulation 17]

METHODS OF ANALYSIS OF FERTILISERS

1. PREPARATION OF SAMPLE:

   (a)   Remove any extraneous matter which cannot be conveniently ground and allow for this when calculating results.

   (b)   Grind the sample as rapidly as possible to pass through a sieve having apertures about 1 mm. square. In the case of granular fertilisers and dry powdered fertilisers grind a representative portion of about 250 g. to pass through a sieve having apertures about 0.25 mm. square.

   (c)   Store the prepared sample in a non-corrodible air-tight container.

   (d)   Where a sample is too moist to be ground in its original condition, mix the sample thoroughly and remove a portion for moisture determination. Dry the remaining portion at 100 degrees C except where the sample may lose ammonia or where the sample contains soluble phosphorus compounds. In these instances dry the sample in a desiccator over calcium chloride or silica gel, or alternatively by passing dry air at room temperature over the sample until it is in a suitable condition for grinding. The results of the analysis of the dried sample should be adjusted to the "as received" condition.

2. DETERMINATION OF MOISTURE:

Weigh to the nearest mg. about 5 g. of the sample and heat to 100ºC for three hours, cool in a desiccator and weigh. Calculate the loss in weight as a percentage of the original weight.

3. DETERMINATION OF NITROGEN:

   (a)   REAGENTS

Ammonia alum.

Standard indigo solution.

Cautiously add 40 ml. of concentrated sulphuric acid to 1 g. of indigo carmine and stir until dissolved. Pour the solution into 800 ml. of water, cool and dilute to 1 litre. Adjust the strength of the solution to comply with the following test:

Add 20 ml. to a solution of 4 mg. of potassium nitrate in 20 ml. of water. Add rapidly 40 ml. of concentrated sulphuric acid and heat to boiling; the blue colour is just discharged in one minute.

Concentrated sulphuric acid.

1 : 9 Sulphuric acid-Cautiously add 100 ml. of concentrated sulphuric acid to 900 ml. of water. Cool and dilute to 1 litre.

1 : 1 Sulphuric acid-Cautiously add 500 ml. of concentrated sulphuric acid to 500 ml. of water. Cool and dilute to 1 litre.

Anhydrous sodium sulphate.

Cupric sulphate.

Paraffin wax.

Granulated zinc.

Light magnesium oxide.

50% sodium hydroxide solution-Dissolve 500 g. of sodium hydroxide in water and dilute to 1 litre.

0.1 N Hydrochloric acid.

Mixed indicator solution-Grind together in an agate mortar 0.6 g. of methyl red

and 0.6 g. of methylene blue. Dissolve the mixture in 500 ml. of 95% ethanol. Shake, filter and store in a dark glass bottle.

2% Boric acid solution-Dissolve 20 g. of boric acid in water, dilute to 1 litre and add 5 ml. of the mixed indicator solution.

Devarda's alloy: Finely powdered-not less than 80% to pass through a sieve having apertures of about 0.25 mm. square.

   (b)   TEST FOR ABSENCE OF NITRATES

Shake 5 g. of the sample with 80 ml. of water in a 100 ml. volumetric flask. Add 1 g. of ammonia alum, dilute to 100 ml., shake well and filter into a dry beaker. Dilute 1 ml. of the filtrate with 8 ml. of water. Add 1 ml. of standard indigo solution and 10 ml. of concentrated sulphuric acid. Heat to boiling point. If the colour is not discharged regard the sample as free from nitrates.

   (c)    TOTAL NITROGEN (ORGANIC AND AMMONIACAL) IN THE ABSENCE OF NITRATES

      (i)   Weigh to the nearest mg. about 2 g. of the sample (or an amount containing not more than 250 mg. of nitrogen) and transfer to a Kjeldahl flask. Add 25 ml. of concentrated sulphuric acid and approximately 10 g. of anhydrous sodium sulphate containing 0.4 g. of cupric sulphate. Heat gently until frothing ceases, increase the heat and continue the digestion until the liquid is practically colourless. Continue to heat for a further hour. If frothing is excessive add about 0.5 g. of paraffin wax. Avoid local overheating.

      (ii)   Transfer the cooled digest to 250 ml. volumetric flask. Thoroughly wash the Kjeldahl flask with successive portions of water carefully adding the washings to the digest in the volumetric flask. When cool adjust the contents of the volumetric flask to a volume of 250 ml. with water. Thoroughly mix the contents of the flask and pipette an aliquot such as to give a final titration of at least 4 ml. into a Kjeldahl flask. Add 250 ml. of water, a small zinc granule and sufficient 50% sodium hydroxide solution to neutralise the acid and give about 10 ml. in excess. Mix well and connect immediately to a distillation apparatus. Distil into an appropriate volume (usually 30 ml.) of 2% boric acid solution. Titrate the contents of the receiving flask with 0.1 N hydrochloric acid. The colour change is from green to purple. Carry out a blank test using 2 g. of sucrose in place of the sample and substract the titration value of the blank from that of the sample. Express the result in terms of nitrogen (N). 1 ml. of 0.1 N hydrochloric acid = 0.0014 g. nitrogen.

   (d)   TOTAL NITROGEN (ORGANIC, AMMONIACAL AND NITRIC) IN THE PRESENCE OF NITRATES

Weigh to the nearest mg. about 1 g. of the sample (or an amount containing not more than 250 mg. of nitrogen) and transfer to a Kjeldahl flask. Add 3 g. of Devarda's alloy and wash down the neck of the flask with 50 ml. of water. Close the flask with a rubber stopper fitted with (a) a tap funnel and (b) a delivery tube connected to a U-tube (with bulbs) containing 20 ml. of 1 : 9 sulphuric acid. Add 5 ml. of 50% sodium hydroxide solution through the tap funnel, allow to stand for 30 minutes and then heat at just below boiling point for 60 minutes. Cool, add 20 ml. of 1 : 1 sulphuric acid through the tap funnel, washing the neck of the flask. Remove the rubber stopper, wash the contents of the U-tube into the Kjeldahl flask, add 25 ml. of concentrated sulphuric acid and heat until all the water has boiled off. Add approximately 10 g. of anhydrous sodium sulphate containing 0.4 g. of cupric sulphate and heat gently until frothing ceases. Increase the heat and continue the digestion for a further hour. Avoid local overheating. Cool, and complete the determination by the method described under (c) (ii).

   (e)   AMMONICAL NITROGEN

Weigh to the nearest mg. about 5 g. of the sample, transfer to a 250 ml. volumetric flask, dissolve in about 200 ml. of water, dilute to the mark and filter if necessary. Transfer 50 ml. of the solution (or an aliquot such as to give a final titration of at least 4 ml.) to a distillation flask, add approximately 300 ml. of water and 20 ml. of 50% sodium hydroxide solution. (If urea is known to be present 10 g. of light magnesium oxide should be used instead of 50% sodium hydroxide solution.) Connect immediately to a distillation apparatus. Distil into 30 ml. of 2% boric acid solution. Titrate the contents of the receiving flask with 0.1 N hydrochloric acid. The colour change is from green to purple. Carry out a blank determination using sucrose in place of the sample and subtract the titration value of the blank from that of the sample. Express the result in terms of nitrogen (N). 1 ml. of 0.1 N hydrochloric acid = 0.0014 g. nitrogen.

   (f)   AMMONICAL AND NITRATE NITROGEN (IN INORGANIC FERTILISERS)

Weigh to the nearest mg. about 2 g. of the sample, transfer to a 250 ml. volumetric flask, dissolve in 200 ml. of water, dilute to volume and filter if necessary. Transfer 10 ml. of the solution (or an aliquot such as to give a final titration of at least 4 ml.) to a distillation flask. Add 10 g. of Devarda's alloy, 250 ml. of water and 15 ml. of 50% sodium hydroxide solution. Connect the flask immediately to the distillation apparatus and allow to stand in the cold for 15 minutes. Warm gently for 30 minutes, slowly increasing the temperature. Distil into 30 ml. of 2% boric acid solution. Titrate the contents of the receiving flask with 0.1 N hydrochloric acid. The colour change is from green to purple. Carry out a blank determination using sucrose in the place of the sample and substract the titration value of the blank from that of the sample. Express the result in terms of nitrogen (N). 1 ml. of 0.1 N hydrochloric acid = 0.0014 g. nitrogen.

4. DETERMINATION OF PHOSPHORUS:

   (a)   EXTRACTION OF SAMPLE

Weigh to the nearest centigram about 10 g. of the sample and transfer to a 500 ml. volumetric flask; add 400 ml. of water and shake the flask continuously for 30 minutes. Dilute the contents to the mark, mix well and filter.

   (b)   QUINOLINIUM PHOSPHOMOLYBDATE METHOD

      (i)   REAGENTS

Concentrated hydrochloric acid.

Concentrated nitric acid.

Calcium oxide-finely ground.

Calcium carbonate.

5 N sodium hydroxide solution.

Dilute hydrochloric acid - Dilute 240 ml. of concentrated hydrochloric acid with water to 1 litre.

Citric - molybdic acid solution-Stir 54 g. of molybdic anhydride (MoO3) with 200 ml. of water, add 11 g. of sodium hydroxide and stir the mixture whilst heating to boiling point until the molybic anhydride dissolves. Dissolve 60 g. of citric acid in about 250 ml. to 300 ml. of water and add 140 ml. of concentrated hydrochloric acid. Pour the molybdate solution into the acid solution, which is stirred throughout the addition. Then cool and, if necessary, filter the solution through a 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 or 1.0%) solution of potassium bromate until the colour is discharged. This reagent should be kept in the dark.

Quinoline solution - Measure 60 ml. of concentrated hydrochloric acid and 300 to 400 ml. of water into a 1 litre beaker and warm to 70-80ºC. Pour 50 ml. of quinoline in a thin stream into the diluted acid while stirring. When the quinoline has dissolved cool the solution, dilute to 1 litre, and, if necessary, filter through a paper pulp filter.

0.5 N sodium hydroxide - carbonate free.

Indicator solution - Mix 3 volumes of thymol blue solution and 2 volumes of phenolphthalein solution prepared as follows:

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

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

0.5 N hydrochloric acid.

0.1 N sodium hydroxide solution - carbonate free.

0.1 N hydrochloric acid.

Surface active agent - 0.5% solution of sodium dodecyl benzene sulphonate is suitable.

Crystallised citric acid - monohydrate

      (ii)   PROCEDURE

Transfer a volume of the aqueous extract containing not less than 30 mg. of phosphorus and preferably about 20 mg. to a 500 ml. stoppered conical flask marked at 150 ml. Dilute with water to 150 ml., add 50 ml. of the citric-molybdic acid reagent, heat the solution to incipient ebullition, maintain it at this temperature for 3 minutes, and then bring it to boiling point. From a burette slowly add 25 ml. of the quinoline solution with constant swirling throughout, the first few ml. being added dropwise, the rest in a slow stream. Keep the solution gently boiling during the addition. Immerse the flask in boiling water for 5 minutes, then cool it to 150ºC in running water.

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. Transfer the filter pad and precipitate to the original flask, rinse the funnel with water and collect the rinsings in the flask. If necessary, wipe the funnel with a small piece of damp filter paper to ensure complete removal of the precipitate and place the paper in the flask. Add water to a total of about but not exceeding 100 ml. Stopper the flask and shake it vigorously until the pulp and the precipitate are completely dispersed.

Remove the stopper and wash it with water, returning the washings to the flask. Add a measured volume of 0.5 N sodium hydroxide solution sufficient to dissolve the precipitate and leave a few ml. in excess. Shake the flask vigorously until all the precipitate dissolves. (To facilitate the dispersal of the precipitate, after addition of 0.5 N sodium hydroxide solution, a few drops of surface active agent may be added.) Add 0.5-1.0 ml. of the indicator solution and titrate the excess of sodium hydroxide with the 0.5 N hydrochloric acid until the indicator changes from violet to green-blue and then very sharply to yellow at the end point. Deduct the number of ml. of 0.5 N hydrochloric acid used from the number of ml. of 0.5 N sodium hydroxide, to ascertain the volume of 0.5 N sodium hydroxide equivalent to phosphorus.

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.

Calculate the amount of phosphorus in the portion taken for analysis from the factor 1.0 ml. 0.5 N sodium hydroxide = 0.597 mg. phosphorus (P).

   (c)   SPECTROPHOTOMETRIC (VANADIUM PHOSPHOMOLYBDATE) METHOD

      (i)   REAGENTS

Potassium dihydrogen phosphate - containing at least 99.8% monopotassium dihydrogen phosphate.

Ammonium molybdate. Ammonium vanadate

Concentrated hydrochloric acid.

Concentrated nitric acid.

Calcium oxide-finely ground.

Standard phosphorus solution - Dissolve in water 2.1953 g. of potassium dihydrogen phosphate previously dried at 105ºC for 1 hour and dilute to 1 litre. Make a 5 fold dilution (1 ml. = 0.1 mg. phosphorus (P)).

Vanadium molybdate reagent - Dissolve separately 20 g. of ammonium molybdate and 1 g. of ammonium vanadate in water, mix, acidify with 140 ml. of concentrated nitric acid and dilute to 1 litre.

Normal sodium hydroxide solution. Crystallised citric acid.

      (ii)   STANDARDISATION OF INSTRUMENT

From a burette measure into a series of 100 ml. volumetric flasks 22.0, 23.0, 24.0, 25.0, 26.0 and 27.0 ml. of the standard phosphorus solution (i.e. 2.2, 2.3, 2.4, 2.5, 2.6 and 2.7 mg of P). Add 25 ml. of the vanadium molybdate reagent to each flask and dilute to 100 ml. with water. Shake and allow to stand for 10 minutes.

Set the spectrophotometer to the correct wavelength, say 4200, fill two 1 cm. cells with the 2.2 mg. solution and check the optical density of the cells. If there is a small difference select the cell with the smaller reading as the standard reference cell.

Determine the apparent optical density (corrected for cell differences) of the 2.3, 2.4, 2.5, 2.6 and 2.7 mg. phosphorus solutions referred to the 2.2 mg. phosphorus solution as standard.

Plot a calibration graph of scale readings against known phosphorus content.

      (iii)   ANALYSIS OF SAMPLE

To 25 ml. of the solution prepared according to paragraph 4 (a) add 1 ml. of concentrated nitric acid; heat to incipient ebullition on a hotplate and maintain it at this temperature for 10 minutes. Cool, neutralise with normal sodium hydroxide solution and then successively dilute until a final volume of about 25 ml. contains between 2.4 and 2.7 mg. of phosphorus.

Transfer this volume to a 100 ml. volumetric flask, add 25 ml. of the vanadium molybdate reagent, dilute to the mark, mix and allow to stand for 10 minutes. At the same time transfer 25 ml. of the standard phosphorus solution into a second 100 ml. volumetric flask. Add 25 ml. of the vanadium molybdate reagent, dilute to the mark, mix and allow to stand for 10 minutes.

Measure the difference in optical density between the two solutions and estimate the phosphorus content of the volume of the unknown solution from the calibration graph. Calculate the phosphorus content of the sample from known dilution factors and the weight of the sample.

NOTE.-Prepare a fresh reference standard for each series of readings on the instrument.

5. DETERMINATION OF POTASSIUM

   (a)   PERCHLORIC ACID METHOD

      (i)   REAGENTS

Concentrated hydrochloric acid.

Barium chloride solution - Dissolve 100 g. of barium chloride in water, filter the solution and dilute to 1 litre.

Dilute hydrochloric acid - Dilute 240 ml. of concentrated hydrochloric acid with water to 1 litre.

Calcium oxide - finely ground.

Ammonium hydroxide solution - sp. gr. 0.912.

Ammonium carbonate solution - saturated aqueous solution.

Ammonium oxalate solution - saturated aqueous solution.

20% perchloric acid solution.

Alcohol - industrial methylated spirit 95-96% v/v.

Wash solution - Add potassium perchlorate to alcohol and shake until a saturated solution is obtained.

Keep the solution over solid potassium perchlorate and filter immediately before use.

      (ii)   PREPARATION OF SAMPLE SOLUTION

      (I)   POTASSIUM SALTS FREE FROM SULPHATES AND OTHER INTERFERING SUBSTANCES

Dissolve in water a portion of the sample weighed to the nearest mg. equivalent in potassium content to 1.2 to 1.7 g. of potassium. Cool the solution, dilute to 500 ml. in volumetric flask, mix well and filter. Determine the potassium in 50 ml. of this solution by the method described in paragraph 5 (a) (iii).

      (II)   POTASSIUM SALTS CONTAINING SULPHATES

NOTE.-If sample contains phosphates, iron, manganese or substances other than sulphate that interfere with the determination of potassium the method described in paragraph 5 (a) (ii) (III) should be used.

Weigh to the nearest mg. a portion of the sample equivalent in potassium content to 1.2 to 1.7 g. of potassium into a 500 ml. beaker, add about 300 ml. of water and 20 ml. of concentrated hydrochloric acid and heat the solution to boiling. 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. Cool the liquid to 20 degrees C, transfer to a 500 ml. volumetric flask, dilute to 500 ml., mix, and filter through a dry filter. Take 50 ml. of the filtrate and evaporate to dryness in a basin; moisten the residue with concentrated hydrochloric acid, again evaporate to dryness, dissolve the residue with 5-10 ml. of dilute hydrochloric acid and filter if necessary. Determine the potassium in the solution by the method described in paragraph 5(a)(iii).

      (III)   POTASSIUM IN MIXED FERTILISERS

Weigh to the nearest centigram about 10 g. of the sample and, if organic matter is present, gently incinerate at a temperature not exceeding 500ºC. Transfer the weighted portion of the sample or the incinerated residue to a 500 ml. beaker with a little water and 10 ml. of concentrated hydrochloric acid and then warm for 10 minutes. Dilute with water to about 300 ml. and bring gradually to boiling point. Add 10 g. of calcium oxide made into a paste with water, bring the contents again gently to boiling point, and keep so heated for about half an hour with frequent stirring. Cool to 20ºC, transfer to a 500 ml. volumetric flask, dilute to 500 ml. and, after thoroughly shaking, filter through a dry filter paper. Transfer 250 ml. of the filtrate to another 500 ml. volumetric flask, make just acid with hydrochloric acid and heat to boiling point. To the boiling solution cautiously add, drop by drop, barium chloride solution until there is no further precipitation of barium sulphate. 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 1 ml. of ammonium oxalate solution. Cool to 20ºC, dilute with water to 500 ml. and after thoroughly shaking, filter through a dry filter paper. Measure 100 ml. 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. Cool the residue, moisten with concentrated hydrochloric acid and again evaporate to dryness. Take up the residue with water and filter if necessary. Determine the potassium in the solution by the method described in paragraph 5(a)(iii).

      (iii)   PROCEDURE

Transfer the solution obtained as described in paragraph 5(a)(iii)(I), 5(a)(ii)(II) or 5(a)(ii)(III) into a basin and add about 7 ml. of perchloric acid solution. Place the basin on a hotplate or sand bath and evaporate the contents until white fumes are copiously evolved. Cool, and dissolve the precipitate in a little hot water. Add about 1 ml. of perchloric acid solution and again concentrate to the fuming stage. Thoroughly cool the residue in the basin and stir in 20 ml. of alcohol. Allow the precipitate to cool and settle; then pour the clear liquid through a dry filter paper, draining the precipitate in the basin as completely as possible. Redissolve the precipitate on the paper and that remaining in the basin with hot water, add 2 ml. of perchloric acid solution to the combined residue in the basin and thoroughly stir the contents with 20 ml. of alcohol. Allow the precipitate to cool and settle and pour clear liquid through a weighed Gooch or sintered glass crucible, draining the precipitate as completely as possible from the liquid before adding 5 ml. of the wash solution. Wash the precipitate by decantation with several similar small portions of the wash solution, pouring the washings through the crucible. Transfer the precipitate to the crucible and wash it well with the wash solution until free from acid. Dry the precipitate at 100ºC and weigh. Regard the precipitate as potassium perchlorate (KClO4) and calculate its equivalent as potassium (K) by multiplying its weight by 0.282. Calculate the potassium content of the sample.

5. (b)   FLAME PHOTOMETRIC PROCEDURE

The determination of potassium by this method depends on the measurement of the characteristic radiation due to potassium emitted by a flame into which a solution of the sample is sprayed. The chosen radiations lie in the spectral range 7660-7700 nm . These radiations may be isolated by either a monochromator or the use of a suitable filter. This method must not be used where the potassium content of the material being analysed exceeds 17% by weight.

      (i)   REAGENTS.

Potassium dihydrogen phosphate - containing at least 99.8% mono-potassium dihydrogen phosphate.

Concentrated hydrochloric acid.

Ammonium oxalate solution - saturated aqueous solution.

