Regulation (EC) No 2003/2003 of the European Parliament and of the Council

of 13 October 2003

relating to fertilisers

THE EUROPEAN PARLIAMENT AND THE COUNCIL OF THE EUROPEAN UNION,

Having regard to the Treaty establishing the European Community, and in particular Article 95 thereof,

Having regard to the proposal from the Commission(1),

Having regard to the Opinion of the European Economic and Social Committee(2),

Acting in accordance with the procedure laid down in Article 251 of the Treaty(3),

Whereas:

(1) Council Directive 76/116/EEC of 18 December 1975 on the approximation of the laws of the Member States relating to fertilisers(4), Council Directive 80/876/EEC of 15 July 1980 on the approximation of the laws of the Member States relating to straight ammonium nitrate fertilisers of high nitrogen content(5), Commission Directive 87/94/EEC of 8 December 1986 on the approximation of the laws of the 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(6), and Commission Directive 77/535/EEC of 22 June 1977 on the approximation of the laws of the Member States relating to methods of sampling and analysis for fertilisers(7), have been substantially amended several times. In accordance with the communication from the Commission to the European Parliament and the Council "Simpler legislation for the internal market" (SLIM) and the Action Plan for the Single Market those Directives should be repealed and replaced by a single legal instrument, in the interests of clarity.

(2) The Community legislation on fertilisers is very technical in its content. A Regulation is therefore the most appropriate legal instrument, as it imposes directly on manufacturers precise requirements to be applied at the same time and in the same manner throughout the Community.

(3) In each Member State fertilisers must display certain technical characteristics laid down by mandatory provisions. These provisions, concerning more particularly the composition and definition types of fertilisers, the designations of these types, their identification and their packaging, differ from one Member State to another. By their disparity they hinder trade within the Community and should therefore be harmonised.

(4) Since the objective of the proposed action, namely to ensure the internal market in fertilisers, cannot be sufficiently achieved by the Member States if there are no common technical criteria and can therefore, by reason of the scale of the action, be better achieved at Community level, the Community may adopt measures in accordance with the principle of subsidiarity as set out in Article 5 of the Treaty. In accordance with the principle of proportionality, as set out in that Article, this Regulation does not go beyond what is necessary in order to achieve this objective.

(5) It is necessary to determine at Community level the designation, definition and composition of certain fertilisers (EC fertilisers).

(6) Community rules on the identification, traceability and labelling of EC fertilisers and on the closure of the packages should also be laid down.

(7) A procedure should be established at Community level to be followed in cases where a Member State deems it necessary to restrict the placing on the market of EC fertilisers.

(8) The production of fertilisers is subject to varying degrees of fluctuation due to manufacturing techniques or basic materials. Sampling and analytical procedures may also contain variations. It is therefore necessary to authorise tolerances on the declared nutrient contents. In the interest of the agricultural user, it is advisable to keep these tolerances within narrow limits.

(9) Official controls on the compliance of EC fertilisers with requirements of this Regulation concerning quality and composition should be carried out by laboratories that are approved by the Member States and notified to the Commission.

(10) Ammonium nitrate is the essential ingredient of a variety of products, some of which are intended for use as fertilisers and others as explosives. It is necessary, having regard to the particular nature of ammonium nitrate fertilisers of high nitrogen content and to the consequent requirements regarding public safety, health and protection of workers, to lay down additional Community rules for EC fertilisers of this type.

(11) Certain of those products could be hazardous and could in certain instances be used for purposes other than those for which they were intended. This could well endanger the security of persons and property. Manufacturers should therefore be obliged to take appropriate steps to avoid such use, and in particular to ensure the traceability of such fertilisers.

(12) In the interest of public safety, it is particularly important to determine at Community level the characteristics and properties distinguishing ammonium nitrate EC fertilisers of high nitrogen content from varieties of ammonium nitrate used in the manufacture of products used as explosives.

(13) Ammonium nitrate EC fertilisers of high nitrogen content should conform to certain characteristics to ensure that they are harmless. Manufacturers should ensure that all high nitrogen content ammonium nitrate fertilisers have passed a test of resistance to detonation before those fertilisers are placed on the market.

(14) It is necessary to establish rules on the methods of the closed thermal cycles even if these methods may not necessarily simulate all conditions arising during transport and storage.

(15) Fertilisers can be contaminated by substances that can potentially pose a risk to human and animal health and the environment. Further to the opinion of the Scientific Committee on Toxicity, Ecotoxicity and the Environment (SCTEE), the Commission intends to address the issue of unintentional cadmium content in mineral fertilisers and will, where appropriate, draw up a proposal for a Regulation, which it intends to present to the European Parliament and the Council. Where appropriate, a similar review will be undertaken for other contaminants.

(16) It is appropriate to establish a procedure, to be observed by any manufacturer or its representative that wishes to include a new type of fertiliser in Annex I in order to use the marking "EC fertiliser".

(17) The measures necessary for the implementation of this Regulation should be adopted in accordance with Council Decision 1999/468/EC of 28 June 1999 laying down the procedures for the exercise of implementing powers conferred on the Commission(8).

(18) Member States should lay down penalties in respect of infringements of the provisions of this Regulation. They may provide that a manufacturer which infringes Article 27 can be fined an amount equivalent to ten times the market value of the shipment that fails to comply.

(19) Directives 76/116/EEC, 77/535/EEC, 80/876/EEC and 87/94/EEC should be repealed,

HAVE ADOPTED THIS REGULATION:

TITLE I

GENERAL PROVISIONS

CHAPTER I

Scope and definitions

Article 1

Scope

This Regulation shall apply to products which are placed on the market as fertilisers designated "EC fertiliser".

Article 2

Definitions

For the purposes of this Regulation the following definitions shall apply:

(a) "Fertiliser" means material, the main function of which is to provide nutrients for plants.

(b) "Primary nutrient" means the elements nitrogen, phosphorus and potassium only.

(c) "Secondary nutrient" means the elements calcium, magnesium, sodium and sulphur.

(d) "Micro-nutrients" means the elements boron, cobalt, copper, iron, manganese, molybdenum and zinc, essential for plant growth in quantities that are small compared with those of primary and secondary nutrients.

(e) "Inorganic fertiliser" means a fertiliser in which the declared nutrients are in the form of minerals obtained by extraction or by physical and/or chemical industrial processes. Calcium cyanamide, urea and its condensation and association products, and fertilisers containing chelated or complexed micro-nutrients may, by convention, be classed as inorganic fertilisers.

(f) "Chelated micro-nutrient" means a micro-nutrient that is held by one of the organic molecules listed in section E.3.1 of Annex I.

(g) "Complexed micro-nutrient" means a micro-nutrient that is held by one of the molecules listed in section E.3.2 of Annex I.

(h) "Type of fertilisers" means fertilisers with a common type designation as indicated in Annex I.

(i) "Straight fertiliser" means a nitrogenous, phosphatic or potassic fertiliser having a declarable content of only one of the primary nutrients.

(j) "Compound fertiliser" means a fertiliser having a declarable content of at least two of the primary nutrients and obtained chemically or by blending or by a combination of both.

(k) "Complex fertiliser" means a compound fertiliser, obtained by chemical reaction, by solution, or in its solid state by granulation, having a declarable content of at least two of the primary nutrients. In its solid state each granule contains all the nutrients in their declared composition.

(l) "Blended fertiliser" means a fertiliser obtained by dry mixing of several fertilisers, with no chemical reaction.

(m) "Foliar fertiliser" means a fertiliser suitable for application to and nutrient uptake by the foliage of a crop.

(n) "Fluid fertiliser" means a fertiliser in suspension or solution.

(o) "Solution fertiliser" means a fluid fertiliser that is free of solid particles.

(p) "Suspension fertiliser" means a two-phase fertiliser in which solid particles are maintained in suspension in the liquid phase.

(q) "Declaration" means a statement of the amount of nutrients, including their forms and solubility, guaranteed within specified tolerances.

(r) "Declared content" means the content of an element, or its oxide, which, in accordance with Community legislation, is given on a label of an EC fertiliser or on the relevant accompanying document.

(s) "Tolerance" means the permitted deviation of the measured value of a nutrient content from its declared value.

(t) "European Standard" means CEN (European Committee for Standardisation) standards, which have been officially recognised by the Community and whose reference has been published in the Official Journal of the European Communities.

