The Fertilisers (Sampling and Analysis) Regulations 1991

This method is applicable to products in Groups 5(a) and 5(b) of Section A of the Table in Schedule I of the Fertilisers Regulations 1990[^f01031].

PRINCIPLE

2

The sample is dissolved in a measured quantity of standard hydrochloric acid, the excess of which is titrated with a standard solution of sodium hydroxide.

REAGENTS

3

• (3.1) Hydrochloric acid, 0.5 N solution.

• (3.2) Sodium hydroxide, 0.5 N solution (carbonate free).

• (3.3) Phenolphthalein indicator solution: dissolve 0.25 g phenolphthalein in 150 ml 95% ethanol and dilute with water to 250 ml.

PREPARATION OF SAMPLE

4

Rapidly grind 50 g of the representative lime sample to pass through a 1 mm sieve.

PROCEDURE

5

Determination 5.1 Weigh to the nearest 0.001 g, 0. 5 g of the prepared sample and transfer to a 300 ml conical flask. Add 50 ml of 0.5 N hydrochloric acid (3.1), cover the flask with a watch glass and boil the contents gently for five minutes. Cool the mixture to room temperature, add two or three drops of the phenolphthalein indicator (3.3) and titrate with 0.5 N sodium hydroxide solution (3.2) to the end point of the indicator.

EXPRESSION OF RESULTS

6

Determine the amount of hydrochloric acid consumed by the sample. 1 ml 0.5 N hydrochloric acid=0.01402 g calcium oxide (CaO).

16. — DETERMINATION OF FINENESS OF PRODUCTS OTHER THAN POTASSIC BASIC SLAG

SCOPE AND FIELD OF APPLICATION

1

This method is applicable to “Rock phosphate” in Group 2(b) and to products in Groups 4(c), 5(a) and 5(b) of Section A of the Table in Schedule I of the Fertilisers Regulations 1990[^f01032].

PRINCIPLE

2

By hand sieve shaking, the proportion of material passing through the prescribed sieve is determined.

APPARATUS

3

Sieves having square apertures of 45 mm, 6.7 mm, 6.3 mm, 5 mm, 3.35 mm, 1.0 mm and 150 microns; lower receiver to fit sieve. Test sieves conforming to British Standard 410: 1986 are suitable.

PROCEDURE

4

For sieving through 3.5 mm, 1.0 mm and 150 micron sieves 4.1 Thoroughly mix the sample and quarter down until a portion of about 100 g is obtained. Heat this portion at 1OO°C until dry and thoroughly mix. Weigh to the nearest 0.01 g, 20 g and transfer to the sieve with the lower receiver attached. Proceed as described in 4.4.

For sieving through 6.7 mm, 6.3 mm and 5 mm sieves 4.2 Oven dry the sample at 1OO°C for 24 hours and thoroughly mix. Weigh to the nearest 0.1 g, 200 g and transfer to the sieve with the lower receiver attached. Proceed as described in 4.4.

For sieving through a 45 mm sieve 4.3 If the sample appears moist or damp, oven dry at 1OO°C for 24 hours, but if the sample appears dry, heating is not necessary. Thoroughly mix the sample and weigh to the nearest 0.1 g, 500 g and transfer to the sieve with the lower receiver attached. Proceed as in 4.4.

Sieving 4.4 Shake the sieve for 5 minutes, frequently tapping the side. Disintegrate soft lumps such as can be caused to crumble by the application of the fibres of a soft brush, taking care that the hard part of the brush does not make contact with the sieve and that the brush is not used to brush particles through the sieve. Brush out the powder in the lower receiver and weigh. Replace the receiver and repeat the shaking and tapping procedure for 2 minutes. Add the powder in the receiver to the first portion and weigh. Repeat the process until not more than 0.04 g passes through the seive during 2 minutes.

EXPRESSION OF RESULTS

5

Calculate the fineness by expressing the weight of the material passing through the sieve as a percentage of the weight of the portion of the dried (or as the case may be, undried) sample taken for sieving.

17. — DETERMINATION OF FINENESS OF POTASSIC BASIC SLAG

SCOPE AND FIELD OF APPLICATION

1

Exclusively to “Potassic basic slag” in Group 3(b) of Section A of the Table in Schedule 1 of the Fertilisers Regulations 1990[^f01033].

