The Fertilisers (Sampling and Analysis) (Amendment) Regulations 1991

• Citation: S.I. 1991/2824
• Sections: 105

Section 1 Title, commencement and interpretation

(1) These Regulations may be cited as the Fertilisers (Sampling and Analysis) (Amendment) Regulations 1991 and shall come into force on 21st January 1992.

(2) In these Regulations, “the principal Regulations” means the Fertilisers (Sampling and Analysis) Regulations 1991 .

Section 2 Amendment of the principal Regulations

The principal Regulations are hereby amended in accordance with regulations 3 and 4 below.

Section 3 Amendment of the principal Regulations

(1) In regulation 2(3), for subparagraphs (b) and (c), there shall be substituted the following subparagraphs–

(b) if any container holds at least 5 tonnes the prescribed amount shall be 5 tonnes; and

(c) if neither subparagraph (a) nor (b) above applies, the prescribed amount shall be the contents of the lowest number of containers together holding at least 5 tonnes.

(2) In regulation 2(7), for subparagraphs (b) and (c) there shall be substituted the following subparagraphs–

(b) if any container holds at least 5,000 litres, the prescribed amount shall be 5,000 litres, and

(c) if neither subparagraph (a) nor (b) above applies, the prescribed amount shall be the contents of the lowest number of containers together holding at least 5,000 litres.

(3) For paragraph (2) of regulation 6 there shall be substituted the following paragraph–

(2) Analytical constituents of materials listed in Groups 1(a), 2(a) and 3(a) of Section A, Groups 1 to 4 of Section B, Groups 1(a), 1(b) and 2 of Section C, and Section E, of the table in Schedule 1 to the Fertilisers Regulations 1991 , shall be determined by the methods prescribed in Part I of Schedule 2.

Section 4 Amendment of the principal Regulations

(1) In Part I of Schedule 2–

(a) paragraph 1(b) shall be omitted;

(b) for paragraph 2 there shall be substituted the provisions set out in Schedule 1 to these Regulations;

(c) in paragraph 3–

(i) items 12a and b, and 13a and b shall be omitted, and

(ii) after item 16g (Determination of copper) there shall be added the provisions set out in Schedule 2 to these Regulations;

(d) in the 11th line of the table for method 10, for the lines indicating nil entries in the fifth and sixth columns there shall be substituted the figures “50” and “500” respectively;

(e) the provisions relating to the following methods of analysis shall be omitted–

(i) method 12a: Determination of water-soluble magnesium — atomic absorption spectrophotometric method,

(ii) method 12b: Determination of water-soluble magnesium — EDTA method,

(iii) method 13a: Determination of total magnesium — atomic absorption spectrophotometric method, and

(iv) method 13b: Determination of total magnesium — EDTA method;

(f) in paragraph 4.3 of method 16c: Determination of Combustible Ingredients, for the expression “(See Figure 1)” there shall be substituted the expression “(See Figure 9)”;

(g) after the provisions relating to method 16g: Determination of copper, there shall be added the provisions set out in Schedule 3 to these Regulations.

(2) In Part II of Schedule 2–

(a) paragraph 1(b) shall be omitted;

(b) for paragraph 2 there shall be substituted the provisions set out in Schedule 1 to these Regulations;

(c) in paragraph 3, for item 8 there shall be substituted

(8) Determination of zinc

(d) for the provisions relating to method 8: Determination of total magnesium, there shall be substituted the provisions set out in Schedule 4 to these Regulations.

(3) At the end of the Appendix to Schedule 2, there shall be inserted the Diagram and key set out in Schedule 5 to these Regulations.

(4) In Schedule 3–

(a) in the first column for the results of analysis, before the line referring to “Chlorine (C)”, there shall be inserted the following provisions–

Calcium oxide (CaO)

Total

Soluble in water

Sodium oxide (Na 2 O)

Total

Soluble in water

Sulphur trioxide (SO 3 )

Total

Soluble in water

(b) in the second column for the results of analysis–

(i) the expression “Magnesium (Mg)” shall be omitted, and

(ii) below the expression “Molybdenum (Mo)” there shall be added “Zinc (Zn)”.

Section 2

Reagents

Except where otherwise specified in the method of analysis, all reagents shall be of analytical quality. Where trace elements are to be determined, the purity of the reagents used shall be checked by means of a blank test.

Section 2A

Water

(a) Except where otherwise specified, a reference in this Part of this Schedule to water shall be a reference to demineralized or distilled water.

(b) For the determination of any form of nitrogen, water shall be free of all nitrogenous compounds and carbon dioxide.

(c) Except where the method of analysis specifies a particular solvent or diluent, all dissolution, dilution, rinsing and washing operations mentioned in the methods of analysis shall be carried out using water.

Section 2B

Apparatus

(a) Only special instruments and apparatus and specifically required apparatus and equipment are mentioned in the methods of analysis.

(b) Apparatus and equipment shall be clean.

(c) The accuracy of graduated glassware shall be assured by reference to the appropriate standards.