Ammonium hydroxide solution - sp. gr. 0.96.

Standard potassium solution - Dissolve in water 6.9608 g. of potassium dihydrogen phosphate previously dried for 1 hour at 105ºC, and dilute to 1 litre in a volumetric flask. Shake well. Transfer 50 ml. to a 1 litre volumetric flask and dilute to the mark. Shake well. This solution contains 100 p.p.m. potassium (K).

      (ii)   PREPARATION OF SAMPLE SOLUTION (I) POTASSIUM SALTS

If the sample contains ammonium, calcium, iron, aluminium or other interfering substances the procedure described under paragraph 5 (b) (ii) (II) should be used.

Weigh to the nearest mg. about 2.5 g. of the sample and transfer to a 400 ml. beaker. Add about 10 ml. of concentrated hydrochloric acid and 50 ml. of water and bring the contents to boiling point, breaking down with a stirring rod any lumps or crystals. Dilute the solution with water to about 100 ml. and boil gently for a few minutes. Cool the solution to 20ºC, transfer to a 250 ml. volumetric flask, and dilute to the mark. Mix and filter through a dry filter. Successively dilute so that the final solution contains approximately 14 p.p.m. potassium (K) and determine potassium in the filtrate by the method described in paragraph 5 (b) (iii).

      (II)   POTASSIUM IN MIXED FERTILISERS

Weigh to the nearest mg. about 2.5 g. of the sample and transfer to a 400 ml. beaker. Add 125 ml. of water and 50 ml. of ammonium oxalate solution. Boil the contents for 30 minutes. If necessary a small quantity of potassium-free anti-foaming agent may be added. Cool the liquid, add a slight excess of ammonium hydroxide solution and cool to 20ºC. Transfer to a 250 ml. volumetric flask and dilute to the mark. Mix the solution and filter through a dry filter. Successively dilute so that the final solution contains approximately 14 p.p.m. potassium (K) and determine the potassium by the method described in paragraph 5 (b) (iii).

      (iii)   METHOD OF ANALYSIS

      (I)   CALIBRATION OF INSTRUMENT

From the standard potassium solution prepare a set of accurate dilutions containing 8, 10, 12, 14, 16 and 18 p.p.m. potassium. Set the sensitivity of the flame photometer so that 100 scale divisions (full scale deflection) is equivalent to 18 p.p.m. potassium solution. Spray the 8, 10, 12, 14 and 16 p.p.m. potassium solutions three times. Take the median reading (not the mean) and construct a calibration graph. After spraying each different strength solution, again spray the 18 p.p.m. solution to ensure that the sensitivity of the flame photometer has not changed.

      (II)   ANALYSIS OF THE SAMPLE SOLUTION

Reset the instrument at 100 scale divisions (full scale deflection) with 18 p.p.m. potassium solution. Spray the diluted fertiliser solution prepared in accordance with paragraph 5 (b) (ii) (I) or 5 (b) (ii) (II) and read from the graph the approximate potassium content of the solution.

Prepare two further dilutions of the standard potassium solution to contain respectively 1 p.p.m. more and 1 p.p.m. less potassium than the estimated potassium content of the diluted solution of the sample. Successively spray the low standard solution, the diluted solution of the sample, and the high standard solution. Repeat this operation twice more. Take the median result of each set of three readings and calculate the potassium content of the sample solution and hence the fertiliser from the proportionality of the radiation given by the sample solution and that given by the two standard solutions containing respectively 1 p.p.m. more and 1 p.p.m. less potassium than the predicted potassium content. Dilute standard solutions should be freshly prepared.

6. FREE ACID IN SULPHATE OF AMMONIA

   (a)   REAGENTS

Methyl red indicator solution - Dissolve 25 mg. of methyl red in 5 ml. of 90% industrial methylated spirit with the aid of 0.5 ml. of 0.1 N sodium hydroxide solution. Dilute to 250 ml. with 50% industrial methylated spirit. If desired screened methyl red indicator may be used. 0.1 N sodium hydroxide solution-carbonate free.

   (b)   PROCEDURE.

Weigh to the nearest centigram about 20 g. of the sample and dissolve in about 50 ml. of water. Filter, wash any insoluble matter and the filter paper free from sulphate and dilute the combined filtrate and washings to about 250 ml. Add 2 or 3 drops of the indicator solution and titrate with 0.1 N sodium hydroxide solution. Express the result as percentage by weight of sulphuric acid (H2SO4). 1ml. O. 1 N sodium hydoxide solution = 0.0049 g. sulphuric acid (H2SO4).

 

FOURTH SCHEDULE

[Section 52(g) and Regulation 18]

LIMITS OF VARIATION

The limits shown shall be the maximum variation allowed above and below the amount stated except in the case of sulphur.

1. Limits Applicable to all Fertilisers Except in 2 below:

Nitrogen

 

All forms of nitrogen expressed as % N:1/10th of amount stated with a minimum of 0.3% N and a maximum of 1.0% N.

Phosphorus

 

Water-soluble phosphorus expressed as % P: 1/20th of amount stated with a minimum of 0.2% P and a maximum of 0.9% P.

Potassium

 

Total potassium expressed as % K: 1/20th of amount stated with a minimum of 0.6% K and a maximum of 1.7% K.

Chloride

 

Percentage chloride expressed as % Cl: 1/20th of amount stated.

Boron

 

Percentage boron expressed as % B: 1/5th of amount stated.

Sulphur

 

No variation allowed below minimum amount stated.

2. Limits Applicable to Borax and Other Borates for Use as Fertilisers:

Percentage boron expressed as % B: 1/10th of amount stated with a maximum of 1.0% B.

3. Sulphate of Ammonia:

In addition to the other limits applicable in 1 above, percentage of free acid content:

1/5th of amount stated or 0.025% whichever is the greater, expressed as percentage by weight of sulphuric acid (H2SO4).

 

FIFTH SCHEDULE

[Sections 28, 29 and 52(k) and Regulations 11 and 12]

STATEMENTS OF ANALYSIS REQUIRED FOR DIFFERENT CLASSES OF FERTILISERS

 

Statement of Analysis to be Shown on Bags, Containers or Labels, and Notes to Accompany

Class of Fertiliser

Sales in Bulk

Nitrogenous fertilisers

Percentage of total nitrogen.

Ammoniated phosphates and ammoniated super-phosphates.

Percentage of total nitrogen.

 

Percentage of water-soluble phosphorus expressed in the elemental form (P).

elemental form (P).

Minimum percentage of sulphur expressed in the elemental form (S).

Single, double or triple super-phosphates.

Percentage of water-soluble phosphorus expressed in the elemental form as (P).

Potassic fertilisers.

Percentage of potassium expressed in the elemental form (K).

Any other inorganic fertiliser or compound, complex, blend or mixture of fertilisers.

Percentage of total nitrogen (N).

 

Percentage of water-soluble phosphorus expressed in the elemental form (P).

 

Percentage of potassium expressed in the elemental form (K).

 

Percentage of boron expressed in the elemental form (B).

 

Minimum percentage of sulphur expressed in the elemental form (S).

Borax and other borates for use as fertilisers.

Percentage of boron expressed in the elemental form.

 

SIXTH SCHEDULE

[Section 30 and Regulation 13]

STATEMENT OF PARTICULARS TO BE LODGED WITH THE REGISTERING OFFICER IN RESPECT OF FERTILISERS SOLD IN BAGS, CONTAINERS, ETC., UNDER ANY TRADE NAME, TRADE MARK, ETC., AS DESCRIBED IN SECTION 30 OF THE ACT

1. Percentage by weight of nitrogen:

   (a)   in the ammonium form;

   (b)   in the nitrate form;

   (c)   in the urea form;

   (d)   in any other form.

2. Percentage by weight of water-soluble phosphorus expressed as (P).

3. Percentage by weight of potassium expressed as (K):

   (a)   in the chloride form;

   (b)   in the sulphate form;

   (c)   in any other form.

4. The minimum percentage by weight of sulphur expressed as (S).

5. The percentage by weight of boron expressed as (B).

6. In the case of sulphate of ammonia only the percentage of free acid.

7. The trade name, brand name, etc., under which the product is to be sold.

8. By whom sold ....................................................................................................................

................................................................................................................................................

Address...................................................................................................................................

................................................................................................................................................

................................................................................................................................................

 

 

AGRICULTURE (FARM FEED) REGULATIONS

[Section 52]

Arrangement of Regulations

   Regulation

PART I
PRELIMINARY

   1.   Title

   2.   Interpretation

   3.   Application

PART II
REGISTRATION

   4.   Registration of plant and fees

   5.   Register of plant

   6.   Requirements of plant

PART III
ANALYSIS AND LABORATORIES

   7.   Approval of analysts

   8.   Approval of laboratories

   9.   Roll of analysts

   10.   Roll of laboratories

PART IV
SEARCHES AND SEIZURES

   11.   Certificate of authority for inspectors

PART V
SALE OF FARM FEED

   12.   Statements of analysis for sales in bags, containers, etc.

   13.   Statements of analysis for sales in bulk

   14.   Statements of analysis and records to be kept for sales under trade names, etc.

   15.   Exemption of farm feed made to specification

   16.   Deleterious ingredients

   17.   Declaration of presence of certain ingredients upon sale

PART VI
SAMPLING, ANALYSIS AND LIMITS OF VARIATION

   18.   Form of report to be used

   19.   Form of certificate to be used

   20.   Method of taking samples

   21.   Methods of analysis

   22.   Limits of variation

      FIRST SCHEDULE

      SECOND SCHEDULE

      THIRD SCHEDULE

      FOURTH SCHEDULE

      FIFTH SCHEDULE

      SIXTH SCHEDULE

      SEVENTH SCHEDULE

      EIGHTH SCHEDULE

[Regulations by the Minister]

SI 197 of 1970.

 

PART I
PRELIMINARY

 

1.   Title

These Regulations may be cited as the Agriculture (Farm Feed) Regulations.

 

2.   Interpretation

In these Regulations, unless the context otherwise requires"”

"the Act" means the Agriculture (Fertilisers and Feed) Act.

"Minister" means the Minister responsible for Agriculture.

 

3.   Application

These Regulations shall apply in relation to any farm feed as defined in section 2 of the Act.

 

PART II
REGISTRATION

 

4.   Registration of plant and fees

   (1) Applications under Part II of the Act for registration, transfer of registration or renewal of registration of plant shall be made in Form FERT 4 in the First Schedule to the Agriculture (Fertilisers) Regulations, 1969 (hereinafter in these Regulations referred to as "the Fertilisers Regulations") and such application shall be accompanied by the appropriate fees shown in the First and Second Schedules to the Act, and be given to the Registering Officer.

   (2) The Registering Officer shall issue a certificate of registration in Form FERT 5 in the First Schedule to the Fertilisers Regulations.

   (3) The Registering Officer shall issue a certificate of provisional registration in Form FERT 6 in the First Schedule to the Fertilisers Regulations.

 

5.   Register of plant

The Registering Officer shall keep a register of plant as prescribed in Form FERT 1 in the First Schedule to the Fertilisers Regulations.

 

6.   Requirement of plant

Any plant within the definition of section 2 of the Act shall be so equipped as to permit the adequate performance therein of the activities described in the application for registration of such plant, to the satisfaction of the Registering Officer.

 

PART III
ANALYSTS AND LABORATORIES

 

7.   Approval of analysts

   (1) For the purposes of the Act an analyst shall furnish proof to the satisfaction of the Minister that he has competent knowledge of chemistry and of chemical analyses, as applied to farm feed, and such proof shall in every case comprise documentary evidence that the analyst holds a certificate or diploma attesting his possession of the requisite knowledge and given by a recognised competent body, and shall be submitted to the Minister when applying for approval, so, however, that the Minister may call for further evidence if required in any particular case.

   (2) Where the requirements referred to in sub-regulation (1) are satisfied, the Registering Officer shall issue a certificate of approval on Form FERT 7 in the First Schedule to the Fertilisers Regulations.

 

8.   Approval of laboratories

   (1) An approved laboratory shall be so equipped as to enable approved analysts to perform accurately for the purposes of the Act all the analyses specified under the Seventh Schedule to these Regulations and such laboratories shall have been inspected by a duly authorised officer of the Ministry of Agriculture, Food and Fisheries before approval by the Minister and may be inspected from time to time as the Registering Officer may deem necessary:

Provided that, in addition, other laboratories may be approved for certain analyses only, such analyses to be specified by the Registering Officer after inspection by a duly authorised officer of the Ministry of Agriculture, Food and Fisheries.

   (2) Where the Minister approves a laboratory, the Registering Officer shall issue a certificate of approval on Form FERT 8 in the First Schedule to the Fertilisers Regulations.

 

9.   Roll of analysts

The Registering Officer shall keep a roll of approved analysts in Form FERT 2 in the First Schedule to the Fertilisers Regulations.

 

10.   Roll of laboratories

The Registering Officer shall keep a roll of approved laboratories in Form FERT 3 in the First Schedule to the Fertilisers Regulations.

 

PART IV
SEARCHES AND SEIZURES

 

11.   Certificate of authority for inspectors

The certificate of authority to be held by inspectors under section 25 of the Act shall be issued by the Registering Officer and shall be"”

   (a)   in the case of general authorisation, in Form FERT 11 in the First Schedule to the Fertilisers Regulations; and

   (b)   in the case of limited authorisation, in Form FERT 12 in the First Schedule to the Fertilisers Regulations.

PART V
SALE OF FARM FEED

 

12.   Statements of analysis for sales in bags, containers, etc.

The statement of analysis for each class of farm feed specified in the Second Schedule to these Regulations shall appear in English in lettering both durable and legible on the bag or container containing the same or on a label securely attached thereto.

 

13.   Statements of analysis for sales in bulk

Where any class of farm feed specified in the Second Schedule to these Regulations is sold in bulk, the statement of analysis for such class shall appear in English in lettering both durable and legible on a note which shall be given to the purchaser or his agent at the time of delivery of such farm feed.

 

14.   Statements of analysis and records to be kept for sales under trade names, etc.

Where any class of farm feed specified in the Second Schedule to these Regulations is sold in a container or a package under a trade name, trade mark, trade label or trade brand, as provided by section 30 of the Act, there shall appear in English in lettering both durable and legible on the container or package, or on a label securely attached thereto, a statement of analysis in respect thereof and, in addition, the Registering Officer shall have access to such records relating thereto as are specified in the Third Schedule to these Regulations.

 

15.   Exemption of farm feed made to specification

Where any farm feed is manufactured to a farmer's own specifications, such farm feed shall be exempted from these Regulations, but only if the farm feed is for the sole use of the farmer supplying the specifications and is not intended for re-sale.

 

16.   Deleterious ingredients

No class of farm feed shall contain any of the ingredients listed as deleterious in the Fourth Schedule to these Regulations.

 

17.   Declaration of presence of certain ingredients upon sale

The presence in any farm feed of any of the materials specified in the Fifth Schedule to these Regulations shall be declared in writing to the purchaser of any farm feed whether sold in containers, in bulk or under any trade name, trade mark, trade label or trade brand.

 

PART VI
SAMPLING, ANALYSIS AND LIMITS OF VARIATION

 

18.   Form of report to be used

A report of analysis shall be issued by the analyst performing the analysis in respect of every sample taken under the Act, and any such report shall be in Form FERT 9 in the First Schedule to the Fertilisers Regulations.

 

19.   Form of certificate to be used

A certificate of analysis shall not be issued unless the sample has been taken in accordance with the Sixth Schedule to these Regulations and such certificate shall be in the Form FERT 10 in the First Schedule to the Fertilisers Regulations.

 

20.   Method of taking samples

Samples for analysis for the purposes of the Act shall be taken in the manner prescribed in the Sixth Schedule to these Regulations and certificates of sampling issued in relation thereto shall be in Form FERT 13 in the First Schedule to the Fertilisers Regulations.

 

21.   Methods of analysis

Methods of analysis shall be as prescribed in the Seventh Schedule to these Regulations.

 

22.   Limits of variation

The limits of variation in respect of any prescribed analysis shall be as prescribed in the Eighth Schedule to these Regulations.

 

FIRST SCHEDULE

[Section 2]

DEFINITIONS IMPLIED ON THE SALE OF FARM FEED UNDER CERTAIN NAMES

Name of Farm Feed or Class of Feed

Implied Definition

Cereal brans

By-products produced in the milling of maize, wheat or other cereal kernels.

Oilseed cakes or meals (undecorticated)

Meals or cakes produced from the residues resulting from the removal of oil from undecorticated groundnuts, cottonseeds, sunflower seeds, soya beans or other oilseeds.

Oilseed cakes or meals (decorticated)

Meals or cakes produced from the residues resulting from the removal of oil from decorticated or partly decorticated groundnuts, cottonseeds, sunflower seeds, soya beans or other oilseeds.

Meat and bone meal

The product, containing not less than 40 per cent of protein (and not more than 4 per cent of salt) obtained by drying and grinding animal carcases or portions thereof (excluding hoof and horn) to which no other matter has been added, but which may have been treated previously for the removal of oil or fat.

Bone meal

Commercially pure bone, raw or degreased, which has been ground or crushed.

Meat meal

The product, containing not less than 55 per cent of protein (and not more than 4 per cent of salt) obtained by drying and grinding animal carcases or portions thereof (excluding hoof and horn) to which no other matter has been added but which may have been treated previously for the removal of oil or fat.

Fish meal

A product obtained by drying and grinding or otherwise treating fish or fish waste.

Molasses

A concentrated syrup product obtained in the manufacture of sugar from sugar cane, to which no other matter has been added.

Molasses feed

Any mixture (containing not less than 10 per cent of sugar) of an absorbent material and molasses.

Mixture of molasses

Any mixture of molasses and urea with or without any absorbent material.

Compound cakes and meals

A homogeneous mixture of two or more farm feeds. Concentrated or high A homogeneous mixture of two or more farm feeds or other substances energy farm feed intended to be mixed with some other farm feed before feeding to livestock.

NOTE:

"Commercially pure" means that no other matter has been added. In the case of every article mentioned in this Schedule the definition shall be deemed not to exclude the presence of a substance added to improve the keeping or handling properties of the farm feed or the presence of any coccidiostat, anti-blackhead remedy, natural or synthetic hormone.

"Synthetic hormone" means a synthetic compound which has similar properties to, or has the property of stimulating the production of, a natural hormone.

"Coccidiostat" means a substance used in the prevention or curative treatment of disease in poultry caused by protozoal organisms of the order coccidia.

"Anti-blackhead remedy" means a substance used in the prevention or curative treatment of infection in poultry due to Histomonas Meleagridis.

 

SECOND SCHEDULE

[Sections 28, 29 and 52K and regulations 12, 13 and 14]

STATEMENTS OF ANALYSIS REQUIRED FOR DIFFERENT CLASSES OF FARM FEED

Class of Farm Feed

Statement of Analysis

Cereal brands (undecorticated)

Percentages of protein, oil and fibre. Oilseed cakes or meals Percentages of protein and oil.

Oilseed cakes or meals (decorticated)

Percentages of protein, oil and fibre.

Meat and bone meal

Percentages of protein, oil and phosphorus.

Bone meal

Percentages of protein and phosphorus.

Meat meal

Percentages of protein, oil and phosphorus.

Fish meal

Percentages of protein, oil, phosphorus and salt.

Molasses

Percentage of sugar.

Molasses feed

Percentages of sugar and fibre.

Mixture of molasses and urea

Percentages of sugar and protein equivalent of urea.

Compound cakes and meals

Percentages of oil, fibre and protein (including the protein equivalent of urea, if any)

Concentrated or high energy feed

Percentages of oil, fibre and protein (including the protein equivalent of urea, if any); a statement of the proportions in which the feed should be mixed with other farm feed defined by name or class.

NOTES:

1. The amount of protein, except in the case of Compound Cakes and Concentrated or High Energy farm feed, means the amount of nitrogen other than ammoniacal, nitric or urea nitrogen, multiplied by 6.25. In the case of Compound Cakes and High Energy farm feed the amount of protein means the amount of nitrogen other than ammoniacal and nitric nitrogen multiplied by 6.25. The amount of protein equivalent of urea means the amount of urea nitrogen multiplied by 6.25.

2. In all cases the names of any added vitamins, minerals, antibiotics and synthetic or natural hormones shall be declared in the statement of analysis.

3. In all cases the maximum percentage of urea present in any farm feed shall be declared.

 

THIRD SCHEDULE

[Section 30 and regulation 14]

STATEMENTS OF ANALYSIS AND RECORDS TO BE KEPT FOR SALES UNDER TRADE NAMES, ETC.