PRINCIPLE

2

By hand sieve shaking and dissolution of the soluble salts, the proportion of slag passing through the prescribed sieve is determined.

APPARATUS

3

Sieve having square apertures of 0.5 mm (500 microns); lower receiver to fit sieve. Test sieves conforming to British Standard 410: 1986 are suitable.

PROCEDURE

4

Preparation of the sample 4.1 Thoroughly mix the sample and quarter down until a portion of about 100 g is obtained. Heat this portion at 1OO°C until dry and thoroughly mix.

Sieving 4.2 Weigh to the nearest 0.1 g, 20 g of the dry sample and transfer to the sieve with the lower receiver attached. Shake the sieve for five minutes, frequently tapping the sides. Disintegrate soft lumps that can be caused to crumble by the application of a soft brush, taking care that the hard part of the brush does not make contact with the sieve and that the brush is not used to brush particles through the sieve. Transfer the finer portion from the container into a 500 ml beaker and add 200 mi of previously boiled water. Stir and then filter through a weighed glass sintered crucible. Thoroughly wash the residue with water, dry and re-weigh the crucible. Calculate the weight of slag in the mixture with a particle size of less than 0.5 mm (A). Weigh to the nearest 0.01 g, about 20 g of the dry sample and transfer to a 500 ml conical flask. Add 200 ml previously boiled water and shake for 30 minutes. Filter through a weighed, sintered glass crucible, wash the residue thoroughly with water, dry and re-weigh the crucible. Calculate the total weight of slag in the mixture (B).

EXPRESSION OF RESULTS

5

$Express the fineness of the slag asAB×100.$

SCHEDULE 3 — FORM OF CERTIFICATE OF ANALYSIS

Signed

In witness whereof the Official Seal of the Minister of Agriculture, Fisheries and Food is hereunto affixed on

John Selwyn Gummer — Minister of Agriculture, Fisheries and Food — 26th March 1991.

Strathclyde — Parliamentary Under Secretary of State, Scottish Office — 27th March 1991

David Hunt — Secretary of State for Wales — 25th March 1991

Explanatory note

(This note is not part of the Regulations)

These Regulations, which apply throughout Great Britain, consolidate and supersede the Fertilisers (Sampling and Analysis) Regulations 1978 (SI. 1978/1108) and the Fertilisers (Sampling and Analysis) (Amendment) Regulations 1980 (SI. 1980/1130). They implement the Directives listed in paragraph 2 below.

2 The Directives implemented are: Commission Directive 77/535/EEC (OJ No. L213, 22.8.77) on the approximation of the laws of the Member States relating to methods of sampling and analysis for fertilisers; Commission Directive 79/138/EEC (OJ No. L39, 14.2.79, p. 3) amending Directive 77/535/EEC in respect of methods of analysis for magnesium; Commission Directive 87/94/EEC (OJ No. L38, 7.2.87) on the approximation of the laws of Member States relating to procedures for the control of characteristics of, limits for and, resistance to detonation of straight ammonium nitrate fertilisers of high nitrogen content; Commission Directive 87/566/EEC (OJ No. L342, 4.12.87, p. 32) amending Directive 77/535/EEC in respect of methods of sampling for fluid fertilisers; Commission Directive 88/126/EEC (OJ No. L63, 9.3.88, p. 12) amending Directive 87/94/EEC, in respect only of its date for implementation by the Member States.

3 The Regulations provide for a number of matters concerning the sampling and analysis of fertilisers including: a the amounts of fertilisers from which samples are to be taken (regulation 2); b the manner of taking, marking, sealing and fastening up of samples (regulation 3 and Schedule 1); c the methods of sending part of a sample (regulation 4); d the required qualifications of agricultural analysts and deputy agricultural analysts (regulation 5); e the methods by which analyses are to be carried out (regulation 6 and Schedule 2) and the form of certificate of analysis (regulation 7 and Schedule 3).

4 The principal changes from the superseded Regulations are the introduction of sampling procedures for fluid fertilisers (in Schedule 1) and of methods of analysis for straight ammonium nitrate fertiliser (in Schedule 2).