(u) "Package" means a sealable receptacle used to hold, protect, handle, and distribute fertilisers and holding not more than 1000 kg.

(v) "Bulk" means a fertiliser not packaged as prescribed by this Regulation.

(w) "Placing on the market" means the supply of fertiliser, whether in return for payment or free of charge, or storage for the purpose of supply. Importation of a fertiliser into the customs territory of the European Community shall be deemed to constitute placing on the market.

(x) "Manufacturer" means the natural or legal person responsible for placing a fertiliser on the market; in particular a producer, an importer, a packager working for its own account, or any person changing the characteristics of a fertiliser, shall be deemed to be a manufacturer. However, a distributor who does not change the characteristics of the fertiliser shall not be deemed to be a manufacturer.

CHAPTER II

Placing on the market

Article 3

EC Fertiliser

A fertiliser belonging to a type of fertilisers listed in Annex I and complying with the conditions laid down in this Regulation, may be designated "EC fertiliser".

The designation "EC fertiliser" shall not be used for a fertiliser which does not comply with this Regulation.

Article 4

Establishment within the Community

The manufacturer shall be established within the Community and shall be responsible for the conformity of the "EC fertiliser" with the provisions of this Regulation.

Article 5

Free circulation

1. Without prejudice to Article 15 and other Community legislation, Member States shall not, on grounds of composition, identification, labelling or packaging, and other provisions contained in this Regulation, prohibit, restrict or hinder the placing on the market of fertilisers marked "EC fertiliser" which comply with the provisions of this Regulation.

2. Fertilisers that are marked "EC fertiliser" in accordance with this Regulation shall circulate freely within the Community.

Article 6

Compulsory statements

1. In order to satisfy the requirements of Article 9, Member States may prescribe that the indication of the nitrogen, phosphorus and potassium contents of fertilisers placed on their market is to be expressed in the following way:

(a) nitrogen solely in the elemental form (N); and either

(b) phosphorus and potassium solely in the elemental form (P, K); or

(c) phosphorus and potassium solely in the oxide form (P2O5, K2O); or

(d) phosphorus and potassium in both elemental and oxide forms simultaneously.

Where the option is chosen to prescribe that the phosphorus and potassium contents be expressed in the form of elements, all references in the Annexes to the oxide form shall be read as being in elemental form and the numerical values shall be converted using the following factors:

(a) phosphorus (P) = phosphorus pentoxide (P2O5) × 0,436;

(b) potassium (K) = potassium oxide (K2O) × 0,830.

2. Member States may prescribe that the calcium, magnesium, sodium and sulphur contents of secondary nutrient fertilisers and, where the conditions of Article 17 are fulfilled, of primary nutrient fertilisers placed on their markets are to be expressed:

(a) in the oxide form (CaO, MgO, Na2O, SO3); or

(b) in the elemental form (Ca, Mg, Na, S); or

(c) in both of these forms.

To convert the calcium oxide, magnesium oxide, sodium oxide and sulphur trioxide contents into calcium, magnesium, sodium and sulphur contents, the following factors shall be used:

(a) calcium (Ca) = calcium oxide (CaO) × 0,715;

(b) magnesium (Mg) = magnesium oxide (MgO) × 0,603;

(c) sodium (Na) = sodium oxide (Na2O) × 0,742;

(d) sulphur (S) = sulphur trioxide (SO3) × 0,400.

For the calculated oxide or elemental content, the figure declared shall be rounded to the nearest decimal place.

3. Member States shall not prevent the placing on the market of an "EC fertiliser" labelled in both of the forms mentioned in paragraphs 1 and 2.

4. The content of one or more of the micro-nutrients boron, cobalt, copper, iron, manganese, molybdenum, or zinc in the EC fertilisers belonging to the types of fertilisers listed in sections A, B, C and D of Annex I shall be declared where the following conditions are fulfilled:

(a) the micro-nutrients are added at least in the minimum quantities specified in section E.2.2 and E.2.3 of Annex I;

(b) the EC fertiliser continues to satisfy the requirements of sections A, B, C and D of Annex I.

5. Where the micro-nutrients are the normal ingredients of the raw materials intended to supply primary (N, P, K) and secondary (Ca, Mg, Na, S) nutrients, they may be declared, provided that these micro-nutrients are present at least in the minimum quantities specified in sections E.2.2 and E.2.3 of Annex I.

6. The micro-nutrient content shall be declared in the following manner:

(a) for fertilisers belonging to the types of fertilisers listed in section E.1 of Annex I, in accordance with the requirements set out in column 6 of that section;

(b) for mixtures of fertilisers referred to in (a) containing at least two different micro-nutrients and meeting the requirements of section E.2.1 of Annex I and for fertilisers belonging to the types of fertilisers listed in sections A, B, C and D of Annex I, by indicating:

(i) the total content, expressed as a percentage of the fertiliser by mass,

(ii) the water-soluble content, expressed as a percentage of the fertiliser by mass, where the soluble content is at least half of the total content.

Where a micro-nutrient is totally water-soluble, only the water-soluble content shall be declared.

Where a micro-nutrient is chemically linked with an organic molecule, the content of the micro-nutrient present in the fertiliser shall be declared immediately following the water-soluble content as a percentage by mass of the product, followed by one of the terms "chelated by", or "complexed by", with the name of the organic molecule as set out in section E.3 of Annex I. The name of the organic molecule may be replaced by its initials.

Article 7

Identification

1. The manufacturer shall provide EC fertilisers with the identification markings listed in Article 9.

2. If the fertilisers are packed, these identification markings shall appear on the packages or labels attached. If the fertilisers are in bulk, these markings shall appear on the accompanying documents.

Article 8

Traceability

Without prejudice to Article 26(3), the manufacturer shall, to ensure traceability of EC fertilisers, maintain records of the origin of the fertilisers. These records shall be available for inspection by Member States for as long as the fertiliser is being supplied to the market, and for a further period of 2 years after the manufacturer stopped supplying it.

Article 9

Markings

1. Without prejudice to other Community rules, the packages, labels and accompanying documents, referred to in Article 7 shall bear the following markings:

(a) Compulsory identification

- The words "EC FERTILISER" in capital letters;

- Where it exists, the designation of the type of fertiliser as set out in Annex 1;

- For blended fertilisers, the marking "blend" after the designation of the type;

- The additional markings specified in Article 19, 21 or 23;

- Nutrients shall be indicated both in words and by the appropriate chemical symbols, e.g. nitrogen (N), phosphorus (P), phosphorus pentoxide (P2O5), potassium (K), potassium oxide (K2O), calcium (Ca), calcium oxide (CaO), magnesium (Mg), magnesium oxide (MgO), sodium (Na), sodium oxide (Na2O), sulphur (S), sulphur trioxide (SO3), boron (B), copper (Cu), cobalt (Co), iron (Fe), manganese (Mn), molybdenum (Mo), zinc (Zn);

- If the fertiliser contains micro-nutrients of which all or part are chemically linked with an organic molecule, the name of the micro-nutrient shall be followed by one of the following qualifiers:

(i) "chelated by ..." (name of chelating agent or its abbreviation as set out in section E.3.1 of Annex I);

(ii) "complexed by ..." (name of complexing agent as set out in section E.3.2 of Annex I);

- Micro-nutrients contained in the fertiliser, listed in the alphabetical order of their chemical symbols: B, Co, Cu, Fe, Mn, Mo, Zn;

- For products listed in sections E.1 and E.2 of Annex I, the specific directions for use;

- Quantities of fluid fertilisers, expressed by mass. The expression of quantities of fluid fertilisers by volume or in terms of mass versus volume (kilograms per hectolitre or grams per litre) shall be optional;

- Net or gross mass and, optionally, volume for fluid fertilisers. If the gross mass is given, the tare mass must be indicated beside it;

- The name or trade name and the address of the manufacturer.

(b) Optional identification

- As listed in Annex I;

- The directions for the storage and handling, and for fertilisers not listed in Annex I, sections E.1 and E.2, the specific directions for the use of the fertiliser;

- Indications of the dose rates and conditions of use suitable for the soil and crop conditions under which the fertiliser is used;

- The mark of the manufacturer and the trade description of the product.

The indications referred to in (b) must not conflict with those referred to in (a) and must be clearly separated from them.

2. All the markings referred to in paragraph 1 must be clearly separated from any other information on the packages, labels and accompanying documents.