Manufacturers of farm feeds shall keep records of all ingredients used in manufacturing any farm feed which is sold under a trade name, trade mark, trade label or trade brand. Such records shall be available for inspection at all reasonable times by a duly authorised officer, and shall be kept in such a manner as to enable the Registering Officer or any duly authorised officer to ascertain the materials from which any lot or batch of farm feed have been manufactured, and the proportions of such materials contained in the farm feed.

 

FOURTH SCHEDULE

[Section 52 and regulation 16]

DELETERIOUS INGREDIENTS IN FARM FEED

1. Salts soluble in water, if present in a farm feed in proportion likely to be injurious to the health of livestock.

2. All poisonous substances in quantities likely to be injurious to the health of livestock for which the farm feed is intended whether or not such substances are naturally present in the farm feed or material(s) from which the farm feed was manufactured.

3. Sand, siliceous matter or other insoluble mineral matter not naturally associated with ingredients of the farm feed which do not fall within the scope of this Schedule, or which, even if naturally so associated, are present in greater proportion than the maximum that may be expected to be due to such natural association.

4. For the purposes of this paragraph the term "insoluble" shall imply insolubility as determined by the prescribed method; the term "natural association" shall be construed as applying to average commercial samples of the farm feed or its ingredients with which it may be claimed that a particular mineral ingredient is associated.

 

FIFTH SCHEDULE

[Section 52 and regulation 17]

INGREDIENTS IN FARM FEED THE PRESENCE OF WHICH MUST BE DECLARED

1. Husks, chaff, glumes, hulls, nutshells or skins of nuts, from any source, whether ground or unground, treated or untreated, when used as separate ingredients or artificial mixtures in the manufacture of farm feed. Where the kernels naturally associated in seeds with one or other of the above materials are present in a farm feed along with material with which they are associated, regard shall be had to the proportion of the above materials that might reasonably be expected to accompany such kernels, when the seed from which they are derived is in its natural condition, provided that feeding in this condition is regarded as a common practice in the feeding of livestock.

2. Peat, peat moss or sugar cane pith, treated or untreated, ground or otherwise.

3. Wheat, maize or sorghum straw, maize rachis, ground or otherwise.

4. Sawdust or any other form of wood, treated or untreated.

 

SIXTH SCHEDULE

[Section 52(h) and regulations 19 and 20]

METHOD OR TAKING SAMPLES

NOTE - In this regulation "metric ton" is defined as 1,000 kg.

1. Where a farm feed is contained in packages the samples shall be taken from different parts of the whole quantity as follows:

   (a)   if the quantity does not exceed one ton, from not less than two unopened packages per ton or part thereof;

   (b)   if the quantity exceeds one ton but does not exceed two tons, from not less than four unopened packages;

   (c)   if the quantity exceeds two tons but does not exceed three tons, from not less than six unopened packages;

   (d)   if the quantity exceeds three tons, from one additional unopened package for every additional ton or part thereof, but in no case need samples be taken from more than 15 packages.

2. Where a farm feed is not contained in packages, a proportion calculated in accordance with paragraph 1 shall be taken from different parts of the whole quantity.

3. The samples shall be taken by means of a suitable sampling probe or by any other means as will ensure, as far as is practicable, the taking of a representative sample.

4. When a farm feed consists of material uneven in character, bulky or likely to get matted together, portions shall be taken from the selected packages, or from different parts of the farm feed if in bulk, any matted portions torn up, and all the portions thoroughly mixed together.

5. The samples thus taken shall be thoroughly mixed and reduced in size to give a final sample not exceeding six pounds in weight. This final sample shall be mixed and divided into three parts and each of these parts shall be transferred to a clean, dry, noncorrodible container capable of being closed in such a manner as to preserve the contents of the container in their original condition. These three containers shall be so sealed that they cannot be opened without breaking the seal. Each of these parts shall be marked with the name of the farm feed, date and place of sampling and the sample number together with the name of the inspector taking the sample.

6. When the farm feed is in liquid condition it should be thoroughly mixed before sampling. When in containers, samples shall be taken as follows:

Where the number of containers-

Portions shall be drawn from-

exceeds 1 but does not exceed 20

not less than 2 containers

exceed 20 but does not exceed 40

not less than 4 containers

exceed 40 but does not exceed 60

not less than 6 containers

exceed 60

one extra container for every 20 containers by which the total exceeds 60.

Where the farm feed is in liquid condition and is in bulk a representative sample shall be taken in accordance with the scale of sampling set out above.

The portions drawn shall be mixed together in a clean, dry container and a sample of 1 kg weight shall be taken. The sample shall be divided into three equal parts by pouring successive portions into each of three clear glass bottles or jars, preferably with wide mouths. The bottles or jars shall be provided with air-tight stoppers or with lids which shall be so fastened that spillage or evaporation of the contents is prevented. Each of the bottles or jars shall be so sealed that they cannot be opened without breaking the seal. Each of the bottles or jars shall be marked with the name of the farm feed, date and place of sampling and the sample number together with the name of the inspector taking the sample.

7. In the case of all samples the first part shall be given to the owner or seller of the farm feed or his agent, the second part shall be delivered to an approved analyst for analysis and the third part shall be retained by the inspector for a period of not less than six months after the date on which the report or certificate of analysis is issued.

8. A certificate of sampling (Form FERT 13 in the First Schedule to the Agriculture (Fertilisers) Regulations, 1969) shall be made out in triplicate at the time of sampling and the relevant copies as detailed in the form should accompany each part of the sample.

 

SEVENTH SCHEDULE

[Section 52(i) and regulation 21]

METHODS OF ANALYSIS

NOTE:

1. In this Schedule "water" means distilled or purified water except where stated.

2. Reagents should be of the appropriate analytical purity.

PREPARATION OF SAMPLE

   (a)   If the sample is in a fine condition and passes through a sieve having apertures of one millimetre square, it shall be thoroughly mixed and a portion not less than 100 grams in weight shall be placed in a stoppered bottle. From this portion the quantities for analysis shall be taken.

   (b)   If the sample does not wholly pass through a sieve having apertures of one millimetre square and wholly passes through a sieve having apertures of three millimetres square, it shall be thoroughly mixed and a portion for the determination of the moisture content shall be taken at once.

   (c)   If the sample is in a coarse condition as, for example, pieces of cake, it shall be carefully pulverised until the whole passes through a sieve having apertures of three millimetres square. It shall then be thoroughly mixed and a portion for the determination of the moisture content shall be taken at once.

   (d)   From the mixed sample as in (b) above, or from the coarsely crushed sample as in (c) above, a portion not less than 100 grams in weight shall be taken and further powdered and passed through a sieve having apertures of one millimetre square. The portion of the sample so prepared shall be placed in a stoppered bottle and from it the quantities for analysis shall be taken.

   (e)   If the original sample is appreciably moist, or if for any reason the operations of pulverisation and mixing are likely to result in loss or gain of moisture, the moisture in the bottled portion shall be determined as well as in the portion taken for that purpose under (b) or (c) above in order that the results of the analysis may be corrected to correspond with the original sample as regards moisture.

   (f)   Materials which cannot conveniently be pulverised or passed through a sieve shall be thoroughly mixed by the most suitable means.

DETERMINATION OF MOISTURE

A weighed quantity of the sample shall be dried at 100ºC and then be reweighed.

DETERMINATION OF OIL OR FAT (ETHER EXTRACT)

Reagents:

Petroleum ether-light petroleum-b.p. 40ºC to 60ºC.

NOTE - If ambient temperature of the laboratory demands then petroleum ether- light petroleum-of b.p.

60ºC to 80ºC may be used.

METHOD

Extract 2 to 5 grams of the sample, which has been dried for 1 hour at 100ºC, in a Soxhlet extraction apparatus with petroleum ether for a period of at least 6 hours. After evaporation of the solvent, dry the oil or fat for 30 minutes at 100ºC, cool in a desiccator and weigh. Calculate the oil or fat percentage as follows:

where A = weight in grams of the Soxhlet flask after extraction

B = weight in grams of the Soxhlet flask before extraction

C = weight in grams of the sample taken.

DETERMINATION OF FIBRE

Reagents:

Sulphuric acid solution - Prepare a solution containing 1.25 grams of sulphuric acid per 100 ml from chemically pure sulphuric acid. (0.255N).

Sodium hydroxide solution - Prepare a solution containing 1.25 grams of sodium hydroxide from carbonate-free sodium hydroxide. (0.313N).

Dilute hydrochloric acid solution (1:100). Ethyl alcohol (95 per cent v/v).

METHOD

Transfer a 2 to 3 gram sample, from which the bulk of the oil or fat has been extracted, to a conical flask (1 litre). Measure 200 ml of the sulphuric acid solution and heat to boiling; add to the flask, connect the flask to a condenser and heat. Bring the contents of the flask to boiling within one minute and boil gently and continuously for exactly 30 minutes. Rotate the flask at intervals of about 5 minutes to mix the contents thoroughly; do not allow any material to adhere to the sides of the flask out of contact with the solution.

At the end of 30 minutes remove the flask and immediately filter with suction through a Whatman No. 54 or No. 541 filter paper (or equivalent) fitted to a Hartley funnel or Buchner funnel. The time of filtration of the bulk of the 200 ml of liquid should not exceed 10 minutes. Wash with boiling water until the washings are free from acid.

Wash the material back into the flask with 200 ml of sodium hydroxide solution (measured at ordinary temperature and heated to boiling point). Boil again for exactly 30 minutes, observing the precautions stated for the acid treatment.

At the end of 30 minutes, remove the flask and immediately either filter direct through a suitable filter crucible or through filter paper and then transfer the charge to a filter crucible for washing. Wash thoroughly with boiling water, then with dilute hydrochloric acid solution, again with boiling water until free from acid and finally three times with ethyl alcohol.

Dry the crucible and residue for 2 hours at 100ºC, cool in a desiccator and weigh. Ignite until free from carbonaceous matter at a temperature not exceeding 600ºC, cool in a desiccator and weigh.

Calculate the percentage of fibre as follows:

Where A = weight in grams of residue after drying

B = weight in grams of residue after washing

C = weight in grams of the sample taken.

DETERMINATION OF ASH

Weigh out accurately 2 to 5 grams of the sample into a tared porcelain or silica dish, previously heated to a temperature of 500ºC and cooled. Char carefully and ignite in a muffle furnace at a temperature of

500ºC for 2 hours or until combustion is complete. Cool in a desiccator and weigh. Calculate the

percentage of ash as follows:

Where A = weight in grams of wash

B = weight in grams of the sample taken.

DETERMINATION OF SALT

Mix 5 grams of the sample with 1 gram of pure sodium carbonate or calcium oxide and thoroughly wet the mixture with a little water. Dry the mixture and heat at a temperature not exceeding 500ºC in order to destroy organic matter. Extract the residue with hot water, make up the volume to 250 ml and filter. Determine the chlorine in an aliquot part of the filtrate and express the result in terms of sodium chloride (NaCl).

DETERMINATION OF PHOSPHORUS

Phosphorus may be determined by either of the matter described below.

QUINOLINIUM PHOSPHOMOLYBDATE METHOD

Reagents:

Calcium oxide - finely ground.

Citric - molybdate acid solution-Stir 54 g of molybdenum trioxide (MoO3) with 200 ml of water; add 11 g sodium hydroxide and stir the mixture whilst heating to boiling point until the molybdenum trioxide dissolves. Dissolve 60 g citric acid in about 250 to 300 ml water and add 140 ml concentrated hydrochloric acid. Pour the molybdate solution into the acid solution, which is stirred throughout the addition. Then cool and, if necessary, filter the solution through a 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 or 1 per cent) solution of potassium bromate until the colour is discharged. This reagent should be kept in the dark.

Hydrochloric Acid, concentrated (S.G. 1.18).

Hydrocloric Acid 25 per cent v/v-Dilute 25 ml of concentrated hydrochloric acid with water to 100 ml. Hydrochloric Acid, 0.5N.

Hydrochloric Acid, 0.1N.

Indicator Solution - Mix 3 volumes of thymol blue solution and 2 volumes of phenolphthalein solution prepared as follows:

Thymol blue solution - Dissolve 0.25 g thymol blue in 5.5 ml of 0.1N sodium hydroxide solution and 125 ml industrial methylated spirit. Dilute with water to 250 ml. Phenolphthalein solution-Dissolve 0.25 g phenolphthalein in 150 ml of industrial methylated spirit and dilute with water to 250 ml.

Reagents:

Nitric Acid, concentrated (S.G. 1.42).

Quinoline Solution - Measure 60 ml concentrated hydrochloric acid and 300 to 400 ml water into a 1 litre beaker and warm to 70º-80ºC. Pour 50 ml quinoline in a thin stream into the diluted acid, whilst stirring. When the quinoline has dissolved, cool the solution, dilute to 1 litre and, if necessary, filter through a paper pulp filter.

Sodium Hydroxide, 5N.

Sodium Hydroxide, 0.5N - carbonate free.

Sodium Hydroxide, 0.1N-carbonate free.

Surface Active Agent - 0.5 per cent solution of sodium dodecylbenzene-sulphonate is suitable.

DISSOLUTION OF THE SAMPLE

Weigh to the nearest mg about 5 g of the sample into a capsule or dish; add 1 g of calcium oxide, mix well and thoroughly wet with a little water. Dry the mixture and incinerate at a temperature not exceeding 500ºC until completely charred. Cool, transfer the contents of the capsule or dish to a 250 ml beaker and add 10 ml water; then slowly add 12 ml of concentrated hydrochloric acid, taking suitable precautions to avoid loss by effervescence, and finally add 5 ml concentrated nitric acid. Heat to incipient boiling and keep at this temperature for 10 minutes. Dilute with about 10 ml water, filter, transfer the insoluble matter to the filter paper with a minimum amount of water and wash twice with small volumes of water. Then transfer the filter paper and insoluble matter to the original capsule or dish and incinerate until all the carbon is destroyed. Combine the ash with the filtrate and heat to boiling point. Cool, transfer to a 250 ml volumetric flask, dilute to the mark, mix well and filter. Discard the first 10 or 20 ml of the filtrate.

METHOD

Transfer a volume of the filtrate containing less than 30 mg phosphorus (P) and preferably about 22 mg phosphorus (P) to 500 ml stoppered conical flask marked at 150 ml. Dilute solution with water to 100 ml and 5N sodium hydroxide solution until a faint permanent turbidity or precipitate is formed. Dissolve the precipitate by the dropwise addition of 25 per cent hydrochloric acid, but avoid an excess.

Dilute to 150 ml, add 50 ml of the citric-molybdate solution, heat to incipient ebullition, maintain it at this temperature for 3 minutes and then bring it to boiling point. From a burette slowly add 25 ml of the quinoline solution with constant swirling throughout, the first few ml being added dropwise, the rest in a slow stream. Keep the solution gently boiling during the addition.

Immerse the flask in boiling (tap) water for 5 minutes, then cool it to 15ºC in running tap water. 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. Transfer the filter pad and precipitate to the original flask, rinse the funnel with water and collect the rinsings in the flask. If necessary, wipe the funnel with a small piece of damp filter paper to ensure complete removal of the precipitate, and place the paper in the flask. Add water to a total of about but not exceeding 100 ml. Stopper the flask and shake it vigorously until the pulp and precipitate are completely dispersed.

Remove the stopper and wash it with water, returning the washings to the flask. Add a measured volume of 0.5N sodium hydroxide solution sufficient to dissolve the precipitate and leave a few ml in excess. Shake the flask vigorously until all the precipitate dissolves. (To facilitate the dispersal of the precipitate after the addition of the 0.5N sodium hydroxide solution, a few drops of the surface active agent may be added if necessary.) Add 0.5-1.0 ml of the indicator solution, and titrate the excess of sodium hydroxide with the 0.5N hydrochloric acid until the indicator changes from violet to green-blue and then very sharply to yellow at the end-point. Deduct the number of ml of 0.5N hydrochloric acid used from the number of ml of 0.5N sodium hydroxide to ascertain the volume of 0.5N sodium hydroxide equivalent to the phosphorus.

Carry out a blank determination on all the reagents, omitting only the sample, and using 0.1N standard alkali and acid instead of 0.5N for the titration. Calculate the amount of phosphorus in the portion taken for analysis from the factor 1.0 ml of 0.5N sodium hydroxide = 0.597 mg P (1.366 mg P2O5).

Reagents:

Calcium Oxide - finely ground.

Hydrochloric Acid, concentrated (S.G. 1.18).

Nitric Acid, concentrated (S.G. 1.42).

Potassium Dihydrogen Phosphate Solution (stock phosphate solution)-Dissolve in water 1.917 g of potassium dihydrogen phosphate previously dried at 105ºC for 1 hour and dilute to 1 litre.

Potassium Dihydrogen Phosphate Solution (standard phosphate solution) - Dilute 50 ml of stock solution to 250 ml with water. 1 ml of this solution = 0.0874 mg phosphorus (0.2 mg P2O5).

Vanado-Molybdate Reagent - Dissolve separately 20 g of ammonium molybdate and 1 g of ammonium vanadate in water, mix, acidify with 140 ml of concentrated nitric acid and dilute to 1 litre.

STANDARDISATION OF INSTRUMENT

From a burette measure into a series of 100 ml volumetric flasks 25.0, 26.0, 27.0, 28.0, 30.0 and 31.0 ml of the standard phosphate solution (i.e. 0.219, 0.227, 0.236, 0.245, 0.254, 0.262 and 0.271 mg phosphorus, corresponding to 5.0, 5.2, 5.4, 5.6, 5.8, 6.0 and 6.2 mg P2O5). Add 25 ml of the vanado- molybdate reagent to each flask and dilute to 100 ml with water. Shake and allow to stand for 10 minutes.

Set the spectrophotometer to the correct wavelength, about 4,200, fill two 1 cm cells with the 0.219 mg solution and check the extinction of the cells. If there is a small difference select the cell with the smaller reading as the standard reference cell.

Determine the apparent extinction (corrected for cell differences) of the 0.227, 0.236, 0.245, 0.254, 0.262 and 0.271 mg phosphorus solutions referred to the 0.219 mg phosphorus solution as standard. Plot a calibration graph of scale readings against known phosphorus content.

ANALYSIS OF THE SAMPLE

Successively dilute a portion of the solution prepared as described under "Dissolution of the Sample" so that the final volume of about 25 ml contains between 2.404 and 2.709 mg of phosphorus (corresponding to 5.5 and 6.2 mg P2O5 respectively).

Transfer this final volume to a 100 ml volumetric flask, add 25 ml of the vanado-molybdate reagent, dilute to the mark, mix, and allow to stand for 10 minutes. At the same time transfer 25 ml of the standard phosphorus solution into a second 100 ml volumetric flask. Add 25 ml of the vanado- molybdate reagent, dilute to the mark, mix, and allow to stand for 10 minutes.

Measure the difference in extinction between the two solutions and estimate the phosphorus content of the volume of the unknown solution from the calibration graph. Calculate the phosphorus content of the sample from the known dilution factors and the weight of the sample.

NOTE - Prepare a fresh reference standard for each series of readings on the instrument.

DETERMINATION OF PROTEIN

The percentage of protein, except in the case of compound cakes or meals and concentrated or high energy farm feed, shall be ascertained by multiplying the percentage of nitrogen, other than nitrogen present as ammoniacal, nitric or urea nitrogen, by 6.25. The presence of nitrogen in these latter forms shall be tested for and the quantity, if any, shall be determined and deducted from the total nitrogen.

In the case of compound cakes or meals and concentrated or high energy farm feed the percentage of protein shall be ascertained by multiplying the percentage of nitrogen, other than nitrogen present as ammoniacal or nitric nitrogen, by 6.25. The presence of nitrogen in these latter forms shall be tested for and the quantity, if any, shall be determined and deducted from the total nitrogen.

NITROGEN

Reagents:

Mixed Indicator Solution - Grind together in an agate mortar 0.6 g of methyl red and 0.6 g of methylene blue. Dissolve the mixture in 500 ml of 95 per cent ethanol. Shake, filter and store in a dark glass bottle.

2 per cent Boric acid solution - Dissolve 20 g of boric acid in water, dilute to 1 litre and add 5 ml of the mixed indicator solution. Concentrated sulphuric acid S.G. 1.84.

Anhydrous sodium sulphate.

Cupric sulphate.

Paraffin wax.

Granulated zinc.

Hydrochloric acid 0.1N.

Sodium Hydroxide solution-50 per cent w/v.

METHOD

Weigh accurately 1 to 2 g of the sample (or such an amount as shall not contain more than 250 mg of nitrogen) and transfer to a kjeldahl flask. Add 25 ml of concentrated sulphuric acid and approximately 10 g of anhydrous sodium sulphate containing 0.4 g of cupric sulphate. Heat gently until frothing ceases, then strongly until the solution becomes clear and almost colourless. Continue heating for at least another hour. Avoid local overheating. If frothing is excessive, add about 0.5 g paraffin wax.