5 The Regulations come into force on 20th May 1991.

Footnotes

[^f00001]: 1970 c. 40; section 74A was inserted by paragraph 6 of Schedule 4 to the European Communities Act 1972 (c. 68) and the Act was amended by the Agriculture Act 1970 Amendment Regulations 1982 (S.I. 1982/980). Section 66(1) contains definitions of the expressions “prescribed” and “regulations”.

[^f00002]: In the case of the Secretary of State for Wales, by virtue of S.I. 1978/272.

[^f00003]: 1926 c. 45.

[^f00004]: S.I. 1990/887.

[^f00005]: S.I. 1978/1108.

[^f00006]: S.I. 1980/1130.

[^f00007]: Whatman 42 or equivalent.

[^f00008]: Whatman 42 or equivalent.

[^f00009]: Whatman 541 or equivalent.

[^f00010]: Whatman 541 or equivalent.

[^f00011]: Whatman 541 or equivalent.

[^f00012]: Commercially available standard copper solution may be used.

[^f00013]: Whatman 541 or equivalent.

[^f00014]: Commercially available standard iron solution may be used.

[^f00015]: Whatman 541 or equivalent.

[^f00016]: Whatman 541 or equivalent.

[^f00017]: Commercially available standard manganese solution may be used.

[^f00018]: Whatman 541 or equivalent.

[^f01003]: Biuret can be prified beforehand by washing with ammoniacal solution (10%), then with acetone and drying in a vacuum.

[^f01004]: S.I. 1990/887.

[^f01005]: S.I. 1990/887.

[^f01006]: S.I. 1990/887.

[^f01007]: S.I. 1990/887.

[^f01008]: S.I. 1990/887.

[^f01009]: Where the fertiliser is normal superphosphate or concentrated superphosphate in Group 2(a) of Section A, or NPK fertiliser in Group 1, NP fertiliser in Group 2, or PK fertiliser in Group 4 of Section B or NPK fertiliser suspension, NP fertiliser suspension or PK fertiliser suspension in Section C of the Table in Schedule 1 of the Fertilisers Regulations 1990.

[^f01010]: Where the fertiliser is triple superphosphate in Group 2(a) of Section A, or NPK fertiliser containing soft ground rock phosphate or partially solubilised rock phosphate in Group 1, or NP fertiliser containing soft ground rock phosphate or partially solubilised rock phosphate in Group 2, or PK fertiliser containing soft ground rock phosphate or partially rock phosphate in Group 4 of Section B of the Table in Schedule 1 of the Fertilisers Regulations 1990.

[^f01011]: If no mechnical shaker is available, the flask may be shaken by hand every 5 minutes.

[^f01012]: Phosphorus soluble in mineral acids, water soluble phosphorus, phosphorus soluble in solutions of ammonium citrate, phosphorus soluble in 2% citric acid and phosphorus soluble in 2% formic acid.

[^f01013]: 21 ml when the solution to be precipitated contains more than 15 ml of citrate solution (neutral citrate, Petermann or Joulie alkaline citrate).

[^f01014]: To precipitate phosphate solutions containing more than 15 ml citrate solution (neutral, Petermann or Joulie) which have been acified with 21 ml concentrated nitirc acid (see footnote to paragraph 6.1) use 80 ml of the precipitating reagent.

[^f01015]: S.I. 1990/887.

[^f01016]: S.I. 1990/887.

[^f01017]: S.I. 1990/887.

[^f01018]: S.I. 1990/887.

[^f01019]: S.I. 1990/887.

[^f01020]: S.I. 1990/887.

[^f01021]: A reaction time of one-and-a-half hours is sufficient in the case of most of the organic substances in the presence of silver nitrate catalyst.

[^f01022]: Commercially available standard copper solution may be used.

[^f01023]: Whatman 541 or equivalent.

[^f01024]: S.I. 1990/887.

[^f01025]: S.I. 1990/887.

[^f01026]: S.I. 1990/887.

[^f01027]: S.I. 1990/887.

[^f01028]: S.I. 1990/887.

[^f01029]: S.I. 1990/887.

[^f01030]: S.I. 1990/887.

[^f01031]: S.I. 1990/887.

[^f01032]: S.I. 1990/887.

[^f01033]: S.I. 1990/887.