3. Fluid fertilisers may be placed on the market only if the manufacturer provides suitable additional instructions covering, in particular, storage temperature and prevention of accidents during storage.

4. Detailed rules for the application of this Article shall be adopted under the procedure referred to in Article 32(2).

Article 10

Labelling

1. The labels or markings printed on the package and giving the particulars mentioned under Article 9 must be placed in a conspicuous position. Labels must be attached to the package or to whatever system is used for closing it. If this system consists of a seal, that seal must bear the name or mark of the packager.

2. The markings referred to in paragraph 1 must be and must remain indelible and clearly legible.

3. In the cases of fertilisers in bulk referred to in the second sentence of Article 7(2) a copy of the documents containing the identification markings must accompany the goods and be accessible for inspection purposes.

Article 11

Languages

The label, the markings on the package and the accompanying documents must appear in at least the national language or languages of the Member State in which the EC fertiliser is marketed.

Article 12

Packaging

In the case of packaged EC fertilisers, the package must be closed in such a way or by such a device that, when it is opened, the fastening, fastening seal or the package itself is irreparably damaged. Valve sacks may be used.

Article 13

Tolerances

1. The nutrient content of EC fertilisers shall comply with the tolerances established in Annex II, which are intended to allow for deviations in manufacture, sampling and analysis.

2. The manufacturer shall not take systematic advantage of the tolerances given in Annex II.

3. No tolerances are allowed in respect of the minimum and maximum contents specified in Annex I.

Article 14

Fertiliser requirements

A type of fertiliser may only be included in Annex I if:

(a) it provides nutrients in an effective manner;

(b) relevant sampling, analysis, and if required, test methods are being provided.

(c) under normal conditions of use it does not adversely affect human, animal, or plant health, or the environment.

Article 15

Safeguard clause

1. Where a Member State has justifiable grounds for believing that a specific EC fertiliser, although satisfying the requirements of this Regulation, constitutes a risk to safety or health of humans, animals or plants or a risk to the environment, it may temporarily prohibit the placing on the market of that fertiliser in its territory or make it subject to special conditions. It shall immediately inform the other Member States and the Commission thereof, giving the reasons for its decision.

2. The Commission shall adopt a decision on the matter within 90 days from the receipt of the information in accordance with the procedure referred to in Article 32(2).

3. The provisions of this Regulation shall not preclude the taking of measures by the Commission or by a Member State which are justified on grounds of public security to prohibit, restrict or hinder the placing on the market of EC fertilisers.

TITLE II

PROVISIONS FOR SPECIFIC TYPES OF FERTILISERS

CHAPTER I

Inorganic primary nutrient fertilisers

Article 16

Scope

This chapter shall apply to inorganic primary nutrient fertilisers, solid or fluid, straight or compound, including those containing secondary nutrients and/or micro-nutrients, with the minimum nutrient content established in sections A, B, C, E.2.2 or E.2.3 of Annex I.

Article 17

Declaration of secondary nutrients in primary nutrient fertilisers

Calcium, magnesium, sodium and sulphur content may be declared as secondary nutrient content of EC fertilisers belonging to the types of fertiliser listed in sections A, B and C of Annex I, provided that these elements are present in at least the following minimum quantities:

(a) 2 % calcium oxide (CaO), i.e. 1,4 % Ca;

(b) 2 % of magnesium oxide (MgO), i.e. 1,2 % Mg;

(c) 3 % of sodium oxide (Na2O), i.e. 2,2 % Na;

(d) 5 % of sulphur trioxide (SO3), i.e. 2 % S.

In such a case, the additional marking specified in Article 19(2)(ii) shall be added to the type designation.

Article 18

Calcium, magnesium, sodium and sulphur

1. The declaration of the magnesium, sodium and sulphur content of the fertilisers listed in sections A, B, and C of Annex I shall be expressed in one of the following ways:

(a) the total content expressed as a percentage of the fertiliser by mass;

(b) the total content and the content soluble in water, expressed as a percentage of the fertiliser by mass where the soluble content is at least a quarter of the total content;

(c) where an element is totally soluble in water, only the content soluble in water shall be declared as a percentage of the mass.

2. Unless otherwise stated in Annex I, a declaration of the calcium content shall only be made if it is soluble in water and shall be expressed as a percentage of the fertiliser by mass.

Article 19

Identification

1. In addition to the compulsory identification markings referred to in Article 9(1)(a), the markings set out in paragraphs 2, 3, 4, 5 and 6 of this Article shall be stated.

2. The following shall be stated after the type designation of compound fertilisers:

(i) The chemical symbols of the declared secondary nutrients, between brackets and after the symbols of the primary nutrients.

(ii) Numbers indicating the primary nutrient content. The declared secondary nutrient content shall be indicated between brackets after the primary nutrient content.

3. The fertiliser type designation shall only be followed by figures indicating primary and secondary nutrient content.

4. Where micro-nutrients are declared, the words "with micro-nutrients" or the word "with" followed by the name or names and chemical symbols of the micro-nutrients present shall be given.

5. The declared content of primary nutrients and secondary nutrients shall be given as a percentage by mass, as whole numbers or, where necessary, where an appropriate method of analysis exists, to one decimal place.

In fertilisers containing more than one declared nutrient, the order shall be for primary nutrients: N, P2O5 and/or P, K2O and/or K, and for secondary nutrients: CaO and/or Ca, MgO and/or Mg, Na2O and/or Na, SO3 and/or S.

The declared content of micro-nutrients shall give the name and symbol of each micro-nutrient, indicating the percentage by mass as specified in sections E.2.2 and E.2.3 of Annex I and according to solubility.

6. The forms and solubility of the nutrients shall also be expressed as a percentage by mass of fertiliser, except where Annex I explicitly provides that this content shall be otherwise expressed.

The number of decimal places shall be one, except for micro-nutrients where it shall be as specified in sections E.2.2 and E.2.3 of Annex I.

CHAPTER II

Inorganic secondary nutrient fertilisers

Article 20

Scope

This chapter shall apply to inorganic secondary nutrient fertilisers, solid or fluid, including those containing micro-nutrients, with the minimum nutrient content established in sections D, E.2.2, and E.2.3 of Annex I.

Article 21

Identification

1. In addition to the compulsory identification markings referred to in Article 9(1)(a), the markings set out in paragraphs 2, 3, 4 and 5 of this Article shall be stated.

2. Where micro-nutrients are declared, the words "with micro-nutrients" or the word "with", followed by the name or names and chemical symbols of the micro-nutrients present, shall be given.

3. The declared content of secondary nutrients shall be given as a percentage by mass, as whole numbers or, where necessary, where an appropriate method of analysis exists, to one decimal place.

Where more than one secondary nutrient is present, the order shall be:

CaO and/or Ca, MgO and/or Mg, Na2O and/or Na, SO3 and/or S.

The declared content of micro-nutrients shall give the name and symbol of each micro-nutrient, indicating the percentage by mass as specified in sections E.2.2 and E.2.3 of Annex I and according to solubility.

4. The forms and solubility of the nutrients shall also be expressed as a percentage by mass of fertiliser, except where Annex I explicitly provides that this content shall be otherwise expressed.

The number of decimal places shall be one, except for micro-nutrients where it shall be as specified in sections E.2.2 and E.2.3 of Annex I.

5. Unless otherwise stated in Annex I, a declaration of the calcium content shall only be made if it is soluble in water and shall be expressed as a percentage of the fertiliser by mass.

CHAPTER III

Inorganic micro-nutrient fertilisers

Article 22

Scope

This chapter shall apply to inorganic micro-nutrient fertilisers, solid or fluid, with the minimum nutrient content established in sections E.1 and E.2.1 of Annex I.

Article 23

Identification

1. In addition to the compulsory identification markings referred to in Article 9(1)(a) the markings set out in paragraphs 2, 3, 4 and 5 of this Article shall be stated.

2. Where the fertiliser contains more than one micro-nutrient, the type designation "mixture of micro-nutrients" followed by the names of the micro-nutrients present and their chemical symbols, shall be given.

3. For fertilisers containing only one micro-nutrient (section E.1 of Annex I), the declared micro-nutrient content shall be given as a percentage by mass, in whole numbers or, where necessary, to one decimal place.