Dissolve the cooled digest in water and make up to a total volume of about 250 ml. Taking precautions against loss of ammonia add some zinc granules and sufficient 50 per cent sodium hydroxide solution to neutralise the acid and to give about 10 ml in excess, mix well and immediately connect to a distillation apparatus. Distil into an appropriate volume of 2 per cent boric acid solution. Titrate the contents of the receiving flask with 0.1N hydrochloric acid. Carry out a blank test using 2 g of sucrose in the place of the sample, and subtract the titration value of the blank from that of the sample. Express the result in terms of nitrogen.

1 ml of 0.1N hydrochloric acid = 0.0014 g nitrogen.

UREA NITROGEN

Reagents:

Activated charcoal.

Carrez solution 1 - Dissolve 21.9 g zinc acetate dihydrate in water, add 3 ml glacial acetic acid and dilute to 100 ml with water.

Carrez solution 2 - Dissolve 10.6 g potassium ferrocyanide in water and dilute to 100 ml. p- Dimethylaminobenzaldehyde solution-Dissolve 2 g of p - Dimethylaminobenzaldehyde in 10 ml of concentrated hydrochloric acid and dilute to 100 ml with propan-2-ol.

Hydrochloric acid-0.02N.

Sodium acetate solution - Dissolve 136 g sodium acetate (CH3COONa.3H2O) in water and dilute to 1 litre.

Urea standard solution - Dissolve 1 g urea in water and dilute to 100 ml.

METHOD

Weight to the nearest mg about 5 g of the sample (or such an amount as shall contain not more than 250 mg urea) and transfer to a 250 ml volumetric flask. Add 150 ml of 0.02N hydrochloric acid, shake for 30 minutes then add 10 ml of sodium acetate solution and mix well. Add 1 g of activated charcoal (see Note) to the flask and shake well, and stand for a further 15 minutes. Add 5 ml of Carrez solution 1, followed by 5 ml of Carrez solution 2 mixing well between additions. Dilute to volume with water and mix well. Filter a portion through a suitable dry filter paper into a dry clean 250 ml beaker. Transfer a 10 ml aliquot of the filtrate to a 50 ml flask, add 10.0 ml of p-dimethylaminobenzaldehyde solution, dilute to 50 ml with water, mix well and allow to stand for 10 minutes. Determine the extinction of the solution at 4,350 using a 1 cm cell against a blank of 10 ml of p-dimethylaminobenzaldehyde reagent

diluted to 50 ml with water. Calculate the urea content of the sample by reference to a calibration graph prepared at the same time as the test sample. (mg urea multiplied by 0.4665 = mg urea nitrogen.)

Establish the calibration graph as follows:

Measure amounts of standard urea solution corresponding to 50, 100, 150, 200 and 250 mg of urea into a series of 250 ml volumetric flasks and proceed as described above commencing at "Add 150 ml 0.02N hydrochloric acid".

Measure the extinctions of the solutions, and construct a graph relating the extinctions to the mg of urea.

NOTE - If the sample is highly coloured the proportion of activated charcoal must be increased up to 5 g. The final solution after filtering should be colourless.

DETERMINATION OF SUGAR

Reagents:

Fehling's solution - Mix equal volumes of a solution of copper sulphate and a solution of sodium potassium tartrate prepared as follows:

Copper sulphate solution-Dissolve 69.28 g of copper sulphate (CUSO4.5H2O) in water and dilute to 1 litre.

Sodium potassium tartrate solution - Dissolve 346 g of sodium potassium tartrate and 100 g of sodium hydroxide in water and dilute to 1 litre.

NOTE - The strength of the Fehling's solution should be such that 10 ml is equivalent to 0.0525 g invert sugar. It should be checked by titrating with a solution of pure sucrose (inverted by the procedure described in the note following the paragraph on "Exact Determination" below) using the procedure described in the paragraph.

Hydrochloric acid N.

Methylene blue solution - Dissolve 2.5 g methylene blue in water and dilute to 250 ml.

Phenolphthalein indicator solution-Dissolve 0.25 g of phenolphthalein in 150 ml of industrial methylated spirit and dilute with water to 250 ml.

Potassium ferrocyanide solution-Dissolve 106 g of potassium ferrocyanide in water and dilute to 1 litre. Potassium oxalate solution-Dissolve 50 g of potassium oxalate in water and dilute to 1 litre.

Sodium hydroxide, 10 per cent w/v-Dissolve 100 g of sodium hydroxide in water and dilute to 1 litre.

Zinc acetate solution-Dissolve 219 g of zinc acetate and 30 ml of glacial acetic acid in water and dilute to 1 litre.

PROCEDURE

Preparation of sample.

WHEN THE SUBSTANCE IS IN SOLID FORM

Weigh to the nearest centigram about 10 g of the sample or a sufficient quantity to contain about 2 g of sugar. Grind in a mortar with hot water (temperature not to exceed 60ºC) and transfer to a 500 ml volumetric flask using in all about 400 ml of water. Shake the flask at intervals during 30 minutes. Add 5 ml of potassium oxalate solution to the contents of the flask, followed by 5 ml of zinc acetate solution; mix well and then add 5 ml of potassium ferrocyanide solution, make up with water to 500 ml at the correct temperature, mix well and filter. Determine the sugar in 100 ml of the filtrate by the method described below.

WHEN THE SUBSTANCE IS IN LIQUID FORM

Weigh to the nearest mg about 5 g of the sample and wash with water into a 250 ml volumetric flask using about 200 ml of water. To clear the solution add 5 ml of zinc acetate solution. Mix, then add 5 ml of potassium ferrocyanide solution, again mix, dilute to 250 ml, mix and filter. Determine the sugar in 25 ml of the filtrate by the method described below.

DETERMINATION OF THE SUGAR CONTENT

Transfer the measured volume of filtrate obtained as described above to a suitable beaker, add 15 ml of N hydrochloric acid, dilute to 150 ml with water, cover with watch glass and heat to boiling point. Continue to boil for 2 minutes, cool, add 2 or 3 drops of phenolphthalein indicator solution, just neutralise with 10 per cent sodium hydroxide solution, transfer to a 200 ml volumetric flask and dilute to 200 ml. Filter if necessary.

PRELIMINARY ESTIMATION

(This estimation is usually necessary where the percentage of sugar is unknown.) Transfer exactly 10 ml of Fehling's solution to a 250 ml conical flask and add 20 ml of water. Add from a burette approximately10 ml of the filtrate prepared as described above, heat to boiling point and boil briskly for 1 minute. Add 3 drops of methylene blue solution and titrate from the burette at the rate of 1 ml per 15 seconds until the blue colour is discharged, the contents of the flask being kept boiling throughout the titration. Note the total number of ml required and call this x ml. This titration should not be outside the range of 15-40 ml otherwise the determination should be repeated using a more appropriate volume of the filtrate.

EXACT DETERMINATION

To 10 ml of Fehling's solution in a 250 ml conical flask add from burette (x-1) ml of the filtrate, together with sufficient water to make a total volume of 60 ml. Heat to boiling point, boil briskly for 11/2 minutes and add 3 drops of methylene blue solution. Titrate from the burette at a rate of approximately 0.25 ml per 15 seconds until the blue colour is discharged, the contents of the flask being kept boiling briskly throughout the titration which must not take more than 11/2 minutes. Then the total number of ml used in the determination equals the sugar equivalent of 10 ml of Fehling's solution.

10 ml of Fehling's solution=0.0525 g invert sugar.

Not more than 1 ml of filtrate should be required for completion of the titration. If more than 1 ml is required then the determination should be repeated using a more closely calculated volume of filtrate for the original addition. The time taken from the initial boiling point until the end of the titration should be about 3 minutes. If this time is exceeded by more than about 20 seconds, the titration should be repeated.

The total copper reducing power should finally be determined in terms of sugar (C12H22O11). NOTE-The Fehling's solution may be standardised as follows:

Dissolve 2.375 g sucrose (dried at 100ºC) in about 100 ml of water in a suitable beaker, add 15 ml of N hydrochloric acid and sufficient water to give a volume of 150 ml. Heat to boiling point, boil for 2 minutes, cool, add 2 or 3 drops of phenolphthalein solution, just neutralise with 10 per cent sodium hydroxide solution, transfer to a 500 ml volumetric flask, dilute to 50 ml. then follow the procedure described in "Exact Determination" above.

1 ml of the solution = 0.00475 invert sugar, i.e., 10 ml of Fehling's solution = 10.5 ml of this standard invert sugar solution.

DETERMINATION OF SAND, SILICEOUS MATTER OR OTHER INSOLUBLE MINERAL MATTER

Reagents:

Hydrochloric acid, concentrated, S.G. 1.18.

Hydrochloric acid, 25 per cent v/v - Dilute 25 ml of concentrated hydrochloric acid with water to 100 ml.

PROCEDURE

Weigh to the nearest mg from 2-5 g of the sample and incinerate until all the carbon has been destroyed. (The ash obtained from the method for "Determination of Ash" may be used for this determination.) Moisten with concentrated hydrochloric acid, evaporate to dryness, bake to render the silica insoluble, and then extract repeatedly with hot 25 per cent hydrochloric acid. Filter, wash the insoluble matter and weigh. Regard the quantity obtained as sand and siliceous matter.

 

EIGHTH SCHEDULE

[Section 52(g) and regulation 22]

LIMITS OF VARIATION

Farm Feed

Limits of Variation

Cereal brands   . .   . .   . .

Protein, one tenth of the amount stated. Oil, 0.75 per cent or one tenth of the amount stated, whichever is the greater. Fibre, one eighth of the amount stated.

Oilseed meals or cakes (undecorticated)   . .   . .

Protein, one tenth of the amount stated. Oil, 0.75 per cent or one tenth of the amount stated, whichever is the greater.

Oilseed meals or cakes (decorticated)   . .   . .   . .

Protein, one tenth of the amount stated. Oil, 0.75 per cent or one tenth of the amount stated, whichever is the greater. Fibre, one eighth of the amount stated.

Meat and bone meal   . .   . .

Protein, one tenth of the amount stated. Oil, 0.75 per cent or one tenth of the amount stated, whichever is the greater. Phosphorus, one tenth of the amount stated.

Bone meal   . .   . .   . .

Protein, one tenth of the amount stated.

Meat meal   . .   . .   . .

Phosphorus, one tenth of the amount stated. Protein, one tenth of the amount stated. Oil, 0.75 per cent or one tenth of the amount stated, whichever is the greater.

Fish meal   . .   . .   . .

Protein, one tenth of the amount stated. Oil, 0.75 per cent or one tenth of the amount stated, whichever is the Salt, 0.75 greater. Phosphorus, one tenth of the amount stated. percent.

Molasses   . .   . .   . .

Sugar, one twentieth of the amount stated.

Molasses feed   . .   . .   . .

one eighth of the Sugar, one tenth of the amount stated. Fibre, amount stated.

Mixtures of molasses and
urea   . .   . .   . .   . .

Sugar, one tenth of the amount stated. Protein equivalent of urea, one fifth of the amount stated.

Compound cakes and meals,
and    . .   . .   . .   . .

Protein, one tenth of the amount stated. Protein, concentrated or one feed, high energy farm equivalent of urea, 1.25 per cent or tenth of the fifth of the amount stated. Oil, 0.75 per cent or one eighth of amount stated, whichever is the greater. Fibre, one the amount stated.

{/mprestriction}


 

CHAPTER 226 - AGRICULTURE (FERTILISERS AND FEED) ACT: SUBSIDIARY LEGISLATION

 

INDEX TO SUBSIDIARY LEGISLATION

Agriculture (Fertilisers) Regulations

Agriculture (Farm Feed) Regulations

 

AGRICULTURE (FERTILISERS) REGULATIONS

[Section 52]

[Currency mentioned in this regulation should be re-denominated as stipulated under S 4 of Re-denomination Act, 2012, read with S 29 of Bank of Zambia Act, 1996.]

Arrangement of Regulations

   Regulation

PART I
PRELIMINARY

   1.   Title

   2.   Application

PART II
REGISTRATION OF PLANT

   3.   Registration of plant and fees

   4.   Register of plant

   5.   Requirements of plant

PART III
ANALYSTS AND LABORATORIES

   6.   Approval of analysts

   7.   Approval of laboratories

   8.   Roll of analysts

   9.   Roll of laboratories

PART IV
SEARCHES AND SEIZURES

   10.   Certificates of authority for inspectors

PART V
SALE OF FARMING REQUISITES

   11.   Statements of analysis for sales in bags, containers, etc.

   12.   Statements of analysis for sales in bulk

   13.   Statements of analysis for sales under trade names, etc.

PART VI
SAMPLING, ANALYSIS AND LIMITS OF VARIATION

   14.   Form of report to be used

   15.   Form of certificate to be used

   16.   Method of taking samples

   17.   Methods of analysis

   18.   Limits of variation

      FIRST SCHEDULE

      SECOND SCHEDULE

      THIRD SCHEDULE

      FOURTH SCHEDULE

      FIFTH SCHEDULE

      SIXTH SCHEDULE

[Regulations by the Minister]

Act 13 of 1994,

SI 476 of 1969,

SI 117 of 1970.

 

PART I
PRELIMINARY

 

1.   Title

These Regulations may be cited as the Agriculture (Fertilisers) Regulations.

 

2.   Application

These Regulations shall apply to any fertiliser as defined in section 2 of the Act.

 

PART II
REGISTRATION OF PLANT

 

3.   Registration of plant and fees

   (1) Applications under Part II of the Act for registration, transfer of registration or renewal of registration of plant shall be made in Form FERT. 4 in the First Schedule, and such application shall be accompanied by the appropriate fees shown in the First Schedule and the Second Schedule to the Act, and be given to the Registering Officer.

   (2) The Registering Officer shall issue a certificate of registration in Form FERT. 5 in the First Schedule.

   (3) The Registering Officer shall issue a certificate of provisional registration in Form FERT. 6 in the First Schedule.

 

4.   Register of plant

The Registering Officer shall keep a register of plant as prescribed in Form FERT. 1 in the First Schedule.

 

5.   Requirements of plant

Any plant within the definition in section 2 of the Act shall be so equipped as to permit the adequate performance therein of the activities described in the application for registration of such plant, to the satisfaction of the Registering Officer.

 

PART III
ANALYSTS AND LABORATORIES

 

6.   Approval of analysis

   (1) For the purposes of the Act, an analyst shall furnish proof to the satisfaction of the Minister that he has competent knowledge of chemistry and of chemical analyses, as applied to fertilisers. Such proof shall in every case comprise documentary evidence that such person holds a certificate or diploma attesting his possession of the requisite knowledge and given by a recognised competent body. All such documentary evidence shall be submitted to the Minister when applying for approval. The Minister may call for further evidence if required in any particular case.

   (2) Where the requirements referred to in sub-regulation (1) are satisfied, the Registering Officer shall issue a certificate of approval in Form FERT. 7 in the First Schedule.

 

7.   Approval of laboratories

   (1) An approved laboratory shall be so equipped as to enable approved analysts to perform accurately for the purposes of the Act all the analyses specified under the Third Schedule, and such laboratories shall have been inspected by a duly authorised officer of the Ministry of Agriculture before approval by the Minister and may be inspected from time to time as the Registering Officer may deem necessary:

Provided that, in addition, other laboratories may be approved for certain analyses only, such analyses to be specified by the Registering Officer after inspection by a duly authorised officer of the Ministry of Agriculture.

   (2) Where the Minister approves a laboratory, the Registering Officer shall issue a certificate of approval in Form FERT. 8 in the First Schedule.

 

8.   Roll of analysts

The Registering Officer shall keep a roll of approved analysts in Form FERT. 2 in the First Schedule.

 

9.   Roll of laboratories

The Registering Officer shall keep a roll of approved laboratories in Form FERT. 3 in the First Schedule.

 

PART IV
SEARCHES AND SEIZURES

 

10.   Certificates of authority for inspectors

The certificate of authority to be held by inspectors under section 25 of the Act shall be issued by the Registering Officer and shall be"”

   (a)   in the case of general authorisation, in Form FERT. 11 in the First Schedule; and

   (b)   in the case of limited authorisation, in Form FERT. 12 in the First Schedule.

 

PART V
SALE OF FARMING REQUISITES

 

11.   Statements of analysis for sales in bags, containers, etc.

The statement of analysis for each class of fertiliser as defined in the Fifth Schedule shall appear in English in lettering both durable and legible on the bag or container containing the same or on a label securely attached thereto.

 

12. Statements of analysis for sales in bulk

Where any class of fertiliser as defined in the Fifth Schedule is sold in bulk, the statement of analysis for such class shall appear in English in lettering both durable and legible on a note which shall be given to the purchaser or his agent at the time of delivery of such fertiliser.

 

13.   Statements of analysis for sales under trade names, etc.

Where any class of fertiliser as defined in the Fifth Schedule is sold in a container or a package under a trade name, trade mark, trade label or trade brand, as provided by section 30 of the Act, there shall appear in English in lettering both legible and durable on the container or package or on a label securely attached thereto, a statement of analysis in respect thereof and, in addition, there shall be lodged with the Registering Officer, in respect of such fertiliser, a statement of particulars specified in the Sixth Schedule.

 

PART VI
SAMPLING, ANALYSIS AND LIMITS OF VARIATION

 

14.   Form of report to be used

A report of analysis shall be issued by the analyst performing the analysis in respect of every sample taken under the Act, and any such report shall be in Form FERT. 9 in the First Schedule.

 

15.   Form of certificate to be used

A certificate of analysis shall not be issued unless the sample has been taken in accordance with the Second Schedule and such certificate shall be in Form FERT. 10 in the First Schedule.

 

16.   Method of taking samples

Samples for analysis for the purposes of the Act shall be taken in the manner prescribed in the Second Schedule and certificates of sampling issued in relation thereto shall be in Form FERT. 13 in the First Schedule.

 

17.   Method of analysis

Methods of analysis shall be as prescribed in the Third Schedule.

 

18.   Limits of variation

The limits of variation in respect of any prescribed analysis shall be as prescribed in the Fourth Schedule.

 

FIRST SCHEDULE

CERTIFICATES AND FORMS

 

FORM FERT. 1

REPUBLIC OF ZAMBIA

AGRICULTURE (FERTILISERS AND FEED) ACT

AGRICULTURE (FERTILISERS) REGULATIONS

[Section 4 and Regulation 4]

REGISTER OF PLANT

Certificate Number and Date

Location

Name and Purposes for which Registered

Address of registered owner

Remarks (e.g., if only provisional)

         

 

 

 

FORM FERT. 2

REPUBLIC OF ZAMBIA

AGRICULTURE (FERTILISERS AND FEED) ACT

AGRICULTURE (FERTILISERS) REGULATIONS

[Section 20(a) and Regulation 8]

ROLL OF APPROVED ANALYSTS AND ANALYSTS APPROVED FOR SPECIAL TECHNIQUES

Name

Address

Recognised qualifications

Purposes for which approved (general or special)

Date approved

Certificate Number

Remarks

             

NOTE.-Date of withdrawal of approval shall be noted in "Remarks" column opposite the analyst.

 

FORM FERT. 3

REPUBLIC OF ZAMBIA

AGRICULTURE (FERTILISERS AND FEED) ACT

AGRICULTURE (FERTILISERS) REGULATIONS

[Section 20(b) and Regulation 9]

ROLL OF APPROVED LABORATORIES

Name and address of Laboratory

Names of approved analysts attached to laboratory

Purposes for which approved

Date of withdrawal

Certificate Number

Remarks (e.g. types of analysis)

           

 

 

FORM FERT. 4

REPUBLIC OF ZAMBIA

AGRICULTURE (FERTILISERS AND FEED) ACT

AGRICULTURE (FERTILISERS) REGULATIONS

[Sections 5(1), 11(1), (3), 17(1), (2) and Regulation 3]

APPLICATION FOR REGISTRATION, TRANSFER OF REGISTRATION OR RENEWAL OF REGISTRATION

Name of applicant .................................................................................................................

Address ................................................................................................................................

Address of plant ...................................................................................................................

Nature of activities to be carried out in plant ........................................................................

...............................................................................................................................................

...............................................................................................................................................

Owner of plant ......................................................................................................................

Address of owner .................................................................................................................

Please state whether you are applying for*"”

 

Fee units

   (a)   First registration of plant . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

60

   (b)   Annual renewal of registration of plant . . . . . . . . . . . . . . . . . . . . . . . . .

30

   (c)   Provisional registration of a plant . . . . . . . . . . . . . . . . . . . . . . . . . . . .

30

   (d)   Provisional registration of a transferee from, or successor in interest to a registered owner, as registered owner on the register of plant . . . . . . . . . .