Section 17

Extraction of total calcium, total magnesium, total sodium and total sulphur in the form of sulphates

Section 18

Extraction of total sulphur

Section 19

Extraction of water-soluble calcium, magnesium, sodium and sulphur (in the form of sulphates)

Section 20

Extraction of water-soluble sulphur

Section 21

Extraction and determination of elemental sulphur

Section 22

Manganimetric determination of extracted calcium following precipitation in the form of oxalate

Section 23

Determination of magnesium by atomic absorption spectrophotometry

Section 24

Determination of magnesium by complexometry

Section 25

Determination of sulphates

Section 26

Determination of the sodium extracted

Section 1 Scope

This method is for the extraction of total calcium, total magnesium, total sodium and total sulphur present in the form of sulphates.

Section 1 Scope

This method is for the extraction of total sulphur contained in fertilisers in elemental form and/or in other chemical combinations.

Section 1 Scope

This method is for the extraction of water-soluble calcium, magnesium, sodium and sulphur (in the form of sulphates), so that the same extract can be used to determine each nutrient required.

Section 1 Scope

This method is for the extraction of water-soluble sulphur contained in fertilisers, in various forms.

Section 1 Scope

This method is for the extraction and determination of the elemental sulphur content of fertilisers.

Section 1 Scope

This method is for the determination of calcium in fertiliser extracts.

Section 1 Scope

This method is for the determination of magnesium in fertiliser extracts.

Section 1 Scope

This method is for the determination of magnesium in fertiliser extracts.

Section 1 Scope

This method is for the determination of sulphur present in fertiliser extracts in the form of sulphates.

Section 1 Scope

This method is for the determination of sodium in fertiliser extracts.

Section 2 Field of application

This method applies to all fertilisers, for which a declaration of the total calcium, total magnesium, total sodium and total sulphur in the form of sulphates is required.

Section 2 Field of application

This method applies to all fertilisers for which a declaration of the total sulphur present in various forms (elemental, thiosulphate, sulphite, sulphate) is required.

Section 2 Field of application

This method applies solely to fertilisers for which a declaration of the water-soluble calcium, magnesium, sodium and sulphur (in the form of sulphates) is required.

Section 2 Field of application

This method applies to all fertilisers for which a declaration of the water-soluble sulphur trioxide is required.

Section 2 Field of application

This method applies to all fertilisers for which a declaration of the total sulphur in elemental form is required.

Section 2 Field of application

This method applies to all fertilisers for which a declaration of the total and/or water-soluble calcium is required.

Section 2 Field of application

This method applies to all fertiliser extracts obtained by methods 17 and 19, for which a declaration of the total magnesium and/or water-soluble magnesium is required, with the exception of kieserite, magnesium sulphate, magnesium chloride solution and kieserite with potassium sulphate to which method 24 applies.

The method set out below applies to all fertiliser extracts containing elements in quantities that might interfere with the complexometric determination of magnesium.

Section 2 Field of application

This method applies to the determination of total magnesium and/or water-soluble magnesium in the following fertilisers:

straight nitrogenous fertilisers (calcium magnesium nitrate, magnesium sulphoni-trate, nitrogenous fertilisers with magnesium) and straight potassic fertilisers (enriched kainite, potassium chloride containing magnesium, potassium sulphate containing magnesium salt), kieserite, magnesium sulphate, magnesium chloride solution, and kieserite with potassium sulphate.

Section 2 Field of application

This method applies to the determination of sulphates present in the extractions performed in methods 17, 18, 19 and 20.

Section 2 Field of application

This method applies to fertilisers for which a declaration of sodium is required.

Section 3 Principle

Dissolution by boiling in dilute hydrochloric acid.

Section 3 Principle

Elemental sulphur is converted in an alkaline medium into polysulphides and thiosulphate; these, together with any sulphites which may be present, are then oxidized with hydrogen peroxide. The various forms of sulphur are thus converted into sulphate which is determined by precipitation as barium sulphate (method 25).

Section 3 Principle

The nutrients are dissolved in boiling water.

Section 3 Principle

Soluble forms of sulphur are dissolved in cold water and converted into sulphate by oxidation with hydrogen peroxide in an alkaline medium.

Section 3 Principle

After the removal of soluble compounds, elemental sulphur is extracted by using carbon disulphide, followed by gravimetric determination of the sulphur extracted.

Section 3 Principle

Precipitation of the calcium contained in an aliquot of the extraction solution in the form of an oxalate, which is determined by titration using potassium permanganate.

Section 3 Principle

Determination of magnesium by atomic absorption spectrophotometry after appropriate dilution of the extract.

Section 3 Principle

The magnesium is extracted by methods 17 and/or 19. First titration: with EDTA and Ca and Mg in the presence of Eriochrome black T. Second titration: with EDTA of Ca in the presence of calcein or of calcon carbonic acid. Determination of magnesium by difference.

Section 3 Principle

Gravimetric determination as barium sulphate.

Section 3 Principle

Following suitable dilution of the extract obtained via method 17 and/or 19 the sodium content of the solution is determined by flame-emission spectrophotometry.

Section 4 Reagents

(4.1) Diluted hydrochloric acid:

One volume of hydrochloric acid (d = 1.18 g/ml) plus one volume of water.

Section 4 Reagents

(4.1) Diluted hydrochloric acid:

One volume of hydrochloric acid (d = 1.18 g/ml) plus one volume of water.

(4.2) Sodium hydroxide solution, NaOH, 30% minimum (d = 1.33).

(4.3) Hydrogen peroxide solution, 30% w/w.

(4.4) Aqueous solution of barium chloride BaC1 2 2H 2 0, 122 gram per litre.

Section 4 Reagents

Distilled or demineralized water of equivalent quality.