4. The forms and solubility of micro-nutrients shall be expressed as a percentage by mass of fertiliser, except where Annex I explicitly provides that this content shall be otherwise expressed.

The number of decimal places for micro-nutrients shall be as specified in section E.2.1 of Annex I.

5. Below the compulsory or optional declarations the following shall be entered on the label and accompanying documents with regard to the products appearing in sections E.1 and E.2.1 of Annex I:

"To be used only where there is a recognised need. Do not exceed the appropriate dose rates."

Article 24

Packaging

EC fertilisers covered by the provisions of this chapter shall be packaged.

CHAPTER IV

Ammonium nitrate fertilisers of high nitrogen content

Article 25

Scope

For the purpose of this chapter, ammonium nitrate fertilisers of high nitrogen content, straight or compound, are ammonium nitrate based products manufactured for use as fertilisers and containing more than 28 % by mass of nitrogen in relation to ammonium nitrate.

This type of fertiliser may contain inorganic or inert substances.

The substances used in the manufacturing of this type of fertiliser must not increase its sensitivity to heat or its tendency to detonate.

Article 26

Safety measures and controls

1. The manufacturer shall ensure that straight ammonium nitrate fertilisers of high nitrogen content comply with the provisions of section 1 of Annex III.

2. The checking, analysis and testing for official controls of straight ammonium nitrate fertilisers of high nitrogen content provided for by this chapter shall be carried out in accordance with the methods described in section 3 of Annex III.

3. To ensure the traceability of ammonium nitrate EC fertilisers of high nitrogen content placed on the market, the manufacturer shall maintain records of the names and addresses of the sites, and of the operators of the sites, at which the fertiliser and its principal components were produced. These records shall be available for inspection by Member States for as long as the fertiliser is being supplied to the market, and for a further period of 2 years after the manufacturer stopped supplying it.

Article 27

Test of resistance to detonation

Without prejudice to the measures referred to in Article 26, the manufacturer shall ensure that each type of EC high nitrogen content ammonium nitrate fertiliser placed on the market has passed the test of resistance to detonation described in sections 2, 3 (method 1, point 3) and 4 of Annex III of this Regulation. This test shall be carried out by one of the approved laboratories referred to in Article 30(1) or 33(1). Manufacturers shall submit the results of the test to the competent authority of the Member State concerned at least 5 days before placing the fertiliser on the market, or at least 5 days before the arrival of the fertiliser at the borders of the European Community in the case of imports. Thereafter, the manufacturer shall continue to guarantee that all supplies of the fertiliser placed on the market are capable of passing the abovementioned test.

Article 28

Packaging

Ammonium nitrate fertilisers of high nitrogen content shall be made available to the final user only in packaged form.

TITLE III

CONFORMITY ASSESSMENT OF FERTILISERS

Article 29

Control measures

1. Member States may subject fertilisers marked "EC fertiliser" to official control measures for the purpose of verifying that they comply with this Regulation.

Member States may charge fees not exceeding the cost of tests needed for such control measures, but this shall not oblige manufacturers to repeat tests or to pay for repeated tests where the first test was made by a laboratory which fulfilled the conditions of Article 30 and where the test showed compliance of the fertiliser in question.

2. Member States shall ensure that sampling and analysis for official controls of EC fertilisers belonging to types of fertilisers listed in Annex I are carried out in accordance with the methods described in Annex III and IV.

3. Compliance with this Regulation in respect of conformity to types of fertiliser and compliance with the declared nutrient content and/or the declared content expressed as forms and solubilities of such nutrients may be verified at official inspections only by means of sampling and analysis methods established in accordance with Annex III and IV and taking into account the tolerances specified in Annex II.

4. The adaptation and modernisation of measuring, sampling and analysis methods shall follow the procedure referred to in Article 32(2), and shall, wherever possible, use European Standards. The same procedure shall apply to the adoption of implementing rules needed to specify the control measures provided for in this Article and in Articles 8, 26 and 27 of this Regulation. Such rules shall in particular address the question of the frequency with which tests need to be repeated, as well as measures that are designed to ensure that the fertiliser put on the market is identical with the fertiliser tested.

Article 30

Laboratories

1. Member States shall notify to the Commission the list of those approved laboratories on their territories that are competent to provide the necessary services for checking compliance of EC fertilisers with the requirements of this Regulation. Such laboratories must meet the standards mentioned in section B of Annex V. Such notification shall be made by 11 June 2004 and on the occasion of each subsequent modification.

2. The Commission shall publish the list of approved laboratories in the Official Journal of the European Union.

3. Where a Member State has justifiable grounds for believing that an approved laboratory does not meet the standards referred to in paragraph 1, it shall raise this matter in the committee referred to in Article 32. If the committee agrees that the laboratory does not meet the standards, the Commission shall remove the name from the list referred to in paragraph 2.

4. The Commission shall adopt a decision on the matter within 90 days from the receipt of the information in accordance with the procedure referred to in Article 32(2).

5. The Commission shall publish the amended list in the Official Journal of the European Union.

TITLE IV

FINAL PROVISIONS

CHAPTER I

Adaptation of the Annexes

Article 31

New EC fertilisers

1. The inclusion of a new type of fertiliser in Annex I of this Regulation shall be adopted in accordance with the procedure referred to in Article 32(2).

2. A manufacturer or its representative which wishes to propose a new type of fertiliser for inclusion in Annex I and is required to compile a technical file for that purpose shall do so by taking into account the technical documents referred to in section A of Annex V.

3. Amendments required to adapt the Annexes to technical progress shall be adopted in accordance with the procedure referred to in Article 32(2).

Article 32

Committee procedure

1. The Commission shall be assisted by a committee.

2. Where reference is made to this paragraph, Articles 5 and 7 of Decision 1999/468/EC shall apply, having regard to the provisions of Article 8 thereof.

The period laid down in Article 5(6) of Decision 1999/468/EC shall be set at three months.

3. The committee shall adopt its rules of procedure.

CHAPTER II

Transitional provisions

Article 33

Competent laboratories

1. Without prejudice to the provisions of Article 30(1), Member States may for a transitional period until 11 December 2007 continue to apply their national provisions for authorising competent laboratories to provide the necessary services for checking compliance of EC fertilisers with the requirements of this Regulation.

2. Member States shall notify the list of these laboratories to the Commission, giving details of their authorisation scheme. Such notification shall be made by 11 June 2004 and on the occasion of each subsequent modification.

Article 34

Packaging and labelling

Notwithstanding Article 35(1), EC fertiliser markings, packagings, labels and accompanying documents provided for by earlier Directives may continue to be used until 11 June 2005.

CHAPTER III

Final provisions

Article 35

Repealed Directives

1. Directives 76/116/EEC, 77/535/EEC, 80/876/EEC and 87/94/EEC are hereby repealed.

2. References to the Directives repealed shall be construed as references to this Regulation. In particular, derogations from Article 7 of Directive 76/116/EEC that were granted by the Commission under Article 95(6) of the Treaty shall be construed as derogations from Article 5 of the present Regulation and shall continue to produce their effects notwithstanding the entry into force of this Regulation. Pending the adoption of penalties under Article 36, Member States may continue to apply penalties for infringements of national rules implementing the Directives mentioned in paragraph 1.

Article 36

Penalties

The Member States shall lay down the rules on penalties applicable to infringements of the provisions of this Regulation and shall take all measures necessary to ensure that they are implemented. The penalties provided for must be effective, proportionate and dissuasive.

Article 37

National provisions

The Member States shall notify the Commission by 11 June 2005 of any national provisions adopted pursuant to Articles 6(1), 6(2), 29(1) and 36 of this Regulation, and shall notify it without delay of any subsequent amendment affecting them.

Article 38

Entry into force

This Regulation shall enter into force on the twentieth day after its publication in the Official Journal of the European Union with the exception of Articles 8 and 26(3), which shall enter into force 11 June 2005.

This Regulation shall be binding in its entirety and directly applicable in all Member States.

Done at Luxembourg, 13 October 2003.

For the European Parliament

The President

P. Cox

For the Council

The President

G. Alemanno

(1) OJ C 51 E, 26.2.2002, p. 1 and OJ C 227 E, 24.9.2002, p. 503.

(2) OJ C 80, 3.4.2002, p. 6.