30

   (e)   Full registration of a transferee from, or successor in interest to a registered owner, as registered owner on the register of plant . . . . . . . . . . . . . . . . .

60

NOTE.-Fees should accompany this application.

* Strike out those inapplicable.

FOR OFFICIAL USE ONLY

Ref. No. ............................................................. Date received ............................................

 

Fee units

First registration........................................

60

Renewal.....................................................

30

Transfer (Provisional)...............................

30

Transfer (Full) ...........................................

60

Provisional registration.............................

30

Fee paid ................................................... Date....................................................................

Inspection by .......................................................................................................................

Remarks .............................................................................................................................

Certificate issued by ...........................................................................................................

Certificate No. ........................................ Date ....................................................................

NOTES:

1. This form should be used when applying for registration of any plant or plant ownership.

2. Where a plant is owned by more than one person then one person should be nominated and registered as owner for the purposes of the Act.

3. After this application has been received your plant will be inspected and you will be informed whether or not your plant has been approved for registration with or without conditions.

4. If such an inspection is not immediately practicable your application for registration may be classed as "provisional".

[Am by Act 13 of 1994.]

 

FORM FERT. 5

REPUBLIC OF ZAMBIA

AGRICULTURE (FERTILISERS AND FEED) ACT

AGRICULTURE (FERTILISERS) REGULATIONS

[Section 10(1) and Regulation 3]

CERTIFICATE OF REGISTRATION OF PLANT

This is to certify that the plant situated at .............................................................................

and used for the purpose of ..................................................................................................

and owned by .................................. has been inspected, approved and registered for the purposes of the Act.

This certificate should be displayed in a prominent place in the plant.

..................................................................

Registering Officer

Date ......................................

No. ........................................

Receipt No. ...........................

 

FORM FERT. 6

REPUBLIC OF ZAMBIA

AGRICULTURE (FERTILISERS AND FEED) ACT

AGRICULTURE (FERTILISERS) REGULATIONS

[Sections 8 and 9 and Regulation 3]

CERTIFICATE OF PROVISIONAL REGISTRATION OF PLANT

This is to certify that the plant situated at ................... and used for the purposes of ........................... and owned by ..................... has been provisionally registered for the purposes of the Act.

This certificate should be displayed in a prominent position in the plant.

..................................................................

Registering Officer

Date .......................................

No. .........................................

Receipt No. ............................

 

FORM FERT. 7

REPUBLIC OF ZAMBIA

AGRICULTURE (FERTILISERS AND FEED) ACT

AGRICULTURE (FERTILISERS) REGULATIONS

[Section 18(1) and Regulation 6]

CERTIFICATE OF APPROVAL OF ANALYST

This is to certify that the Minister of Agriculture, Food and Fisheries has approved ................................................

.................................................................... as an analyst for the purposes of the Act.

..................................................................

Registering Officer

Date .................................

No. ...................................

 

FORM FERT. 8

REPUBLIC OF ZAMBIA

AGRICULTURE (FERTILISERS AND FEED) ACT

AGRICULTURE (FERTILISERS) REGULATIONS

[Section 19(1) and Regulation 7]

CERTIFICATE OF APPROVAL OF LABORATORY

This is to certify that the Minister of Agriculture has approved .................................... as a laboratory for the purposes of the Act, subject to the following limitations ...................

..............................................................................................

..............................................................................................

..............................................................................................

..................................................................

Registering Officer

Date ................................

Roll No. ...................................

 

FORM FERT. 9

REPUBLIC OF ZAMBIA

AGRICULTURE (FERTILISERS AND FEED) ACT

AGRICULTURE (FERTILISERS) REGULATIONS

[Section 21 and Regulation 14]

REPORT OF ANALYSIS

I certify that I received on ............................................ 20..........., a sample of ......................................................................... from ..............................................................

The report is as follows:

Laboratory number ....................................................

Sample number .........................................................

...............................................................................................................................................

...............................................................................................................................................

...............................................................................................................................................

...............................................................................................................................................

...............................................................................................................................................

...............................................................................................................................................

Date ....................................................

.................................................

 

Analyst

NOTE.-To be completed in triplicate and copies despatched as follows:

Original - Owner or Seller.

Duplicate - Inspector.

Triplicate - To be retained by Analyst.

 

FORM FERT. 10

REPUBLIC OF ZAMBIA

AGRICULTURE (FERTILISERS AND FEED) ACT

AGRICULTURE (FERTILISERS) REGULATIONS

[Sections 21 and 47 and Regulation 15]

CERTIFICATE OF ANALYSIS

I certify that I received on ..................................., 20............... a sample of ............................................................. from ..................................................... and the analysis of this sample is as declared below.

Laboratory number ...............................................................................................................

Sample number ...................................................................................................................

Constituent

Declared Analysis

Actual Analysis

     
     
     
     
     

Date ....................................................

.................................................

 

Analyst

NOTE.- To be completed in triplicate and copies dispatched as follows:

Original - Owner or Seller.

Duplicate - Inspector.

Triplicate - To be retained by Analyst.

 

FORM FERT. 11

REPUBLIC OF ZAMBIA

THE AGRICULTURE (FERTILISERS AND FEED) ACT

THE AGRICULTURE (FERTILISERS) REGULATIONS

[Sections 24(2) and 25(2) and Regulation 10]

CERTIFICATE OF AUTHORITY FOR INSPECTOR

This is to certify that .................................................................................................. has been duly authorised as an Inspector of farming requisites for the purposes of the Act and is empowered to exercise all the powers therein described anywhere in Zambia.

 

Certificate number ......................................

 
 

..................................................
Inspector

Date ................................................................

.................................................
Registering Officer

 

 


{mprestriction ids="2,3,5"}

FORM FERT. 12

REPUBLIC OF ZAMBIA

AGRICULTURE (FERTILISERS AND FEED) ACT

AGRICULTURE (FERTILISERS) REGULATIONS

[Section 24 and Regulation 10]

CERTIFICATE OF LIMITED AUTHORITY FOR INSPECTOR

This is to certify that ............................................................................................................. has been granted limited authorisation to act as an Inspector of farming requisites for the purposes of the Act and is empowered to exercise all the powers therein described except as stated below.

...............................................................................................................................................

...............................................................................................................................................

...............................................................................................................................................

...............................................................................................................................................

...............................................................................................................................................

Signature of Inspector ...............................................................

Certificate number .....................................................................

Date ...........................................................................................

 

..................................................................

 

Registering Officer

 

 

FORM FERT. 13

REPUBLIC OF ZAMBIA

AGRICULTURE (FERTILISERS AND FEED) ACT

AGRICULTURE (FERTILISERS) REGULATIONS

[Section 52(h) and Regulation 16]

CERTIFICATE OF SAMPLING

I certify that the accompanying is/are sample(s) of ............................................ taken by me on ..................................., 20.........., at .................................. from stock in charge of .......................................................................................................... in the presence of ..................................................................................................................

....................................................

(name and address of witness)

The following particulars are given in connection with this/these sample(s).

Sample No.

Description of goods represented by this sample

Quantity of goods represented by this sample

     

Other particulars ..................................................................................................................

..............................................................................................................................................

Declared analysis as set out in the Fifth Schedule and trade name, trade brand or trade mark, etc., under which sold

..............................................................................................................................................

Signature of witness ......................................

Signature of Inspector ...................................

Date ...............................................................

NOTE.- This form is to be completed in triplicate and should be despatched as follows:

Original - Analyst.

Duplicate - Owner or Seller.

Triplicate - To be retained by Inspector.

 

SECOND SCHEDULE

[Section 25(1)(a), (1)(b) and Regulation 16]

METHOD OF TAKING SAMPLES

NOTE.- In this regulation "metric ton" is defined as 1,000 kg.

1. Where the fertiliser is contained in packages the samples shall be taken from different parts of the whole quantity as follows:

   (a)   if the quantity does not exceed two and a half metric tons, from not less than two unopened packages per ton or part thereof;

   (b)   if the quantity exceeds two and a half metric tons, from one additional unopened package for every additional ton or part thereof:

Provided that in no case need samples be taken from more than 20 packages.

2. Where the fertiliser is not contained in packages, not less than two samples per ton or part thereof shall be taken from different parts of the whole quantity:

Provided that not less than six shall be taken and not more than 50 need be taken.

3. The samples shall be taken by means of a suitable sampling probe or by such other means as will ensure, as far as is practicable, the taking of a representative sample.

4. The samples thus taken shall be thoroughly mixed and reduced in size to give a final sample not exceeding six pounds in weight. This final sample shall be mixed and divided into three parts and each of these parts shall be transferred to a clean, dry, non-corrodible container capable of being closed in such a manner as to preserve the contents of the container in their original condition. These three containers shall be so sealed so that they cannot be opened without breaking the seal. Each of these three parts shall be marked with the name of the fertiliser, date and place of sampling and the sample number together with the name of the inspector taking the sample.

5. The first part shall be given to the owner or seller of the fertiliser or his agent, the second part shall be delivered to an approved analyst for analysis, and the third part shall be retained by the inspector for a period of not less than six months after the date on which the Report or Certificate of Analysis is issued.

6. A Certificate of Sampling (Form FERT. 13 in the First Schedule) shall be made out in triplicate at the time of sampling and the relevant copies as detailed in Form FERT. 13 in the First Schedule should accompany each part of the sample.

[Am by SI 117 of 1970.]

 

THIRD SCHEDULE

[Section 52(i) and Regulation 17]

METHODS OF ANALYSIS OF FERTILISERS

1. PREPARATION OF SAMPLE:

   (a)   Remove any extraneous matter which cannot be conveniently ground and allow for this when calculating results.

   (b)   Grind the sample as rapidly as possible to pass through a sieve having apertures about 1 mm. square. In the case of granular fertilisers and dry powdered fertilisers grind a representative portion of about 250 g. to pass through a sieve having apertures about 0.25 mm. square.

   (c)   Store the prepared sample in a non-corrodible air-tight container.

   (d)   Where a sample is too moist to be ground in its original condition, mix the sample thoroughly and remove a portion for moisture determination. Dry the remaining portion at 100 degrees C except where the sample may lose ammonia or where the sample contains soluble phosphorus compounds. In these instances dry the sample in a desiccator over calcium chloride or silica gel, or alternatively by passing dry air at room temperature over the sample until it is in a suitable condition for grinding. The results of the analysis of the dried sample should be adjusted to the "as received" condition.

2. DETERMINATION OF MOISTURE:

Weigh to the nearest mg. about 5 g. of the sample and heat to 100ºC for three hours, cool in a desiccator and weigh. Calculate the loss in weight as a percentage of the original weight.

3. DETERMINATION OF NITROGEN:

   (a)   REAGENTS

Ammonia alum.

Standard indigo solution.

Cautiously add 40 ml. of concentrated sulphuric acid to 1 g. of indigo carmine and stir until dissolved. Pour the solution into 800 ml. of water, cool and dilute to 1 litre. Adjust the strength of the solution to comply with the following test:

Add 20 ml. to a solution of 4 mg. of potassium nitrate in 20 ml. of water. Add rapidly 40 ml. of concentrated sulphuric acid and heat to boiling; the blue colour is just discharged in one minute.

Concentrated sulphuric acid.

1 : 9 Sulphuric acid-Cautiously add 100 ml. of concentrated sulphuric acid to 900 ml. of water. Cool and dilute to 1 litre.

1 : 1 Sulphuric acid-Cautiously add 500 ml. of concentrated sulphuric acid to 500 ml. of water. Cool and dilute to 1 litre.

Anhydrous sodium sulphate.

Cupric sulphate.

Paraffin wax.

Granulated zinc.

Light magnesium oxide.

50% sodium hydroxide solution-Dissolve 500 g. of sodium hydroxide in water and dilute to 1 litre.

0.1 N Hydrochloric acid.

Mixed indicator solution-Grind together in an agate mortar 0.6 g. of methyl red

and 0.6 g. of methylene blue. Dissolve the mixture in 500 ml. of 95% ethanol. Shake, filter and store in a dark glass bottle.

2% Boric acid solution-Dissolve 20 g. of boric acid in water, dilute to 1 litre and add 5 ml. of the mixed indicator solution.

Devarda's alloy: Finely powdered-not less than 80% to pass through a sieve having apertures of about 0.25 mm. square.

   (b)   TEST FOR ABSENCE OF NITRATES

Shake 5 g. of the sample with 80 ml. of water in a 100 ml. volumetric flask. Add 1 g. of ammonia alum, dilute to 100 ml., shake well and filter into a dry beaker. Dilute 1 ml. of the filtrate with 8 ml. of water. Add 1 ml. of standard indigo solution and 10 ml. of concentrated sulphuric acid. Heat to boiling point. If the colour is not discharged regard the sample as free from nitrates.

   (c)    TOTAL NITROGEN (ORGANIC AND AMMONIACAL) IN THE ABSENCE OF NITRATES

      (i)   Weigh to the nearest mg. about 2 g. of the sample (or an amount containing not more than 250 mg. of nitrogen) and transfer to a Kjeldahl flask. Add 25 ml. of concentrated sulphuric acid and approximately 10 g. of anhydrous sodium sulphate containing 0.4 g. of cupric sulphate. Heat gently until frothing ceases, increase the heat and continue the digestion until the liquid is practically colourless. Continue to heat for a further hour. If frothing is excessive add about 0.5 g. of paraffin wax. Avoid local overheating.

      (ii)   Transfer the cooled digest to 250 ml. volumetric flask. Thoroughly wash the Kjeldahl flask with successive portions of water carefully adding the washings to the digest in the volumetric flask. When cool adjust the contents of the volumetric flask to a volume of 250 ml. with water. Thoroughly mix the contents of the flask and pipette an aliquot such as to give a final titration of at least 4 ml. into a Kjeldahl flask. Add 250 ml. of water, a small zinc granule and sufficient 50% sodium hydroxide solution to neutralise the acid and give about 10 ml. in excess. Mix well and connect immediately to a distillation apparatus. Distil into an appropriate volume (usually 30 ml.) of 2% boric acid solution. Titrate the contents of the receiving flask with 0.1 N hydrochloric acid. The colour change is from green to purple. Carry out a blank test using 2 g. of sucrose in place of the sample and substract the titration value of the blank from that of the sample. Express the result in terms of nitrogen (N). 1 ml. of 0.1 N hydrochloric acid = 0.0014 g. nitrogen.

   (d)   TOTAL NITROGEN (ORGANIC, AMMONIACAL AND NITRIC) IN THE PRESENCE OF NITRATES

Weigh to the nearest mg. about 1 g. of the sample (or an amount containing not more than 250 mg. of nitrogen) and transfer to a Kjeldahl flask. Add 3 g. of Devarda's alloy and wash down the neck of the flask with 50 ml. of water. Close the flask with a rubber stopper fitted with (a) a tap funnel and (b) a delivery tube connected to a U-tube (with bulbs) containing 20 ml. of 1 : 9 sulphuric acid. Add 5 ml. of 50% sodium hydroxide solution through the tap funnel, allow to stand for 30 minutes and then heat at just below boiling point for 60 minutes. Cool, add 20 ml. of 1 : 1 sulphuric acid through the tap funnel, washing the neck of the flask. Remove the rubber stopper, wash the contents of the U-tube into the Kjeldahl flask, add 25 ml. of concentrated sulphuric acid and heat until all the water has boiled off. Add approximately 10 g. of anhydrous sodium sulphate containing 0.4 g. of cupric sulphate and heat gently until frothing ceases. Increase the heat and continue the digestion for a further hour. Avoid local overheating. Cool, and complete the determination by the method described under (c) (ii).

   (e)   AMMONICAL NITROGEN

Weigh to the nearest mg. about 5 g. of the sample, transfer to a 250 ml. volumetric flask, dissolve in about 200 ml. of water, dilute to the mark and filter if necessary. Transfer 50 ml. of the solution (or an aliquot such as to give a final titration of at least 4 ml.) to a distillation flask, add approximately 300 ml. of water and 20 ml. of 50% sodium hydroxide solution. (If urea is known to be present 10 g. of light magnesium oxide should be used instead of 50% sodium hydroxide solution.) Connect immediately to a distillation apparatus. Distil into 30 ml. of 2% boric acid solution. Titrate the contents of the receiving flask with 0.1 N hydrochloric acid. The colour change is from green to purple. Carry out a blank determination using sucrose in place of the sample and subtract the titration value of the blank from that of the sample. Express the result in terms of nitrogen (N). 1 ml. of 0.1 N hydrochloric acid = 0.0014 g. nitrogen.

   (f)   AMMONICAL AND NITRATE NITROGEN (IN INORGANIC FERTILISERS)

Weigh to the nearest mg. about 2 g. of the sample, transfer to a 250 ml. volumetric flask, dissolve in 200 ml. of water, dilute to volume and filter if necessary. Transfer 10 ml. of the solution (or an aliquot such as to give a final titration of at least 4 ml.) to a distillation flask. Add 10 g. of Devarda's alloy, 250 ml. of water and 15 ml. of 50% sodium hydroxide solution. Connect the flask immediately to the distillation apparatus and allow to stand in the cold for 15 minutes. Warm gently for 30 minutes, slowly increasing the temperature. Distil into 30 ml. of 2% boric acid solution. Titrate the contents of the receiving flask with 0.1 N hydrochloric acid. The colour change is from green to purple. Carry out a blank determination using sucrose in the place of the sample and substract the titration value of the blank from that of the sample. Express the result in terms of nitrogen (N). 1 ml. of 0.1 N hydrochloric acid = 0.0014 g. nitrogen.

4. DETERMINATION OF PHOSPHORUS:

   (a)   EXTRACTION OF SAMPLE

Weigh to the nearest centigram about 10 g. of the sample and transfer to a 500 ml. volumetric flask; add 400 ml. of water and shake the flask continuously for 30 minutes. Dilute the contents to the mark, mix well and filter.

   (b)   QUINOLINIUM PHOSPHOMOLYBDATE METHOD

      (i)   REAGENTS

Concentrated hydrochloric acid.

Concentrated nitric acid.

Calcium oxide-finely ground.

Calcium carbonate.

5 N sodium hydroxide solution.

Dilute hydrochloric acid - Dilute 240 ml. of concentrated hydrochloric acid with water to 1 litre.

Citric - molybdic acid solution-Stir 54 g. of molybdic anhydride (MoO3) with 200 ml. of water, add 11 g. of sodium hydroxide and stir the mixture whilst heating to boiling point until the molybic anhydride dissolves. Dissolve 60 g. of citric acid in about 250 ml. to 300 ml. of water and add 140 ml. of concentrated hydrochloric acid. Pour the molybdate solution into the acid solution, which is stirred throughout the addition. Then cool and, if necessary, filter the solution through a 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 or 1.0%) solution of potassium bromate until the colour is discharged. This reagent should be kept in the dark.

Quinoline solution - Measure 60 ml. of concentrated hydrochloric acid and 300 to 400 ml. of water into a 1 litre beaker and warm to 70-80ºC. Pour 50 ml. of quinoline in a thin stream into the diluted acid while stirring. When the quinoline has dissolved cool the solution, dilute to 1 litre, and, if necessary, filter through a paper pulp filter.

0.5 N sodium hydroxide - carbonate free.

Indicator solution - Mix 3 volumes of thymol blue solution and 2 volumes of phenolphthalein solution prepared as follows:

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

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

0.5 N hydrochloric acid.

0.1 N sodium hydroxide solution - carbonate free.

0.1 N hydrochloric acid.

Surface active agent - 0.5% solution of sodium dodecyl benzene sulphonate is suitable.

Crystallised citric acid - monohydrate

      (ii)   PROCEDURE

Transfer a volume of the aqueous extract containing not less than 30 mg. of phosphorus and preferably about 20 mg. to a 500 ml. stoppered conical flask marked at 150 ml. Dilute with water to 150 ml., add 50 ml. of the citric-molybdic acid reagent, heat the solution to incipient ebullition, maintain it at this temperature for 3 minutes, and then bring it to boiling point. From a burette slowly add 25 ml. of the quinoline solution with constant swirling throughout, the first few ml. being added dropwise, the rest in a slow stream. Keep the solution gently boiling during the addition. Immerse the flask in boiling water for 5 minutes, then cool it to 150ºC in running water.

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. Transfer the filter pad and precipitate to the original flask, rinse the funnel with water and collect the rinsings in the flask. If necessary, wipe the funnel with a small piece of damp filter paper to ensure complete removal of the precipitate and place the paper in the flask. Add water to a total of about but not exceeding 100 ml. Stopper the flask and shake it vigorously until the pulp and the precipitate are completely dispersed.

Remove the stopper and wash it with water, returning the washings to the flask. Add a measured volume of 0.5 N sodium hydroxide solution sufficient to dissolve the precipitate and leave a few ml. in excess. Shake the flask vigorously until all the precipitate dissolves. (To facilitate the dispersal of the precipitate, after addition of 0.5 N sodium hydroxide solution, a few drops of surface active agent may be added.) Add 0.5-1.0 ml. of the indicator solution and titrate the excess of sodium hydroxide with the 0.5 N hydrochloric acid until the indicator changes from violet to green-blue and then very sharply to yellow at the end point. Deduct the number of ml. of 0.5 N hydrochloric acid used from the number of ml. of 0.5 N sodium hydroxide, to ascertain the volume of 0.5 N sodium hydroxide equivalent to phosphorus.

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.

Calculate the amount of phosphorus in the portion taken for analysis from the factor 1.0 ml. 0.5 N sodium hydroxide = 0.597 mg. phosphorus (P).

   (c)   SPECTROPHOTOMETRIC (VANADIUM PHOSPHOMOLYBDATE) METHOD

      (i)   REAGENTS

Potassium dihydrogen phosphate - containing at least 99.8% monopotassium dihydrogen phosphate.

Ammonium molybdate. Ammonium vanadate

Concentrated hydrochloric acid.

Concentrated nitric acid.

Calcium oxide-finely ground.

Standard phosphorus solution - Dissolve in water 2.1953 g. of potassium dihydrogen phosphate previously dried at 105ºC for 1 hour and dilute to 1 litre. Make a 5 fold dilution (1 ml. = 0.1 mg. phosphorus (P)).

Vanadium molybdate reagent - Dissolve separately 20 g. of ammonium molybdate and 1 g. of ammonium vanadate in water, mix, acidify with 140 ml. of concentrated nitric acid and dilute to 1 litre.

Normal sodium hydroxide solution. Crystallised citric acid.

      (ii)   STANDARDISATION OF INSTRUMENT

From a burette measure into a series of 100 ml. volumetric flasks 22.0, 23.0, 24.0, 25.0, 26.0 and 27.0 ml. of the standard phosphorus solution (i.e. 2.2, 2.3, 2.4, 2.5, 2.6 and 2.7 mg of P). Add 25 ml. of the vanadium molybdate reagent to each flask and dilute to 100 ml. with water. Shake and allow to stand for 10 minutes.

Set the spectrophotometer to the correct wavelength, say 4200, fill two 1 cm. cells with the 2.2 mg. solution and check the optical density of the cells. If there is a small difference select the cell with the smaller reading as the standard reference cell.

Determine the apparent optical density (corrected for cell differences) of the 2.3, 2.4, 2.5, 2.6 and 2.7 mg. phosphorus solutions referred to the 2.2 mg. phosphorus solution as standard.

Plot a calibration graph of scale readings against known phosphorus content.

      (iii)   ANALYSIS OF SAMPLE

To 25 ml. of the solution prepared according to paragraph 4 (a) add 1 ml. of concentrated nitric acid; heat to incipient ebullition on a hotplate and maintain it at this temperature for 10 minutes. Cool, neutralise with normal sodium hydroxide solution and then successively dilute until a final volume of about 25 ml. contains between 2.4 and 2.7 mg. of phosphorus.

Transfer this volume to a 100 ml. volumetric flask, add 25 ml. of the vanadium molybdate reagent, dilute to the mark, mix and allow to stand for 10 minutes. At the same time transfer 25 ml. of the standard phosphorus solution into a second 100 ml. volumetric flask. Add 25 ml. of the vanadium molybdate reagent, dilute to the mark, mix and allow to stand for 10 minutes.

Measure the difference in optical density between the two solutions and estimate the phosphorus content of the volume of the unknown solution from the calibration graph. Calculate the phosphorus content of the sample from known dilution factors and the weight of the sample.

NOTE.-Prepare a fresh reference standard for each series of readings on the instrument.

5. DETERMINATION OF POTASSIUM

   (a)   PERCHLORIC ACID METHOD

      (i)   REAGENTS

Concentrated hydrochloric acid.

Barium chloride solution - Dissolve 100 g. of barium chloride in water, filter the solution and dilute to 1 litre.

Dilute hydrochloric acid - Dilute 240 ml. of concentrated hydrochloric acid with water to 1 litre.

Calcium oxide - finely ground.

Ammonium hydroxide solution - sp. gr. 0.912.

Ammonium carbonate solution - saturated aqueous solution.

Ammonium oxalate solution - saturated aqueous solution.

20% perchloric acid solution.

Alcohol - industrial methylated spirit 95-96% v/v.

Wash solution - Add potassium perchlorate to alcohol and shake until a saturated solution is obtained.

Keep the solution over solid potassium perchlorate and filter immediately before use.

      (ii)   PREPARATION OF SAMPLE SOLUTION

      (I)   POTASSIUM SALTS FREE FROM SULPHATES AND OTHER INTERFERING SUBSTANCES

Dissolve in water a portion of the sample weighed to the nearest mg. equivalent in potassium content to 1.2 to 1.7 g. of potassium. Cool the solution, dilute to 500 ml. in volumetric flask, mix well and filter. Determine the potassium in 50 ml. of this solution by the method described in paragraph 5 (a) (iii).

      (II)   POTASSIUM SALTS CONTAINING SULPHATES

NOTE.-If sample contains phosphates, iron, manganese or substances other than sulphate that interfere with the determination of potassium the method described in paragraph 5 (a) (ii) (III) should be used.

Weigh to the nearest mg. a portion of the sample equivalent in potassium content to 1.2 to 1.7 g. of potassium into a 500 ml. beaker, add about 300 ml. of water and 20 ml. of concentrated hydrochloric acid and heat the solution to boiling. 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. Cool the liquid to 20 degrees C, transfer to a 500 ml. volumetric flask, dilute to 500 ml., mix, and filter through a dry filter. Take 50 ml. of the filtrate and evaporate to dryness in a basin; moisten the residue with concentrated hydrochloric acid, again evaporate to dryness, dissolve the residue with 5-10 ml. of dilute hydrochloric acid and filter if necessary. Determine the potassium in the solution by the method described in paragraph 5(a)(iii).

      (III)   POTASSIUM IN MIXED FERTILISERS

Weigh to the nearest centigram about 10 g. of the sample and, if organic matter is present, gently incinerate at a temperature not exceeding 500ºC. Transfer the weighted portion of the sample or the incinerated residue to a 500 ml. beaker with a little water and 10 ml. of concentrated hydrochloric acid and then warm for 10 minutes. Dilute with water to about 300 ml. and bring gradually to boiling point. Add 10 g. of calcium oxide made into a paste with water, bring the contents again gently to boiling point, and keep so heated for about half an hour with frequent stirring. Cool to 20ºC, transfer to a 500 ml. volumetric flask, dilute to 500 ml. and, after thoroughly shaking, filter through a dry filter paper. Transfer 250 ml. of the filtrate to another 500 ml. volumetric flask, make just acid with hydrochloric acid and heat to boiling point. To the boiling solution cautiously add, drop by drop, barium chloride solution until there is no further precipitation of barium sulphate. 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 1 ml. of ammonium oxalate solution. Cool to 20ºC, dilute with water to 500 ml. and after thoroughly shaking, filter through a dry filter paper. Measure 100 ml. 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. Cool the residue, moisten with concentrated hydrochloric acid and again evaporate to dryness. Take up the residue with water and filter if necessary. Determine the potassium in the solution by the method described in paragraph 5(a)(iii).

      (iii)   PROCEDURE

Transfer the solution obtained as described in paragraph 5(a)(iii)(I), 5(a)(ii)(II) or 5(a)(ii)(III) into a basin and add about 7 ml. of perchloric acid solution. Place the basin on a hotplate or sand bath and evaporate the contents until white fumes are copiously evolved. Cool, and dissolve the precipitate in a little hot water. Add about 1 ml. of perchloric acid solution and again concentrate to the fuming stage. Thoroughly cool the residue in the basin and stir in 20 ml. of alcohol. Allow the precipitate to cool and settle; then pour the clear liquid through a dry filter paper, draining the precipitate in the basin as completely as possible. Redissolve the precipitate on the paper and that remaining in the basin with hot water, add 2 ml. of perchloric acid solution to the combined residue in the basin and thoroughly stir the contents with 20 ml. of alcohol. Allow the precipitate to cool and settle and pour clear liquid through a weighed Gooch or sintered glass crucible, draining the precipitate as completely as possible from the liquid before adding 5 ml. of the wash solution. Wash the precipitate by decantation with several similar small portions of the wash solution, pouring the washings through the crucible. Transfer the precipitate to the crucible and wash it well with the wash solution until free from acid. Dry the precipitate at 100ºC and weigh. Regard the precipitate as potassium perchlorate (KClO4) and calculate its equivalent as potassium (K) by multiplying its weight by 0.282. Calculate the potassium content of the sample.

5. (b)   FLAME PHOTOMETRIC PROCEDURE

The determination of potassium by this method depends on the measurement of the characteristic radiation due to potassium emitted by a flame into which a solution of the sample is sprayed. The chosen radiations lie in the spectral range 7660-7700 nm . These radiations may be isolated by either a monochromator or the use of a suitable filter. This method must not be used where the potassium content of the material being analysed exceeds 17% by weight.

      (i)   REAGENTS.

Potassium dihydrogen phosphate - containing at least 99.8% mono-potassium dihydrogen phosphate.

Concentrated hydrochloric acid.

Ammonium oxalate solution - saturated aqueous solution.

Ammonium hydroxide solution - sp. gr. 0.96.

Standard potassium solution - Dissolve in water 6.9608 g. of potassium dihydrogen phosphate previously dried for 1 hour at 105ºC, and dilute to 1 litre in a volumetric flask. Shake well. Transfer 50 ml. to a 1 litre volumetric flask and dilute to the mark. Shake well. This solution contains 100 p.p.m. potassium (K).

      (ii)   PREPARATION OF SAMPLE SOLUTION (I) POTASSIUM SALTS

If the sample contains ammonium, calcium, iron, aluminium or other interfering substances the procedure described under paragraph 5 (b) (ii) (II) should be used.

Weigh to the nearest mg. about 2.5 g. of the sample and transfer to a 400 ml. beaker. Add about 10 ml. of concentrated hydrochloric acid and 50 ml. of water and bring the contents to boiling point, breaking down with a stirring rod any lumps or crystals. Dilute the solution with water to about 100 ml. and boil gently for a few minutes. Cool the solution to 20ºC, transfer to a 250 ml. volumetric flask, and dilute to the mark. Mix and filter through a dry filter. Successively dilute so that the final solution contains approximately 14 p.p.m. potassium (K) and determine potassium in the filtrate by the method described in paragraph 5 (b) (iii).

      (II)   POTASSIUM IN MIXED FERTILISERS

Weigh to the nearest mg. about 2.5 g. of the sample and transfer to a 400 ml. beaker. Add 125 ml. of water and 50 ml. of ammonium oxalate solution. Boil the contents for 30 minutes. If necessary a small quantity of potassium-free anti-foaming agent may be added. Cool the liquid, add a slight excess of ammonium hydroxide solution and cool to 20ºC. Transfer to a 250 ml. volumetric flask and dilute to the mark. Mix the solution and filter through a dry filter. Successively dilute so that the final solution contains approximately 14 p.p.m. potassium (K) and determine the potassium by the method described in paragraph 5 (b) (iii).

      (iii)   METHOD OF ANALYSIS

      (I)   CALIBRATION OF INSTRUMENT

From the standard potassium solution prepare a set of accurate dilutions containing 8, 10, 12, 14, 16 and 18 p.p.m. potassium. Set the sensitivity of the flame photometer so that 100 scale divisions (full scale deflection) is equivalent to 18 p.p.m. potassium solution. Spray the 8, 10, 12, 14 and 16 p.p.m. potassium solutions three times. Take the median reading (not the mean) and construct a calibration graph. After spraying each different strength solution, again spray the 18 p.p.m. solution to ensure that the sensitivity of the flame photometer has not changed.

      (II)   ANALYSIS OF THE SAMPLE SOLUTION

Reset the instrument at 100 scale divisions (full scale deflection) with 18 p.p.m. potassium solution. Spray the diluted fertiliser solution prepared in accordance with paragraph 5 (b) (ii) (I) or 5 (b) (ii) (II) and read from the graph the approximate potassium content of the solution.

Prepare two further dilutions of the standard potassium solution to contain respectively 1 p.p.m. more and 1 p.p.m. less potassium than the estimated potassium content of the diluted solution of the sample. Successively spray the low standard solution, the diluted solution of the sample, and the high standard solution. Repeat this operation twice more. Take the median result of each set of three readings and calculate the potassium content of the sample solution and hence the fertiliser from the proportionality of the radiation given by the sample solution and that given by the two standard solutions containing respectively 1 p.p.m. more and 1 p.p.m. less potassium than the predicted potassium content. Dilute standard solutions should be freshly prepared.

6. FREE ACID IN SULPHATE OF AMMONIA

   (a)   REAGENTS

Methyl red indicator solution - Dissolve 25 mg. of methyl red in 5 ml. of 90% industrial methylated spirit with the aid of 0.5 ml. of 0.1 N sodium hydroxide solution. Dilute to 250 ml. with 50% industrial methylated spirit. If desired screened methyl red indicator may be used. 0.1 N sodium hydroxide solution-carbonate free.

   (b)   PROCEDURE.

Weigh to the nearest centigram about 20 g. of the sample and dissolve in about 50 ml. of water. Filter, wash any insoluble matter and the filter paper free from sulphate and dilute the combined filtrate and washings to about 250 ml. Add 2 or 3 drops of the indicator solution and titrate with 0.1 N sodium hydroxide solution. Express the result as percentage by weight of sulphuric acid (H2SO4). 1ml. O. 1 N sodium hydoxide solution = 0.0049 g. sulphuric acid (H2SO4).

 

FOURTH SCHEDULE

[Section 52(g) and Regulation 18]

LIMITS OF VARIATION

The limits shown shall be the maximum variation allowed above and below the amount stated except in the case of sulphur.

1. Limits Applicable to all Fertilisers Except in 2 below:

Nitrogen

 

All forms of nitrogen expressed as % N:1/10th of amount stated with a minimum of 0.3% N and a maximum of 1.0% N.

Phosphorus

 

Water-soluble phosphorus expressed as % P: 1/20th of amount stated with a minimum of 0.2% P and a maximum of 0.9% P.

Potassium

 

Total potassium expressed as % K: 1/20th of amount stated with a minimum of 0.6% K and a maximum of 1.7% K.

Chloride

 

Percentage chloride expressed as % Cl: 1/20th of amount stated.

Boron

 

Percentage boron expressed as % B: 1/5th of amount stated.

Sulphur

 

No variation allowed below minimum amount stated.

2. Limits Applicable to Borax and Other Borates for Use as Fertilisers:

Percentage boron expressed as % B: 1/10th of amount stated with a maximum of 1.0% B.

3. Sulphate of Ammonia:

In addition to the other limits applicable in 1 above, percentage of free acid content:

1/5th of amount stated or 0.025% whichever is the greater, expressed as percentage by weight of sulphuric acid (H2SO4).

 

FIFTH SCHEDULE

[Sections 28, 29 and 52(k) and Regulations 11 and 12]

STATEMENTS OF ANALYSIS REQUIRED FOR DIFFERENT CLASSES OF FERTILISERS

 

Statement of Analysis to be Shown on Bags, Containers or Labels, and Notes to Accompany

Class of Fertiliser

Sales in Bulk

Nitrogenous fertilisers

Percentage of total nitrogen.

Ammoniated phosphates and ammoniated super-phosphates.

Percentage of total nitrogen.

 

Percentage of water-soluble phosphorus expressed in the elemental form (P).

elemental form (P).

Minimum percentage of sulphur expressed in the elemental form (S).

Single, double or triple super-phosphates.

Percentage of water-soluble phosphorus expressed in the elemental form as (P).

Potassic fertilisers.

Percentage of potassium expressed in the elemental form (K).

Any other inorganic fertiliser or compound, complex, blend or mixture of fertilisers.

Percentage of total nitrogen (N).

 

Percentage of water-soluble phosphorus expressed in the elemental form (P).

 

Percentage of potassium expressed in the elemental form (K).

 

Percentage of boron expressed in the elemental form (B).

 

Minimum percentage of sulphur expressed in the elemental form (S).

Borax and other borates for use as fertilisers.

Percentage of boron expressed in the elemental form.

 

SIXTH SCHEDULE

[Section 30 and Regulation 13]

STATEMENT OF PARTICULARS TO BE LODGED WITH THE REGISTERING OFFICER IN RESPECT OF FERTILISERS SOLD IN BAGS, CONTAINERS, ETC., UNDER ANY TRADE NAME, TRADE MARK, ETC., AS DESCRIBED IN SECTION 30 OF THE ACT

1. Percentage by weight of nitrogen:

   (a)   in the ammonium form;

   (b)   in the nitrate form;

   (c)   in the urea form;

   (d)   in any other form.

2. Percentage by weight of water-soluble phosphorus expressed as (P).

3. Percentage by weight of potassium expressed as (K):

   (a)   in the chloride form;

   (b)   in the sulphate form;

   (c)   in any other form.

4. The minimum percentage by weight of sulphur expressed as (S).

5. The percentage by weight of boron expressed as (B).

6. In the case of sulphate of ammonia only the percentage of free acid.

7. The trade name, brand name, etc., under which the product is to be sold.

8. By whom sold ....................................................................................................................

................................................................................................................................................

Address...................................................................................................................................

................................................................................................................................................

................................................................................................................................................

 

 

AGRICULTURE (FARM FEED) REGULATIONS

[Section 52]

Arrangement of Regulations

   Regulation

PART I
PRELIMINARY

   1.   Title

   2.   Interpretation

   3.   Application

PART II
REGISTRATION

   4.   Registration of plant and fees

   5.   Register of plant

   6.   Requirements of plant

PART III
ANALYSIS AND LABORATORIES

   7.   Approval of analysts

   8.   Approval of laboratories

   9.   Roll of analysts

   10.   Roll of laboratories

PART IV
SEARCHES AND SEIZURES

   11.   Certificate of authority for inspectors

PART V
SALE OF FARM FEED

   12.   Statements of analysis for sales in bags, containers, etc.

   13.   Statements of analysis for sales in bulk

   14.   Statements of analysis and records to be kept for sales under trade names, etc.

   15.   Exemption of farm feed made to specification

   16.   Deleterious ingredients

   17.   Declaration of presence of certain ingredients upon sale

PART VI
SAMPLING, ANALYSIS AND LIMITS OF VARIATION

   18.   Form of report to be used

   19.   Form of certificate to be used

   20.   Method of taking samples

   21.   Methods of analysis

   22.   Limits of variation

      FIRST SCHEDULE

      SECOND SCHEDULE

      THIRD SCHEDULE

      FOURTH SCHEDULE

      FIFTH SCHEDULE

      SIXTH SCHEDULE

      SEVENTH SCHEDULE

      EIGHTH SCHEDULE

[Regulations by the Minister]

SI 197 of 1970.

 

PART I
PRELIMINARY

 

1.   Title

These Regulations may be cited as the Agriculture (Farm Feed) Regulations.

 

2.   Interpretation

In these Regulations, unless the context otherwise requires"”

"the Act" means the Agriculture (Fertilisers and Feed) Act.

"Minister" means the Minister responsible for Agriculture.

 

3.   Application

These Regulations shall apply in relation to any farm feed as defined in section 2 of the Act.

 

PART II
REGISTRATION

 

4.   Registration of plant and fees

   (1) Applications under Part II of the Act for registration, transfer of registration or renewal of registration of plant shall be made in Form FERT 4 in the First Schedule to the Agriculture (Fertilisers) Regulations, 1969 (hereinafter in these Regulations referred to as "the Fertilisers Regulations") and such application shall be accompanied by the appropriate fees shown in the First and Second Schedules to the Act, and be given to the Registering Officer.

   (2) The Registering Officer shall issue a certificate of registration in Form FERT 5 in the First Schedule to the Fertilisers Regulations.

   (3) The Registering Officer shall issue a certificate of provisional registration in Form FERT 6 in the First Schedule to the Fertilisers Regulations.

 

5.   Register of plant

The Registering Officer shall keep a register of plant as prescribed in Form FERT 1 in the First Schedule to the Fertilisers Regulations.

 

6.   Requirement of plant

Any plant within the definition of section 2 of the Act shall be so equipped as to permit the adequate performance therein of the activities described in the application for registration of such plant, to the satisfaction of the Registering Officer.