(3) Opinion of the European Parliament of 10 April 2002 (OJ C 127 E, 29.5.2002, p. 160), Council Common Position of 14 April 2003 (OJ C 153 E, 1.7.2003, p. 56) and Decision of the European Parliament of 2 September 2003 (not yet published in the Official Journal).

(4) OJ L 24, 30.1.1976, p. 21. Directive as last amended by Directive 98/97/EC of the European Parliament and the Council (OJ L 18, 23.1.1999, p. 60).

(5) OJ L 250, 23.9.1980, p. 7. Directive as amended by Directive 97/63/EC of the European Parliament and the Council (OJ L 335, 6.12.1997, p. 15).

(6) OJ L 38, 7.2.1987, p. 1. Directive as amended by Directive 88/126/EEC (OJ L 63, 9.3.1988, p. 12).

(7) OJ L 213, 22.8.1977, p. 1. Directive as last amended by Directive 95/8/EC (OJ L 86, 20.4.1995, p. 41).

(8) OJ L 184, 17.7.1999, p. 23.

TABLE OF CONTENTS

>TABLE>

ANNEX I

LIST OF TYPES OF EC FERTILISERS

A. Inorganic straight primary nutrient fertilisers

A.1. Nitrogenous fertilisers

>TABLE>

A.2. Phosphatic fertilisers

Where a particle size criterion is prescribed for the basic constituent materials of fertilisers sold in granular form (fertilisers 1, 3, 4, 5, 6 and 7), it will be established by an appropriate analytical method.

>TABLE>

A.3. Potassic fertilisers

>TABLE>

B. Inorganic compound primary nutrient fertilisers

B.1. NPK fertilisers

>TABLE>

>TABLE>

>TABLE>

>TABLE>

B.2. NP fertilisers

>TABLE>

>TABLE>

>TABLE>

>TABLE>

B.3. NK fertilisers

>TABLE>

>TABLE>

>TABLE>

>TABLE>

B.4. PK fertilisers

>TABLE>

>TABLE>

C. Inorganic fluid fertilisers

C.1. Straight fluid fertilisers

>TABLE>

C.2. Compound fluid fertilisers

>TABLE>

>TABLE>

>TABLE>

>TABLE>

>TABLE>

>TABLE>

>TABLE>

>TABLE>

>TABLE>

>TABLE>

>TABLE>

>TABLE>

>TABLE>

>TABLE>

>TABLE>

>TABLE>

D. Inorganic secondary nutrient fertilisers

>TABLE>

E. Inorganic micro-nutrient fertilisers

Explanatory note:

The following notes are applicable to the whole of Part E.

Note 1:

A chelating agent may be designated by means of its initials as set out in E.3.

Note 2:

If the product leaves no solid residue after being dissolved in water it may be described as "for dissolution".

Note 3:

Where a micro-nutrient is present in a chelated form, the pH range guaranteeing acceptable stability of the chelated fraction shall be stated.

E.1. Fertilisers containing only one micro-nutrient

E.1.1. Boron

>TABLE>

E.1.2. Cobalt

>TABLE>

E.1.3. Copper

>TABLE>

E.1.4. Iron

>TABLE>

E.1.5. Manganese

>TABLE>

E.1.6. Molybdenum

>TABLE>

E.1.7. Zinc

>TABLE>

E.2. Minimum micro-nutrient content, percentage weight of fertilisers

E.2.1. Solid or fluid mixtures of micro-nutrient

>TABLE>

Minimum total of micro-nutrient in a solid mixture: 5 % by mass of the fertiliser.

Minimum total of micro-nutrient in a fluid mixture: 2 % by mass of the fertiliser.

E.2.2. EC fertilisers containing primary and/or secondary nutrient with micro-nutrient applied to the soil

>TABLE>

E.2.3. EC fertilisers containing primary and/or secondary nutrient with micro-nutrients for leaf sprays

>TABLE>

E.3. List of authorised organic chelating and complexing agents for micro-nutrients

The following products are authorised provided they have complied with the requirements of Directive 67/548/EEC(1) as amended.

E.3.1. Chelating agents(2)

Sodium, potassium or ammonium acid or salts of:

>TABLE>

E.3.2. Complexing agents:

List to be drawn up.

(1) OJ L 196, 16.8.1967, p. 1.

(2) The chelating agents are to be identified and quantified by European Standard EN 13368 part 1 and part 2, to the extent that this standard covers the above agents.

ANNEX II

TOLERANCES

The tolerances given in this Annex are negative values in percentage by mass.

The tolerance allowed in respect of the declared nutrient contents in the various types of EC fertiliser are as follows:

1. Inorganic straight primary nutrient fertilisers absolute value in percentage by mass expressed as N, P2O5, K2O, MgO, Cl

1.1. Nitrogenous fertilisers

>TABLE>

1.2. Phosphatic fertilisers

>TABLE>

Other phosphatic fertilisers

>TABLE>

1.3. Potassic fertilisers

>TABLE>

1.4. Other components

>TABLE>

2. Inorganic compound primary nutrient fertilisers

2.1. Nutrient elements

>TABLE>

2.2. Total negative deviations from the declared value

>TABLE>

3. Secondary nutrients in fertilisers

The tolerances allowed in respect of the declared calcium, magnesium, sodium and sulphur contents shall be a quarter of the declared contents of these nutrients up to a maximum of 0,9 % in absolute terms for CaO, MgO, Na2O, and SO3, i.e. 0,64 for Ca, 0,55 for Mg, 0,67 for Na and 0,36 for S.

4. Micro-nutrients in fertilisers

The tolerance allowed in respect of the declared micro-nutrient content shall be:

- 0,4 % in absolute terms for a content of more than 2 %,

- one fifth of the declared value for a content not exceeding 2 %.

The tolerance allowed in respect of the declared content for the various forms of nitrogen or the declared solubilities of phosphorus pentoxide is one-tenth of the overall content of the nutrient concerned with a maximum of 2 % by mass, provided that the overall content of that nutrient remains within the limits specified in Annex I and the tolerances specified above.

ANNEX III

TECHNICAL PROVISIONS FOR AMMONIUM NITRATE FERTILISERS OF HIGH NITROGEN CONTENT

1. Characteristics of and limits for straight ammonium nitrate fertilisers of high nitrogen content

1.1. Porosity (oil retention)

The oil retention of the fertiliser, which must first have undergone two thermal cycles of a temperature ranging from 25 to 50 °C and conforming with the provisions of part 2 of section 3. of this Annex, must not exceed 4 % by mass.

1.2. Combustible ingredients

The percentage by mass of combustible material measured as carbon must not exceed 0,2 % for fertilisers having a nitrogen content of at least 31,5 % by mass and must not exceed 0,4 % for fertilisers having a nitrogen content of at least 28 % but less than 31,5 % by mass.

1.3. pH

A solution of 10 g of fertiliser in 100 ml of water must have a pH of at least 4.5.

1.4. Particle size analysis

Not more than 5 % by mass of the fertiliser must pass through a 1 mm mesh sieve and not more than 3 % by mass must pass through a 0,5 mm mesh sieve.

1.5. Chlorine

The maximum chlorine content is set at 0,02 % by mass.

1.6. Heavy metals

Heavy metals should not be added deliberately, and any traces which are incidental to the production process should not exceed the limit fixed by the Committee.

The copper content shall not be higher than 10 mg/kg.

No limits are specified for other heavy metals.

2. Description of the test of resistance to detonation concerning ammonium nitrate fertilisers of high nitrogen content

The test must be carried out on a representative sample of fertiliser. Before being tested for resistance to detonation, the whole mass of the sample is to be thermally cycled five times complying with the provisions of part 3 in section 3. of this Annex.

The fertiliser must be subjected to the test of resistance to detonation in a horizontal steel tube under the following conditions:

- seamless steel tube,

- Tube length: 1000 mm at least,

- Nominal external diameter: 114 mm at least,

- Nominal wall thickness: 5 mm at least,

- Booster: the type and mass of the booster chosen should be such as to maximise the detonation pressure applied to the sample in order to determine its susceptibility to the transmission of detonation,

- Test temperature: 15-25 °C,

- Witness lead cylinders for detecting detonation: 50 mm diameter and 100 mm high

- placed at 150 mm intervals and supporting the tube horizontally. The test is to be carried out twice. The test is deemed conclusive if in both tests one or more of the supporting lead cylinders is crushed by less than 5 %.