 

PART III
ANALYSTS AND LABORATORIES

 

7.   Approval of analysts

   (1) For the purposes of the Act an analyst shall furnish proof to the satisfaction of the Minister that he has competent knowledge of chemistry and of chemical analyses, as applied to farm feed, and such proof shall in every case comprise documentary evidence that the analyst holds a certificate or diploma attesting his possession of the requisite knowledge and given by a recognised competent body, and shall be submitted to the Minister when applying for approval, so, however, that the Minister may call for further evidence if required in any particular case.

   (2) Where the requirements referred to in sub-regulation (1) are satisfied, the Registering Officer shall issue a certificate of approval on Form FERT 7 in the First Schedule to the Fertilisers Regulations.

 

8.   Approval of laboratories

   (1) An approved laboratory shall be so equipped as to enable approved analysts to perform accurately for the purposes of the Act all the analyses specified under the Seventh Schedule to these Regulations and such laboratories shall have been inspected by a duly authorised officer of the Ministry of Agriculture, Food and Fisheries before approval by the Minister and may be inspected from time to time as the Registering Officer may deem necessary:

Provided that, in addition, other laboratories may be approved for certain analyses only, such analyses to be specified by the Registering Officer after inspection by a duly authorised officer of the Ministry of Agriculture, Food and Fisheries.

   (2) Where the Minister approves a laboratory, the Registering Officer shall issue a certificate of approval on Form FERT 8 in the First Schedule to the Fertilisers Regulations.

 

9.   Roll of analysts

The Registering Officer shall keep a roll of approved analysts in Form FERT 2 in the First Schedule to the Fertilisers Regulations.

 

10.   Roll of laboratories

The Registering Officer shall keep a roll of approved laboratories in Form FERT 3 in the First Schedule to the Fertilisers Regulations.

 

PART IV
SEARCHES AND SEIZURES

 

11.   Certificate of authority for inspectors

The certificate of authority to be held by inspectors under section 25 of the Act shall be issued by the Registering Officer and shall be"”

   (a)   in the case of general authorisation, in Form FERT 11 in the First Schedule to the Fertilisers Regulations; and

   (b)   in the case of limited authorisation, in Form FERT 12 in the First Schedule to the Fertilisers Regulations.

PART V
SALE OF FARM FEED

 

12.   Statements of analysis for sales in bags, containers, etc.

The statement of analysis for each class of farm feed specified in the Second Schedule to these Regulations shall appear in English in lettering both durable and legible on the bag or container containing the same or on a label securely attached thereto.

 

13.   Statements of analysis for sales in bulk

Where any class of farm feed specified in the Second Schedule to these Regulations is sold in bulk, the statement of analysis for such class shall appear in English in lettering both durable and legible on a note which shall be given to the purchaser or his agent at the time of delivery of such farm feed.

 

14.   Statements of analysis and records to be kept for sales under trade names, etc.

Where any class of farm feed specified in the Second Schedule to these Regulations is sold in a container or a package under a trade name, trade mark, trade label or trade brand, as provided by section 30 of the Act, there shall appear in English in lettering both durable and legible on the container or package, or on a label securely attached thereto, a statement of analysis in respect thereof and, in addition, the Registering Officer shall have access to such records relating thereto as are specified in the Third Schedule to these Regulations.

 

15.   Exemption of farm feed made to specification

Where any farm feed is manufactured to a farmer's own specifications, such farm feed shall be exempted from these Regulations, but only if the farm feed is for the sole use of the farmer supplying the specifications and is not intended for re-sale.

 

16.   Deleterious ingredients

No class of farm feed shall contain any of the ingredients listed as deleterious in the Fourth Schedule to these Regulations.

 

17.   Declaration of presence of certain ingredients upon sale

The presence in any farm feed of any of the materials specified in the Fifth Schedule to these Regulations shall be declared in writing to the purchaser of any farm feed whether sold in containers, in bulk or under any trade name, trade mark, trade label or trade brand.

 

PART VI
SAMPLING, ANALYSIS AND LIMITS OF VARIATION

 

18.   Form of report to be used

A report of analysis shall be issued by the analyst performing the analysis in respect of every sample taken under the Act, and any such report shall be in Form FERT 9 in the First Schedule to the Fertilisers Regulations.

 

19.   Form of certificate to be used

A certificate of analysis shall not be issued unless the sample has been taken in accordance with the Sixth Schedule to these Regulations and such certificate shall be in the Form FERT 10 in the First Schedule to the Fertilisers Regulations.

 

20.   Method of taking samples

Samples for analysis for the purposes of the Act shall be taken in the manner prescribed in the Sixth Schedule to these Regulations and certificates of sampling issued in relation thereto shall be in Form FERT 13 in the First Schedule to the Fertilisers Regulations.

 

21.   Methods of analysis

Methods of analysis shall be as prescribed in the Seventh Schedule to these Regulations.

 

22.   Limits of variation

The limits of variation in respect of any prescribed analysis shall be as prescribed in the Eighth Schedule to these Regulations.

 

FIRST SCHEDULE

[Section 2]

DEFINITIONS IMPLIED ON THE SALE OF FARM FEED UNDER CERTAIN NAMES

Name of Farm Feed or Class of Feed

Implied Definition

Cereal brans

By-products produced in the milling of maize, wheat or other cereal kernels.

Oilseed cakes or meals (undecorticated)

Meals or cakes produced from the residues resulting from the removal of oil from undecorticated groundnuts, cottonseeds, sunflower seeds, soya beans or other oilseeds.

Oilseed cakes or meals (decorticated)

Meals or cakes produced from the residues resulting from the removal of oil from decorticated or partly decorticated groundnuts, cottonseeds, sunflower seeds, soya beans or other oilseeds.

Meat and bone meal

The product, containing not less than 40 per cent of protein (and not more than 4 per cent of salt) obtained by drying and grinding animal carcases or portions thereof (excluding hoof and horn) to which no other matter has been added, but which may have been treated previously for the removal of oil or fat.

Bone meal

Commercially pure bone, raw or degreased, which has been ground or crushed.

Meat meal

The product, containing not less than 55 per cent of protein (and not more than 4 per cent of salt) obtained by drying and grinding animal carcases or portions thereof (excluding hoof and horn) to which no other matter has been added but which may have been treated previously for the removal of oil or fat.

Fish meal

A product obtained by drying and grinding or otherwise treating fish or fish waste.

Molasses

A concentrated syrup product obtained in the manufacture of sugar from sugar cane, to which no other matter has been added.

Molasses feed

Any mixture (containing not less than 10 per cent of sugar) of an absorbent material and molasses.

Mixture of molasses

Any mixture of molasses and urea with or without any absorbent material.

Compound cakes and meals

A homogeneous mixture of two or more farm feeds. Concentrated or high A homogeneous mixture of two or more farm feeds or other substances energy farm feed intended to be mixed with some other farm feed before feeding to livestock.

NOTE:

"Commercially pure" means that no other matter has been added. In the case of every article mentioned in this Schedule the definition shall be deemed not to exclude the presence of a substance added to improve the keeping or handling properties of the farm feed or the presence of any coccidiostat, anti-blackhead remedy, natural or synthetic hormone.

"Synthetic hormone" means a synthetic compound which has similar properties to, or has the property of stimulating the production of, a natural hormone.

"Coccidiostat" means a substance used in the prevention or curative treatment of disease in poultry caused by protozoal organisms of the order coccidia.

"Anti-blackhead remedy" means a substance used in the prevention or curative treatment of infection in poultry due to Histomonas Meleagridis.

 

SECOND SCHEDULE

[Sections 28, 29 and 52K and regulations 12, 13 and 14]

STATEMENTS OF ANALYSIS REQUIRED FOR DIFFERENT CLASSES OF FARM FEED

Class of Farm Feed

Statement of Analysis

Cereal brands (undecorticated)

Percentages of protein, oil and fibre. Oilseed cakes or meals Percentages of protein and oil.

Oilseed cakes or meals (decorticated)

Percentages of protein, oil and fibre.

Meat and bone meal

Percentages of protein, oil and phosphorus.

Bone meal

Percentages of protein and phosphorus.

Meat meal

Percentages of protein, oil and phosphorus.

Fish meal

Percentages of protein, oil, phosphorus and salt.

Molasses

Percentage of sugar.

Molasses feed

Percentages of sugar and fibre.

Mixture of molasses and urea

Percentages of sugar and protein equivalent of urea.

Compound cakes and meals

Percentages of oil, fibre and protein (including the protein equivalent of urea, if any)

Concentrated or high energy feed

Percentages of oil, fibre and protein (including the protein equivalent of urea, if any); a statement of the proportions in which the feed should be mixed with other farm feed defined by name or class.

NOTES:

1. The amount of protein, except in the case of Compound Cakes and Concentrated or High Energy farm feed, means the amount of nitrogen other than ammoniacal, nitric or urea nitrogen, multiplied by 6.25. In the case of Compound Cakes and High Energy farm feed the amount of protein means the amount of nitrogen other than ammoniacal and nitric nitrogen multiplied by 6.25. The amount of protein equivalent of urea means the amount of urea nitrogen multiplied by 6.25.

2. In all cases the names of any added vitamins, minerals, antibiotics and synthetic or natural hormones shall be declared in the statement of analysis.

3. In all cases the maximum percentage of urea present in any farm feed shall be declared.

 

THIRD SCHEDULE

[Section 30 and regulation 14]

STATEMENTS OF ANALYSIS AND RECORDS TO BE KEPT FOR SALES UNDER TRADE NAMES, ETC.

Manufacturers of farm feeds shall keep records of all ingredients used in manufacturing any farm feed which is sold under a trade name, trade mark, trade label or trade brand. Such records shall be available for inspection at all reasonable times by a duly authorised officer, and shall be kept in such a manner as to enable the Registering Officer or any duly authorised officer to ascertain the materials from which any lot or batch of farm feed have been manufactured, and the proportions of such materials contained in the farm feed.

 

FOURTH SCHEDULE

[Section 52 and regulation 16]

DELETERIOUS INGREDIENTS IN FARM FEED

1. Salts soluble in water, if present in a farm feed in proportion likely to be injurious to the health of livestock.

2. All poisonous substances in quantities likely to be injurious to the health of livestock for which the farm feed is intended whether or not such substances are naturally present in the farm feed or material(s) from which the farm feed was manufactured.

3. Sand, siliceous matter or other insoluble mineral matter not naturally associated with ingredients of the farm feed which do not fall within the scope of this Schedule, or which, even if naturally so associated, are present in greater proportion than the maximum that may be expected to be due to such natural association.

4. For the purposes of this paragraph the term "insoluble" shall imply insolubility as determined by the prescribed method; the term "natural association" shall be construed as applying to average commercial samples of the farm feed or its ingredients with which it may be claimed that a particular mineral ingredient is associated.

 

FIFTH SCHEDULE

[Section 52 and regulation 17]

INGREDIENTS IN FARM FEED THE PRESENCE OF WHICH MUST BE DECLARED

1. Husks, chaff, glumes, hulls, nutshells or skins of nuts, from any source, whether ground or unground, treated or untreated, when used as separate ingredients or artificial mixtures in the manufacture of farm feed. Where the kernels naturally associated in seeds with one or other of the above materials are present in a farm feed along with material with which they are associated, regard shall be had to the proportion of the above materials that might reasonably be expected to accompany such kernels, when the seed from which they are derived is in its natural condition, provided that feeding in this condition is regarded as a common practice in the feeding of livestock.

2. Peat, peat moss or sugar cane pith, treated or untreated, ground or otherwise.

3. Wheat, maize or sorghum straw, maize rachis, ground or otherwise.

4. Sawdust or any other form of wood, treated or untreated.

 

SIXTH SCHEDULE

[Section 52(h) and regulations 19 and 20]

METHOD OR TAKING SAMPLES

NOTE - In this regulation "metric ton" is defined as 1,000 kg.

1. Where a farm feed is contained in packages the samples shall be taken from different parts of the whole quantity as follows:

   (a)   if the quantity does not exceed one ton, from not less than two unopened packages per ton or part thereof;

   (b)   if the quantity exceeds one ton but does not exceed two tons, from not less than four unopened packages;

   (c)   if the quantity exceeds two tons but does not exceed three tons, from not less than six unopened packages;

   (d)   if the quantity exceeds three tons, from one additional unopened package for every additional ton or part thereof, but in no case need samples be taken from more than 15 packages.

2. Where a farm feed is not contained in packages, a proportion calculated in accordance with paragraph 1 shall be taken from different parts of the whole quantity.

3. The samples shall be taken by means of a suitable sampling probe or by any other means as will ensure, as far as is practicable, the taking of a representative sample.

4. When a farm feed consists of material uneven in character, bulky or likely to get matted together, portions shall be taken from the selected packages, or from different parts of the farm feed if in bulk, any matted portions torn up, and all the portions thoroughly mixed together.

5. The samples thus taken shall be thoroughly mixed and reduced in size to give a final sample not exceeding six pounds in weight. This final sample shall be mixed and divided into three parts and each of these parts shall be transferred to a clean, dry, noncorrodible container capable of being closed in such a manner as to preserve the contents of the container in their original condition. These three containers shall be so sealed that they cannot be opened without breaking the seal. Each of these parts shall be marked with the name of the farm feed, date and place of sampling and the sample number together with the name of the inspector taking the sample.

6. When the farm feed is in liquid condition it should be thoroughly mixed before sampling. When in containers, samples shall be taken as follows:

Where the number of containers-

Portions shall be drawn from-

exceeds 1 but does not exceed 20

not less than 2 containers

exceed 20 but does not exceed 40

not less than 4 containers

exceed 40 but does not exceed 60

not less than 6 containers

exceed 60

one extra container for every 20 containers by which the total exceeds 60.

Where the farm feed is in liquid condition and is in bulk a representative sample shall be taken in accordance with the scale of sampling set out above.

The portions drawn shall be mixed together in a clean, dry container and a sample of 1 kg weight shall be taken. The sample shall be divided into three equal parts by pouring successive portions into each of three clear glass bottles or jars, preferably with wide mouths. The bottles or jars shall be provided with air-tight stoppers or with lids which shall be so fastened that spillage or evaporation of the contents is prevented. Each of the bottles or jars shall be so sealed that they cannot be opened without breaking the seal. Each of the bottles or jars shall be marked with the name of the farm feed, date and place of sampling and the sample number together with the name of the inspector taking the sample.

7. In the case of all samples the first part shall be given to the owner or seller of the farm feed or his agent, the second part shall be delivered to an approved analyst for analysis and the third part shall be retained by the inspector for a period of not less than six months after the date on which the report or certificate of analysis is issued.

8. A certificate of sampling (Form FERT 13 in the First Schedule to the Agriculture (Fertilisers) Regulations, 1969) shall be made out in triplicate at the time of sampling and the relevant copies as detailed in the form should accompany each part of the sample.

 

SEVENTH SCHEDULE

[Section 52(i) and regulation 21]

METHODS OF ANALYSIS

NOTE:

1. In this Schedule "water" means distilled or purified water except where stated.

2. Reagents should be of the appropriate analytical purity.

PREPARATION OF SAMPLE

   (a)   If the sample is in a fine condition and passes through a sieve having apertures of one millimetre square, it shall be thoroughly mixed and a portion not less than 100 grams in weight shall be placed in a stoppered bottle. From this portion the quantities for analysis shall be taken.

   (b)   If the sample does not wholly pass through a sieve having apertures of one millimetre square and wholly passes through a sieve having apertures of three millimetres square, it shall be thoroughly mixed and a portion for the determination of the moisture content shall be taken at once.

   (c)   If the sample is in a coarse condition as, for example, pieces of cake, it shall be carefully pulverised until the whole passes through a sieve having apertures of three millimetres square. It shall then be thoroughly mixed and a portion for the determination of the moisture content shall be taken at once.

   (d)   From the mixed sample as in (b) above, or from the coarsely crushed sample as in (c) above, a portion not less than 100 grams in weight shall be taken and further powdered and passed through a sieve having apertures of one millimetre square. The portion of the sample so prepared shall be placed in a stoppered bottle and from it the quantities for analysis shall be taken.

   (e)   If the original sample is appreciably moist, or if for any reason the operations of pulverisation and mixing are likely to result in loss or gain of moisture, the moisture in the bottled portion shall be determined as well as in the portion taken for that purpose under (b) or (c) above in order that the results of the analysis may be corrected to correspond with the original sample as regards moisture.

   (f)   Materials which cannot conveniently be pulverised or passed through a sieve shall be thoroughly mixed by the most suitable means.

DETERMINATION OF MOISTURE

A weighed quantity of the sample shall be dried at 100ºC and then be reweighed.

DETERMINATION OF OIL OR FAT (ETHER EXTRACT)

Reagents:

Petroleum ether-light petroleum-b.p. 40ºC to 60ºC.

NOTE - If ambient temperature of the laboratory demands then petroleum ether- light petroleum-of b.p.

60ºC to 80ºC may be used.

METHOD

Extract 2 to 5 grams of the sample, which has been dried for 1 hour at 100ºC, in a Soxhlet extraction apparatus with petroleum ether for a period of at least 6 hours. After evaporation of the solvent, dry the oil or fat for 30 minutes at 100ºC, cool in a desiccator and weigh. Calculate the oil or fat percentage as follows:

where A = weight in grams of the Soxhlet flask after extraction

B = weight in grams of the Soxhlet flask before extraction

C = weight in grams of the sample taken.

DETERMINATION OF FIBRE

Reagents:

Sulphuric acid solution - Prepare a solution containing 1.25 grams of sulphuric acid per 100 ml from chemically pure sulphuric acid. (0.255N).

Sodium hydroxide solution - Prepare a solution containing 1.25 grams of sodium hydroxide from carbonate-free sodium hydroxide. (0.313N).

Dilute hydrochloric acid solution (1:100). Ethyl alcohol (95 per cent v/v).

METHOD

Transfer a 2 to 3 gram sample, from which the bulk of the oil or fat has been extracted, to a conical flask (1 litre). Measure 200 ml of the sulphuric acid solution and heat to boiling; add to the flask, connect the flask to a condenser and heat. Bring the contents of the flask to boiling within one minute and boil gently and continuously for exactly 30 minutes. Rotate the flask at intervals of about 5 minutes to mix the contents thoroughly; do not allow any material to adhere to the sides of the flask out of contact with the solution.

At the end of 30 minutes remove the flask and immediately filter with suction through a Whatman No. 54 or No. 541 filter paper (or equivalent) fitted to a Hartley funnel or Buchner funnel. The time of filtration of the bulk of the 200 ml of liquid should not exceed 10 minutes. Wash with boiling water until the washings are free from acid.

Wash the material back into the flask with 200 ml of sodium hydroxide solution (measured at ordinary temperature and heated to boiling point). Boil again for exactly 30 minutes, observing the precautions stated for the acid treatment.

At the end of 30 minutes, remove the flask and immediately either filter direct through a suitable filter crucible or through filter paper and then transfer the charge to a filter crucible for washing. Wash thoroughly with boiling water, then with dilute hydrochloric acid solution, again with boiling water until free from acid and finally three times with ethyl alcohol.

Dry the crucible and residue for 2 hours at 100ºC, cool in a desiccator and weigh. Ignite until free from carbonaceous matter at a temperature not exceeding 600ºC, cool in a desiccator and weigh.

Calculate the percentage of fibre as follows:

Where A = weight in grams of residue after drying

B = weight in grams of residue after washing

C = weight in grams of the sample taken.

DETERMINATION OF ASH

Weigh out accurately 2 to 5 grams of the sample into a tared porcelain or silica dish, previously heated to a temperature of 500ºC and cooled. Char carefully and ignite in a muffle furnace at a temperature of

500ºC for 2 hours or until combustion is complete. Cool in a desiccator and weigh. Calculate the

percentage of ash as follows:

Where A = weight in grams of wash

B = weight in grams of the sample taken.

DETERMINATION OF SALT

Mix 5 grams of the sample with 1 gram of pure sodium carbonate or calcium oxide and thoroughly wet the mixture with a little water. Dry the mixture and heat at a temperature not exceeding 500ºC in order to destroy organic matter. Extract the residue with hot water, make up the volume to 250 ml and filter. Determine the chlorine in an aliquot part of the filtrate and express the result in terms of sodium chloride (NaCl).

DETERMINATION OF PHOSPHORUS

Phosphorus may be determined by either of the matter described below.

QUINOLINIUM PHOSPHOMOLYBDATE METHOD

Reagents:

Calcium oxide - finely ground.

Citric - molybdate acid solution-Stir 54 g of molybdenum trioxide (MoO3) with 200 ml of water; add 11 g sodium hydroxide and stir the mixture whilst heating to boiling point until the molybdenum trioxide dissolves. Dissolve 60 g citric acid in about 250 to 300 ml water and add 140 ml concentrated hydrochloric acid. Pour the molybdate solution into the acid solution, which is stirred throughout the addition. Then cool and, if necessary, filter the solution through a 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 or 1 per cent) solution of potassium bromate until the colour is discharged. This reagent should be kept in the dark.

Hydrochloric Acid, concentrated (S.G. 1.18).

Hydrocloric Acid 25 per cent v/v-Dilute 25 ml of concentrated hydrochloric acid with water to 100 ml. Hydrochloric Acid, 0.5N.

Hydrochloric Acid, 0.1N.

Indicator Solution - Mix 3 volumes of thymol blue solution and 2 volumes of phenolphthalein solution prepared as follows:

Thymol blue solution - Dissolve 0.25 g thymol blue in 5.5 ml of 0.1N sodium hydroxide solution and 125 ml industrial methylated spirit. Dilute with water to 250 ml. Phenolphthalein solution-Dissolve 0.25 g phenolphthalein in 150 ml of industrial methylated spirit and dilute with water to 250 ml.

Reagents:

Nitric Acid, concentrated (S.G. 1.42).

Quinoline Solution - Measure 60 ml concentrated hydrochloric acid and 300 to 400 ml water into a 1 litre beaker and warm to 70º-80ºC. Pour 50 ml quinoline in a thin stream into the diluted acid, whilst stirring. When the quinoline has dissolved, cool the solution, dilute to 1 litre and, if necessary, filter through a paper pulp filter.

Sodium Hydroxide, 5N.

Sodium Hydroxide, 0.5N - carbonate free.

Sodium Hydroxide, 0.1N-carbonate free.

Surface Active Agent - 0.5 per cent solution of sodium dodecylbenzene-sulphonate is suitable.

DISSOLUTION OF THE SAMPLE

Weigh to the nearest mg about 5 g of the sample into a capsule or dish; add 1 g of calcium oxide, mix well and thoroughly wet with a little water. Dry the mixture and incinerate at a temperature not exceeding 500ºC until completely charred. Cool, transfer the contents of the capsule or dish to a 250 ml beaker and add 10 ml water; then slowly add 12 ml of concentrated hydrochloric acid, taking suitable precautions to avoid loss by effervescence, and finally add 5 ml concentrated nitric acid. Heat to incipient boiling and keep at this temperature for 10 minutes. Dilute with about 10 ml water, filter, transfer the insoluble matter to the filter paper with a minimum amount of water and wash twice with small volumes of water. Then transfer the filter paper and insoluble matter to the original capsule or dish and incinerate until all the carbon is destroyed. Combine the ash with the filtrate and heat to boiling point. Cool, transfer to a 250 ml volumetric flask, dilute to the mark, mix well and filter. Discard the first 10 or 20 ml of the filtrate.

METHOD

Transfer a volume of the filtrate containing less than 30 mg phosphorus (P) and preferably about 22 mg phosphorus (P) to 500 ml stoppered conical flask marked at 150 ml. Dilute solution with water to 100 ml and 5N sodium hydroxide solution until a faint permanent turbidity or precipitate is formed. Dissolve the precipitate by the dropwise addition of 25 per cent hydrochloric acid, but avoid an excess.

Dilute to 150 ml, add 50 ml of the citric-molybdate solution, heat to incipient ebullition, maintain it at this temperature for 3 minutes and then bring it to boiling point. From a burette slowly add 25 ml of the quinoline solution with constant swirling throughout, the first few ml being added dropwise, the rest in a slow stream. Keep the solution gently boiling during the addition.

Immerse the flask in boiling (tap) water for 5 minutes, then cool it to 15ºC in running tap water. 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. Transfer the filter pad and precipitate to the original flask, rinse the funnel with water and collect the rinsings in the flask. If necessary, wipe the funnel with a small piece of damp filter paper to ensure complete removal of the precipitate, and place the paper in the flask. Add water to a total of about but not exceeding 100 ml. Stopper the flask and shake it vigorously until the pulp and precipitate are completely dispersed.

Remove the stopper and wash it with water, returning the washings to the flask. Add a measured volume of 0.5N sodium hydroxide solution sufficient to dissolve the precipitate and leave a few ml in excess. Shake the flask vigorously until all the precipitate dissolves. (To facilitate the dispersal of the precipitate after the addition of the 0.5N sodium hydroxide solution, a few drops of the surface active agent may be added if necessary.) Add 0.5-1.0 ml of the indicator solution, and titrate the excess of sodium hydroxide with the 0.5N hydrochloric acid until the indicator changes from violet to green-blue and then very sharply to yellow at the end-point. Deduct the number of ml of 0.5N hydrochloric acid used from the number of ml of 0.5N sodium hydroxide to ascertain the volume of 0.5N sodium hydroxide equivalent to the phosphorus.

Carry out a blank determination on all the reagents, omitting only the sample, and using 0.1N standard alkali and acid instead of 0.5N for the titration. Calculate the amount of phosphorus in the portion taken for analysis from the factor 1.0 ml of 0.5N sodium hydroxide = 0.597 mg P (1.366 mg P2O5).

Reagents:

Calcium Oxide - finely ground.

Hydrochloric Acid, concentrated (S.G. 1.18).

Nitric Acid, concentrated (S.G. 1.42).

Potassium Dihydrogen Phosphate Solution (stock phosphate solution)-Dissolve in water 1.917 g of potassium dihydrogen phosphate previously dried at 105ºC for 1 hour and dilute to 1 litre.

Potassium Dihydrogen Phosphate Solution (standard phosphate solution) - Dilute 50 ml of stock solution to 250 ml with water. 1 ml of this solution = 0.0874 mg phosphorus (0.2 mg P2O5).

Vanado-Molybdate Reagent - Dissolve separately 20 g of ammonium molybdate and 1 g of ammonium vanadate in water, mix, acidify with 140 ml of concentrated nitric acid and dilute to 1 litre.

STANDARDISATION OF INSTRUMENT

From a burette measure into a series of 100 ml volumetric flasks 25.0, 26.0, 27.0, 28.0, 30.0 and 31.0 ml of the standard phosphate solution (i.e. 0.219, 0.227, 0.236, 0.245, 0.254, 0.262 and 0.271 mg phosphorus, corresponding to 5.0, 5.2, 5.4, 5.6, 5.8, 6.0 and 6.2 mg P2O5). Add 25 ml of the vanado- molybdate reagent to each flask and dilute to 100 ml with water. Shake and allow to stand for 10 minutes.

Set the spectrophotometer to the correct wavelength, about 4,200, fill two 1 cm cells with the 0.219 mg solution and check the extinction of the cells. If there is a small difference select the cell with the smaller reading as the standard reference cell.

Determine the apparent extinction (corrected for cell differences) of the 0.227, 0.236, 0.245, 0.254, 0.262 and 0.271 mg phosphorus solutions referred to the 0.219 mg phosphorus solution as standard. Plot a calibration graph of scale readings against known phosphorus content.

ANALYSIS OF THE SAMPLE

Successively dilute a portion of the solution prepared as described under "Dissolution of the Sample" so that the final volume of about 25 ml contains between 2.404 and 2.709 mg of phosphorus (corresponding to 5.5 and 6.2 mg P2O5 respectively).

Transfer this final volume to a 100 ml volumetric flask, add 25 ml of the vanado-molybdate reagent, dilute to the mark, mix, and allow to stand for 10 minutes. At the same time transfer 25 ml of the standard phosphorus solution into a second 100 ml volumetric flask. Add 25 ml of the vanado- molybdate reagent, dilute to the mark, mix, and allow to stand for 10 minutes.

Measure the difference in extinction between the two solutions and estimate the phosphorus content of the volume of the unknown solution from the calibration graph. Calculate the phosphorus content of the sample from the known dilution factors and the weight of the sample.

NOTE - Prepare a fresh reference standard for each series of readings on the instrument.

DETERMINATION OF PROTEIN

The percentage of protein, except in the case of compound cakes or meals and concentrated or high energy farm feed, shall be ascertained by multiplying the percentage of nitrogen, other than nitrogen present as ammoniacal, nitric or urea nitrogen, by 6.25. The presence of nitrogen in these latter forms shall be tested for and the quantity, if any, shall be determined and deducted from the total nitrogen.

In the case of compound cakes or meals and concentrated or high energy farm feed the percentage of protein shall be ascertained by multiplying the percentage of nitrogen, other than nitrogen present as ammoniacal or nitric nitrogen, by 6.25. The presence of nitrogen in these latter forms shall be tested for and the quantity, if any, shall be determined and deducted from the total nitrogen.

NITROGEN

Reagents:

Mixed Indicator Solution - Grind together in an agate mortar 0.6 g of methyl red and 0.6 g of methylene blue. Dissolve the mixture in 500 ml of 95 per cent ethanol. Shake, filter and store in a dark glass bottle.

2 per cent Boric acid solution - Dissolve 20 g of boric acid in water, dilute to 1 litre and add 5 ml of the mixed indicator solution. Concentrated sulphuric acid S.G. 1.84.

Anhydrous sodium sulphate.

Cupric sulphate.

Paraffin wax.

Granulated zinc.

Hydrochloric acid 0.1N.

Sodium Hydroxide solution-50 per cent w/v.

METHOD

Weigh accurately 1 to 2 g of the sample (or such an amount as shall not contain more than 250 mg of nitrogen) and transfer to a kjeldahl flask. Add 25 ml of concentrated sulphuric acid and approximately 10 g of anhydrous sodium sulphate containing 0.4 g of cupric sulphate. Heat gently until frothing ceases, then strongly until the solution becomes clear and almost colourless. Continue heating for at least another hour. Avoid local overheating. If frothing is excessive, add about 0.5 g paraffin wax.

Dissolve the cooled digest in water and make up to a total volume of about 250 ml. Taking precautions against loss of ammonia add some zinc granules and sufficient 50 per cent sodium hydroxide solution to neutralise the acid and to give about 10 ml in excess, mix well and immediately connect to a distillation apparatus. Distil into an appropriate volume of 2 per cent boric acid solution. Titrate the contents of the receiving flask with 0.1N hydrochloric acid. Carry out a blank test using 2 g of sucrose in the place of the sample, and subtract the titration value of the blank from that of the sample. Express the result in terms of nitrogen.

1 ml of 0.1N hydrochloric acid = 0.0014 g nitrogen.

UREA NITROGEN

Reagents:

Activated charcoal.

Carrez solution 1 - Dissolve 21.9 g zinc acetate dihydrate in water, add 3 ml glacial acetic acid and dilute to 100 ml with water.

Carrez solution 2 - Dissolve 10.6 g potassium ferrocyanide in water and dilute to 100 ml. p- Dimethylaminobenzaldehyde solution-Dissolve 2 g of p - Dimethylaminobenzaldehyde in 10 ml of concentrated hydrochloric acid and dilute to 100 ml with propan-2-ol.

Hydrochloric acid-0.02N.

Sodium acetate solution - Dissolve 136 g sodium acetate (CH3COONa.3H2O) in water and dilute to 1 litre.

Urea standard solution - Dissolve 1 g urea in water and dilute to 100 ml.

METHOD

Weight to the nearest mg about 5 g of the sample (or such an amount as shall contain not more than 250 mg urea) and transfer to a 250 ml volumetric flask. Add 150 ml of 0.02N hydrochloric acid, shake for 30 minutes then add 10 ml of sodium acetate solution and mix well. Add 1 g of activated charcoal (see Note) to the flask and shake well, and stand for a further 15 minutes. Add 5 ml of Carrez solution 1, followed by 5 ml of Carrez solution 2 mixing well between additions. Dilute to volume with water and mix well. Filter a portion through a suitable dry filter paper into a dry clean 250 ml beaker. Transfer a 10 ml aliquot of the filtrate to a 50 ml flask, add 10.0 ml of p-dimethylaminobenzaldehyde solution, dilute to 50 ml with water, mix well and allow to stand for 10 minutes. Determine the extinction of the solution at 4,350 using a 1 cm cell against a blank of 10 ml of p-dimethylaminobenzaldehyde reagent

diluted to 50 ml with water. Calculate the urea content of the sample by reference to a calibration graph prepared at the same time as the test sample. (mg urea multiplied by 0.4665 = mg urea nitrogen.)

Establish the calibration graph as follows:

Measure amounts of standard urea solution corresponding to 50, 100, 150, 200 and 250 mg of urea into a series of 250 ml volumetric flasks and proceed as described above commencing at "Add 150 ml 0.02N hydrochloric acid".

Measure the extinctions of the solutions, and construct a graph relating the extinctions to the mg of urea.

NOTE - If the sample is highly coloured the proportion of activated charcoal must be increased up to 5 g. The final solution after filtering should be colourless.

DETERMINATION OF SUGAR

Reagents:

Fehling's solution - Mix equal volumes of a solution of copper sulphate and a solution of sodium potassium tartrate prepared as follows:

Copper sulphate solution-Dissolve 69.28 g of copper sulphate (CUSO4.5H2O) in water and dilute to 1 litre.

Sodium potassium tartrate solution - Dissolve 346 g of sodium potassium tartrate and 100 g of sodium hydroxide in water and dilute to 1 litre.

NOTE - The strength of the Fehling's solution should be such that 10 ml is equivalent to 0.0525 g invert sugar. It should be checked by titrating with a solution of pure sucrose (inverted by the procedure described in the note following the paragraph on "Exact Determination" below) using the procedure described in the paragraph.

Hydrochloric acid N.

Methylene blue solution - Dissolve 2.5 g methylene blue in water and dilute to 250 ml.

Phenolphthalein indicator solution-Dissolve 0.25 g of phenolphthalein in 150 ml of industrial methylated spirit and dilute with water to 250 ml.

Potassium ferrocyanide solution-Dissolve 106 g of potassium ferrocyanide in water and dilute to 1 litre. Potassium oxalate solution-Dissolve 50 g of potassium oxalate in water and dilute to 1 litre.

Sodium hydroxide, 10 per cent w/v-Dissolve 100 g of sodium hydroxide in water and dilute to 1 litre.

Zinc acetate solution-Dissolve 219 g of zinc acetate and 30 ml of glacial acetic acid in water and dilute to 1 litre.

PROCEDURE

Preparation of sample.

WHEN THE SUBSTANCE IS IN SOLID FORM

Weigh to the nearest centigram about 10 g of the sample or a sufficient quantity to contain about 2 g of sugar. Grind in a mortar with hot water (temperature not to exceed 60ºC) and transfer to a 500 ml volumetric flask using in all about 400 ml of water. Shake the flask at intervals during 30 minutes. Add 5 ml of potassium oxalate solution to the contents of the flask, followed by 5 ml of zinc acetate solution; mix well and then add 5 ml of potassium ferrocyanide solution, make up with water to 500 ml at the correct temperature, mix well and filter. Determine the sugar in 100 ml of the filtrate by the method described below.

WHEN THE SUBSTANCE IS IN LIQUID FORM

Weigh to the nearest mg about 5 g of the sample and wash with water into a 250 ml volumetric flask using about 200 ml of water. To clear the solution add 5 ml of zinc acetate solution. Mix, then add 5 ml of potassium ferrocyanide solution, again mix, dilute to 250 ml, mix and filter. Determine the sugar in 25 ml of the filtrate by the method described below.

DETERMINATION OF THE SUGAR CONTENT

Transfer the measured volume of filtrate obtained as described above to a suitable beaker, add 15 ml of N hydrochloric acid, dilute to 150 ml with water, cover with watch glass and heat to boiling point. Continue to boil for 2 minutes, cool, add 2 or 3 drops of phenolphthalein indicator solution, just neutralise with 10 per cent sodium hydroxide solution, transfer to a 200 ml volumetric flask and dilute to 200 ml. Filter if necessary.

PRELIMINARY ESTIMATION

(This estimation is usually necessary where the percentage of sugar is unknown.) Transfer exactly 10 ml of Fehling's solution to a 250 ml conical flask and add 20 ml of water. Add from a burette approximately10 ml of the filtrate prepared as described above, heat to boiling point and boil briskly for 1 minute. Add 3 drops of methylene blue solution and titrate from the burette at the rate of 1 ml per 15 seconds until the blue colour is discharged, the contents of the flask being kept boiling throughout the titration. Note the total number of ml required and call this x ml. This titration should not be outside the range of 15-40 ml otherwise the determination should be repeated using a more appropriate volume of the filtrate.

EXACT DETERMINATION

To 10 ml of Fehling's solution in a 250 ml conical flask add from burette (x-1) ml of the filtrate, together with sufficient water to make a total volume of 60 ml. Heat to boiling point, boil briskly for 11/2 minutes and add 3 drops of methylene blue solution. Titrate from the burette at a rate of approximately 0.25 ml per 15 seconds until the blue colour is discharged, the contents of the flask being kept boiling briskly throughout the titration which must not take more than 11/2 minutes. Then the total number of ml used in the determination equals the sugar equivalent of 10 ml of Fehling's solution.

10 ml of Fehling's solution=0.0525 g invert sugar.

Not more than 1 ml of filtrate should be required for completion of the titration. If more than 1 ml is required then the determination should be repeated using a more closely calculated volume of filtrate for the original addition. The time taken from the initial boiling point until the end of the titration should be about 3 minutes. If this time is exceeded by more than about 20 seconds, the titration should be repeated.

The total copper reducing power should finally be determined in terms of sugar (C12H22O11). NOTE-The Fehling's solution may be standardised as follows:

Dissolve 2.375 g sucrose (dried at 100ºC) in about 100 ml of water in a suitable beaker, add 15 ml of N hydrochloric acid and sufficient water to give a volume of 150 ml. Heat to boiling point, boil for 2 minutes, cool, add 2 or 3 drops of phenolphthalein solution, just neutralise with 10 per cent sodium hydroxide solution, transfer to a 500 ml volumetric flask, dilute to 50 ml. then follow the procedure described in "Exact Determination" above.

1 ml of the solution = 0.00475 invert sugar, i.e., 10 ml of Fehling's solution = 10.5 ml of this standard invert sugar solution.

DETERMINATION OF SAND, SILICEOUS MATTER OR OTHER INSOLUBLE MINERAL MATTER

Reagents:

Hydrochloric acid, concentrated, S.G. 1.18.

Hydrochloric acid, 25 per cent v/v - Dilute 25 ml of concentrated hydrochloric acid with water to 100 ml.

PROCEDURE

Weigh to the nearest mg from 2-5 g of the sample and incinerate until all the carbon has been destroyed. (The ash obtained from the method for "Determination of Ash" may be used for this determination.) Moisten with concentrated hydrochloric acid, evaporate to dryness, bake to render the silica insoluble, and then extract repeatedly with hot 25 per cent hydrochloric acid. Filter, wash the insoluble matter and weigh. Regard the quantity obtained as sand and siliceous matter.

 

EIGHTH SCHEDULE

[Section 52(g) and regulation 22]

LIMITS OF VARIATION

Farm Feed

Limits of Variation

Cereal brands   . .   . .   . .

Protein, one tenth of the amount stated. Oil, 0.75 per cent or one tenth of the amount stated, whichever is the greater. Fibre, one eighth of the amount stated.

Oilseed meals or cakes (undecorticated)   . .   . .

Protein, one tenth of the amount stated. Oil, 0.75 per cent or one tenth of the amount stated, whichever is the greater.

Oilseed meals or cakes (decorticated)   . .   . .   . .

Protein, one tenth of the amount stated. Oil, 0.75 per cent or one tenth of the amount stated, whichever is the greater. Fibre, one eighth of the amount stated.

Meat and bone meal   . .   . .

Protein, one tenth of the amount stated. Oil, 0.75 per cent or one tenth of the amount stated, whichever is the greater. Phosphorus, one tenth of the amount stated.

Bone meal   . .   . .   . .

Protein, one tenth of the amount stated.

Meat meal   . .   . .   . .

Phosphorus, one tenth of the amount stated. Protein, one tenth of the amount stated. Oil, 0.75 per cent or one tenth of the amount stated, whichever is the greater.

Fish meal   . .   . .   . .

Protein, one tenth of the amount stated. Oil, 0.75 per cent or one tenth of the amount stated, whichever is the Salt, 0.75 greater. Phosphorus, one tenth of the amount stated. percent.

Molasses   . .   . .   . .

Sugar, one twentieth of the amount stated.

Molasses feed   . .   . .   . .

one eighth of the Sugar, one tenth of the amount stated. Fibre, amount stated.

Mixtures of molasses and
urea   . .   . .   . .   . .

Sugar, one tenth of the amount stated. Protein equivalent of urea, one fifth of the amount stated.

Compound cakes and meals,
and    . .   . .   . .   . .

Protein, one tenth of the amount stated. Protein, concentrated or one feed, high energy farm equivalent of urea, 1.25 per cent or tenth of the fifth of the amount stated. Oil, 0.75 per cent or one eighth of amount stated, whichever is the greater. Fibre, one the amount stated.

{/mprestriction}