3. Methods of checking compliance with the limits specified in Annexes III-1 and III-2

Method 1 Methods for the application of thermal cycles

1. Scope and field of application

This document defines the procedures for the application of thermal cycles prior to the execution of the oil retention test for straight ammonium nitrate fertilisers of high nitrogen content and of the test on the resistance to detonation for both, straight and compound ammonium nitrate fertiliser of high nitrogen content.

The methods of the closed thermal cycles as described in this section are regarded as simulating sufficiently the conditions to be taken into account within the scope of application of title II, chapter IV, however, these methods may not necessarily simulate all conditions arising during transport and storage;

2. Thermal cycles referred to in Annex III-1

2.1. Field of application

This procedure is for thermal cycling prior to determining the oil retention of the fertiliser.

2.2. Principle and definition

In an Erlenmeyer flask, heat the sample from ambient temperature to 50 °C and maintain at this temperature for a period of two hours (phase at 50 °C). Thereupon cool the sample until a temperature of 25 °C is achieved and maintain at that temperature for two hours (phase at 25 °C). The combination of the successive phases at 50 °C and 25 °C forms one thermal cycle. After being subjected to two thermal cycles, the test sample is held at a temperature of 20 ±3 °C for the determination of the oil retention value.

2.3. Apparatus

Normal laboratory apparatus, in particular:

- water baths thermostated at 25 (± 1) and 50 (± 1) °C respectively,

- Erlenmeyer flasks with an individual capacity of 150 ml.

2.4. Procedure

Put each test sample of 70 (± 5) grams into an Erlenmeyer flask which is then sealed with a stopper.

Move each flask every two hours from the 50 °C bath to the 25 °C bath and vice versa.

Maintain the water in each bath at constant temperature and keep in motion by rapid stirring to ensure the water level comes above the level of the sample. Protect the stopper from condensation by a foam rubber cap.

3. Thermal cycles to be used for Annex III-2

3.1. Field of application

This procedure is for thermal cycling prior to the execution of the detonability test.

3.2. Principle and definition

In a watertight box heat the sample from ambient temperature to 50 °C and maintain at this temperature for a period of one hour (phase at 50 °C). Thereupon cool the sample until a temperature of 25 °C is achieved and maintain at that temperature for one hour (phase at 25 °C). The combination of the successive phases at 50 °C and 25 °C forms one thermal cycle. After being subjected to the required number of thermal cycles, the test sample is held at a temperature of 20 ±3 °C pending the execution of the detonability test.

3.3. Apparatus

- A water bath, thermostated in a temperature range of 20 to 51 °C with a minimum heating and cooling rate of 10 °C/h, or two water baths, one thermostated at a temperature of 20 °C, the other at 51 °C. The water in the bath(s) is continuously stirred; the volume of the bath should be large enough to guarantee ample circulation of the water.

- A stainless steel box, watertight all around and provided with a thermocouple in the centre. The outside width of the box is 45 (± 2) mm and the wall thickness is 1,5 mm (see Figure 1). The height and length of the box can be chosen to suit the dimensions of the water bath, e.g. length 600 mm, height 400 mm.

3.4. Procedure

Place a quantity of fertilisers sufficient for a single detonation into the box and close the cover. Place the box in the water bath. Heat the water to 51 °C and measure the temperature in the centre of the fertiliser. One hour after the temperature at the centre has reached 50 °C cool the water. One hour after the temperature at the centre has reached 25 °C heat the water to start the second cycle. In the case of two water baths, transfer the box to the other bath after each heating/cooling period.

Figure 1

>PIC FILE= "L_2003304EN.005501.TIF">

Method 2 Determination of oil retention

1. Scope and field of application

This document defines the procedure for the determination of oil retention of straight ammonium nitrate fertilisers of high nitrogen content.

The method is applicable to both prilled and granular fertilisers which do not contain oil-soluble materials.

2. Definition

Oil retention of a fertiliser: the quantity of oil retained by the fertiliser determined under the operating conditions specified, and expressed as a percentage by mass.

3. Principle

Total immersion of the test portion in gas oil for a specified period, followed by the draining away of surplus oil under specified conditions. Measurement of the increase in mass of the test portion.

4. Reagent

Gas oil

Viscosity max.: 5 mPas at 40 °C

Density: 0,8 to 0,85 g/ml at 20 °C

Sulphur content: <= 1,0 % (m/m)

Ash: <= 0,1 % (m/m)

5. Apparatus

Ordinary laboratory apparatus, and:

5.1. Balance, capable of weighing to the nearest 0,01 gram.

5.2. Beakers, of capacity 500 ml.

5.3. Funnel, of plastic materials, preferably with a cylindrical wall at the upper end, diameter approximately 200 mm.

5.4. Test sieve, aperture 0,5 mm, fitting into the funnel (5.3).

Note:

The size of the funnel and sieve is such as to ensure that only a few granules lie one above another and the oil is able to drain easily.

5.5. Filter paper, rapid filtering grade, creped, soft, mass 150 g/m2.

5.6. Absorbent tissue (laboratory grade).

6. Procedure

6.1. Two individual determinations are carried out in quick succession on separate portions of the same test sample.

6.2. Remove particles smaller than 0,5 mm using the test sieve (5.4). Weigh to the nearest 0,01 gram approximately 50 grams of the sample into the beaker (5.2). Add sufficient gas oil (section 4) to cover the prills completely and stir carefully to ensure that the surfaces of all the prills are fully wetted. Cover the beaker with a watch glass and leave to stand for one hour at 25 (± 2) °C.

6.3. Filter the entire contents of the beaker through the funnel (5.3) containing the test sieve (5.4). Allow the portion retained by the sieve to remain there for one hour so that most of the excess oil can drain away.

6.4. Lay two sheets of filter paper (5.5) (about 500 × 500 mm) on top of each other on a smooth surface; fold the four edges of both filter papers upwards to a width of about 40 mm to prevent the prills from rolling away. Place two layers of absorbent tissue (5.6) in the centre of the filter papers. Pour the entire contents of the sieve (5.4) over the absorbent tissues and spread the prills evenly with a soft, flat brush. After two minutes lift one side of the tissues to transfer the prills to the filter papers beneath and spread them evenly over these with the brush. Lay another sheet of filter paper, similarly with its edges turned upward, on the sample and roll the prills between the filter papers with circular movements while exerting a little pressure. Pause after every eight circular movements to lift the opposite edges of the filter papers and return to the centre the prills that have rolled to the periphery. Keep to the following procedure: make four complete circular movements, first clockwise and then anticlockwise. Then roll the prills back to the centre as described above. This procedure to be carried out three times (24 circular movements, edges lifted twice). Carefully insert a new sheet of filter paper between the bottom sheet and the one above it and allow the prills to roll onto the new sheet by lifting the edges of the upper sheet. Cover the prills with a new sheet of filter paper and repeat the same procedure as described above. Immediately after rolling, pour the prills into a tared dish and reweigh to the nearest 0,01 gram to determine the mass of the quantity of gas oil retained.

6.5. Repeating the rolling procedure and reweighing

If the quantity of gas oil retained in the portion is found to be greater than 2 grams, place the portion on a fresh set of filter papers and repeat the rolling procedure, lifting the corners in accordance with section 6.4 (two times eight circular movements, lifting once). Then reweigh the portion.

7. Expression of the results

7.1. Method of calculation and formula

The oil retention, from each determination (6.1) expressed as a percentage by mass of the sieved test portion, is given by the equation:

>REFERENCE TO A GRAPHIC>

where:

m1 is the mass, in grams, of the sieved test portion (6.2),

m2 is the mass, in grams, of the test portion according to section 6.4 or 6.5 respectively as the result of the last weighing.

Take as the result the arithmetic mean of the two individual determinations.

Method 3 Determination of the combustible ingredients

1. Scope and field of application

This document defines the procedure for the determination of the combustible content of straight ammonium nitrate fertilisers of high nitrogen content.

2. Principle

The carbon dioxide produced by inorganic fillers is removed in advance with an acid. The organic compounds are oxidised by means of a chromic acid/sulphuric acid mixture. Carbon dioxide formed is absorbed in a barium hydroxide solution. The precipitate is dissolved in a solution of hydrochloric acid and measured by back-titration with sodium hydroxide solution.

3. Reagents

3.1. Analytical-grade chromium (VI) trioxide Cr2O3;

3.2. Sulphuric acid, 60 % by volume: pour 360 ml of water into a one-litre beaker and carefully add 640 ml of sulphuric acid (density at 20 °C = 1.83 g/ml).

3.3. Silver nitrate: 0,1 mol/l solution.

3.4. Barium hydroxide

Weigh out 15 grams of barium hydroxide [Ba(OH)2. 8H2O], and dissolve completely in hot water. Allow to cool and transfer to a one-litre flask. Fill up to the mark and mix. Filter through a pleated filter paper.

3.5. Hydrochloric acid: 0,1 mol/l standard solution.

3.6. Sodium hydroxide: 0,1 mol/l standard solution.

3.7. Bromophenol blue: solution of 0,4 grams per litre in water.

3.8. Phenolphthalein: solution of 2 grams per litre in 60 % by volume ethanol.

3.9. Soda lime: particle dimensions, about 1,0 to 1,5 mm.

3.10. Demineralised water, freshly boiled to remove carbon dioxide.

4. Apparatus

4.1. Standard laboratory equipment, in particular:

- filter crucible with a plate of sintered glass and a capacity of 15 ml; plate diameter: 20 mm; total height: 50 mm; porosity 4 (pore diameter from 5 to 15 µm),

- 600-ml beaker.

4.2. Compressed nitrogen supply.

4.3. Apparatus made up of the following parts and assembled, if possible, by means of spherical ground joints (see Figure 2).

4.3.1. Absorption tube A about 200 mm long and 30 mm in diameter filled with soda lime (3.9) kept in place by fibreglass plugs.

4.3.2. 500-ml reaction flask B with side arm and a round bottom.

4.3.3. Vigreux fractionating column about 150 mm long (C').

4.3.4. Double-surface condenser C, 200 mm long.

4.3.5. Drechsel bottle D acting as a trap for any excess acid which may distil over.

4.3.6. Ice bath E to cool the Drechsel bottle.

4.3.7. Two absorption vessels F1 and F2, 32 to 35 mm in diameter, the gas distributor of which comprises a 10 mm disc of low-porosity sintered glass.

4.3.8. Suction pump and suction regulating device G comprising a T-shaped glass piece inserted into the circuit, the free arm of which is connected to the fine capillary tube by a short rubber tube fitted with a screw clamp.

Caution:

The use of boiling chromic acid solution in an apparatus under reduced pressure is a hazardous operation and requires appropriate precautions.

5. Procedure

5.1. Sample for analysis

Weigh approximately 10 grams of ammonium nitrate to the nearest 0,001 grams.

5.2. Removal of carbonates

Place the sample for analysis in the reaction flask B. Add 100 ml of H2SO4(3.2). The prills dissolve in about 10 minutes at ambient temperature. Assemble the apparatus as indicated in the diagram: connect one end of the absorption tube (A) to the nitrogen source (4.2) via a non-return flow device containing a pressure equivalent to 5 to 6 mm of mercury and the other end to the feed tube which enters the reaction flask. Place the Vigreux fractionating column (C') and the condenser (C) with cooling water supply in position. Adjust the nitrogen to provide a moderate flow through the solution, bring the solution to boiling point and heat for two minutes. At the end of this time there should be no more effervescence. If effervescence is seen, continue heating for 30 minutes. Allow solution to cool for at least 20 minutes with the nitrogen flowing through it.

Complete assembly of the apparatus as indicated in the diagram by connecting the condenser tube to the Drechsel bottle (D) and the bottle to the absorption vessels F1 and F2. The nitrogen must continue to pass through the solution during the assembly operation. Rapidly introduce 50 ml of barium hydroxide solution (3.4) into each of the absorption vessels (F1 and F2).

Bubble a stream of nitrogen through for about 10 minutes. The solution must remain clear in the absorbers. If this does not happen, the carbonate removal process must be repeated.

5.3. Oxidation and absorption

After withdrawing the nitrogen feed tube, rapidly introduce 20 grams of chromium trioxide (3.1) and 6 ml of silver nitrate solution (3.3) via the side arm of the reaction flask (B). Connect the apparatus to the suction pump and adjust the nitrogen flow so that a steady stream of gas bubbles passes through the sintered-glass absorbers F1 and F2.

Heat the reaction flask (B) until the liquid boils and keep it boiling for one and a half hours(1). It may be necessary to adjust the suction-regulating valve (G) to control the nitrogen flow since it is possible that the barium carbonate precipitated during the test may block the sintered-glass discs. The operation is satisfactory when the barium hydroxide solution in the absorber F2 remains clear. Otherwise repeat the test. Stop heating and dismantle the apparatus. Wash each of the distributors (3.10) both inside and outside to remove barium hydroxide and collect the washings in the corresponding absorber. Place the distributors one after the other in a 600-ml beaker which will subsequently be used for the determination.

Rapidly filter under vacuum firstly the contents of absorber F2 and then of absorber F1 using the sintered-glass crucible. Collect the precipitate by rinsing the absorbers with water (3.10) and wash the crucible with 50 ml of the same water. Place the crucible in the 600-ml beaker and add about 100 ml of boiled water (3.10). Introduce 50 ml of boiled water into each of the absorbers and pass nitrogen through the distributors for five minutes. Combine the water with that from the beaker. Repeat the operation once to ensure that the distributors are rinsed thoroughly.

5.4. Measurement of the carbonates originating from organic material

Add five drops of phenolphthalein (3.8) to the contents of the beaker. The solution becomes red in colour. Add hydrochloric acid (3.5) drop by drop until the pink colour just disappears. Stir the solution well in the crucible to check that the pink colour does not reappear. Add five drops of bromphenol blue (3.7) and titrate with hydrochloric acid (3.5) until the solution turns yellow. Add a further 10 ml of hydrochloric acid.

Heat the solution to boiling point and continue boiling for a maximum of one minute. Check carefully that no precipitate remains in the liquid.

Allow to cool and back titrate with the sodium hydroxide solution (3.6).

6. Blank test

Carry out a blank test following the same procedure and using the same quantities of all reagents.

7. Expression of the results

The content of combustible ingredients (C), expressed as carbon, as a percentage by mass of the sample, is given by the formula:

>REFERENCE TO A GRAPHIC>

where:

E= the mass in grams of the test portion,

V1= the total volume in ml of 0,1 mol/l hydrochloric acid added after the change in colour of the phenolphthalein,

V2= the volume in ml of the 0,1 mol/l sodium hydroxide solution used for back titration.

Figure 2

>PIC FILE= "L_2003304EN.006001.TIF">

Method 4 Determination of the pH value

1. Scope and field of application

This document defines the procedure for measuring the pH value of a solution of a straight ammonium nitrate fertiliser of high nitrogen content.

2. Principle

Measurement of the pH of an ammonium nitrate solution by means of a pH meter.

3. Reagents

Distilled or demineralised water, free from carbon dioxide.

3.1. Buffer solution, pH 6,88 at 20 °C

Dissolve 3,40 ± 0,01 grams of potassium dihydrogen orthophosphate (KH2PO4) in approximately 400 ml of water. Then dissolve 3,55 ± 0,01 grams of disodium hydrogen orthophosphate (Na2HPO4) in approximately 400 ml of water. Transfer the two solutions without loss into a 1000-ml graduated flask, make up to the mark and mix. Keep this solution in an airtight vessel.

3.2. Buffer solution, pH 4,00 at 20 °C

Dissolve 10,21 ± 0,01 grams of potassium hydrogen phthalate (KHC8O4H4) in water, transfer without loss into a 1000-ml graduated flask, make up to the mark and mix.

Keep this solution in an airtight vessel.

3.3. Commercially available pH standard solutions may be used.

4. Apparatus

pH meter, equipped with glass and calomel electrodes or equivalent, sensitivity 0,05 pH unit.

5. Procedure

5.1. Calibration of the pH meter

Calibrate the pH meter (4) at a temperature of 20 (± 1) °C, using the buffer solutions (3.1), (3.2) or (3.3). Pass a slow stream of nitrogen onto the surface of the solution and maintain this throughout the test.

5.2. Determination

Pour 100,0 ml of water onto 10 (± 0,01) grams of the sample in a 250 ml beaker. Remove the insolubles by filtering, decanting or centrifuging the liquid. Measure the pH value of the clear solution at a temperature of 20 (± 1) °C according to the same procedure as for the calibration of the meter.

6. Expression of the results

Express the result in pH units, to the nearest 0,1 unit, and state the temperature used.

Method 5 Determination of the particle size

1. Scope and field of application

This document defines the procedure for the test sieving of straight ammonium nitrate fertilisers of high nitrogen content.

2. Principle

The test sample is sieved on a nest of three sieves, either by hand or by mechanical means. The mass retained on each sieve is recorded and the percentage of material passing the required sieves are calculated.

3. Apparatus

3.1. 200-mm-diameter woven-wire test sieves with apertures of 2,0 mm, 1,0 mm and 0,5 mm respectively of standard ranges. One lid and one receiver for these sieves.

3.2. Balance to weigh to 0,1 gram.

3.3. Mechanical sieve shaker (if available) capable of imparting both vertical and horizontal motion to the test sample.

4. Procedure

4.1. The sample is divided representatively into portions of approximately 100 grams.

4.2. Weigh one of these portions to the nearest 0,1 gram.

4.3. Arrange the nest of sieves in ascending order; receiver, 0,5 mm, 1 mm, 2 mm and place the weighed test portion on the top sieve. Fit the lid to the top of the nest of sieves.

4.4. Shake by hand or machine, imparting both a vertical and horizontal motion and if by hand, tapping occasionally. Continue this process for 10 minutes or until the quantity passing through each sieve in one minute is less than 0,1 gram.

4.5. Remove the sieves from the nest in turn and collect the material retained, brush gently from the reverse side with a soft brush, if necessary.

4.6. Weigh the material retained on each sieve and that collected in the receiver, to the nearest 0,1 gram.

5. Evaluation of the results

5.1. Convert the fraction masses to a percentage of the total of the fraction masses (not of the original charge).

Calculate the percentage in the receiver (i.e. < 0,5 mm): A %

Calculate the percentage retained on the 0,5 mm sieve: B %

Calculate the percentage passing 1,0 mm, i.e. (A + B) %

The sum of the fraction masses should be within 2 % of the initial mass taken.

5.2. At least two separate analyses should be carried out and the individual results for A should not differ by more than 1,0 % absolute and for B by more than 1,5 % absolute. Repeat the test if this is not the case.

6. Expression of the results

Report the mean of the two values obtained for A on the one hand and for A + B on the other.

Method 6 Determination of the chlorine content (as chloride ion)

1. Scope and field of application

This document defines the procedure for the determination of the chlorine content (as chloride ion) of straight ammonium nitrate fertilisers with a high nitrogen content.

2. Principle

Chloride ions dissolved in water are determined by potentiometric titration with silver nitrate in an acidic medium.

3. Reagents

Distilled or demineralised water, free from chloride ions.

3.1. Acetone AR.

3.2. Concentrated nitric acid (density at 20 °C = 1,40 g/ml)

3.3. Silver nitrate 0,1 mol/l standard solution. Store this solution in a brown glass bottle.

3.4. Silver nitrate 0,004 mol/l standard solution - prepare this solution at the time of use.

3.5. Potassium chloride 0,1 mol/l standard reference solution. Weigh, to the nearest 0,1 mg, 3,7276 grams of analytical-grade potassium chloride, previously dried for one hour in an oven at 130 °C and cooled in a desiccator to ambient temperature. Dissolve in a little water, transfer the solution without loss into a 500-ml standard flask, dilute to the mark and mix.

3.6. Potassium chloride, 0,004 mol/l standard reference solution - prepare this solution at the time of use.

4. Apparatus

4.1. Potentiometer with silver indicating electrode and calomel reference electrode, sensitivity 2 mV, covering the range - 500 to + 500 mV.

4.2. Bridge, containing a saturated potassium nitrate solution, connected to the calomel electrode (4.1), fitted at the ends with porous plugs.

4.3. Magnetic stirrer, with a Teflon-coated rod.

4.4. Microburette with fine-pointed tip, graduated in 0,01 ml divisions.

5. Procedure

5.1. Standardisation of the silver nitrate solution

Take 5,00 ml and 10,00 ml of the standard reference potassium chloride solution (3.6) and place in two low-form beakers of convenient capacity (for example 250 ml). Carry out the following titration of the contents of each beaker.

Add 5 ml of the nitric acid solution (3.2), 120 ml of the acetone (3.1) and sufficient water to bring the total volume to about 150 ml. Place the rod of the magnetic stirrer (4.3) in the beaker and set the stirrer in motion. Immerse the silver electrode (4.1) and the free end of the bridge (4.2) in the solution. Connect the electrodes to the potentiometer (4.1) and, after verifying the zero of the apparatus, note the value of the starting potential.

Titrate, using the microburette (4.4), adding initially 4 or 9 ml respectively of the silver nitrate solution corresponding to the standard reference potassium chloride solution used. Continue the addition in 0,1 ml portions for the 0,004 mol/l solutions and in 0,05 ml portions for the 0,1 mol/l solutions. After each addition, await the stabilisation of the potential.

Record the volumes added and the corresponding values of the potential in the first two columns of a table.

In a third column of the table, record the successive increments (Ä1E) of the potential E. In a fourth column, record the differences (Ä2E) positive or negative, between the potential increments (Ä1E). The end of the titration corresponds to the addition of the 0,1 or 0,05 ml portion (V1) of the silver nitrate solution which gives the maximum value of Ä1E.

In order to calculate the exact volume (Veq) of the silver nitrate solution corresponding to the end of the reaction, use the formula:

>REFERENCE TO A GRAPHIC>

where:

V0 is the total volume, in ml, of the silver nitrate solution immediately lower than the volume which gives the maximum increment of Δ1E,

V1 is the volume, in ml, of the last portion of the silver nitrate solution added (0,1 or 0,05 ml),

b is the last positive value of Δ2E,

B is the sum of the absolute values of the last positive values of Δ2E and the first negative value of Δ2E (see example in Table 1).

5.2. Blank test

Carry out a blank test and take account thereof when calculating the final result.

The result V4 of the blank test on the reagents is given, in ml, by the formula:

>REFERENCE TO A GRAPHIC>

where:

V2 is the value, in ml, of the exact volume (Veq) of the silver nitrate solution corresponding to the titration of 10 ml of the potassium chloride standard reference solution used,

V3 is the value, in ml, of the exact volume (Veq) of the silver nitrate solution corresponding to the titration of 5 ml of the potassium chloride standard reference solution used.

5.3. Check test

The blank test can at the same time serve as a check that the apparatus is functioning satisfactorily and that the test procedure is being implemented correctly.

5.4. Determination

Take a portion of sample in the range 10 to 20 grams and weigh to the nearest 0,01 gram. Transfer quantitatively to a 250-ml beaker. Add 20 ml of water, 5 ml of nitric acid solution (3.2), 120 ml of acetone (3.1) and sufficient water to bring the total volume to about 150 ml.

Place the rod of the magnetic stirrer (4.3) in the beaker, place the beaker on the stirrer and set the stirrer in motion. Immerse the silver electrode (4.1) and the free end of the bridge (4.2) in the solution, connect the electrodes to the potentiometer (4.1) and, after having verified the zero of the apparatus, note the value of the starting potential.

Titrate with the silver nitrate solution, by additions from the microburette (4.4) in increments of 0,1 ml. After each addition, await the stabilisation of the potential.

Continue the titration as specified in 5.1, starting from the fourth paragraph: "Record the volumes added and the corresponding values of the potential in the first two columns of a table ...".

6. Expression of the results

Express the result of the analysis as the percentage of chlorine contained in the sample as received for analysis. Calculate the percentage of chlorine (Cl) content from the formula:

>REFERENCE TO A GRAPHIC>

where:

T is the concentration of silver nitrate solution used, in mol/l

V4 is the result, in ml, of the blank test (5.2),

V5 is the value, in ml, of Veq corresponding to the determination (5.4),

m is the mass, in grams, of the test portion.

Table 1: Example

>TABLE>

Method 7 Determination of copper

1. Scope and field of application

This document defines the procedure for the determination of copper content of straight ammonium nitrate fertilisers of high nitrogen content.

2. Principle

The sample is dissolved in dilute hydrochloric acid and the copper is determined by atomic absorption spectrophotometry.

3. Reagents

3.1. Hydrochloric acid (density at 20 °C = 1,18 g/ml).

3.2. Hydrochloric acid, 6 mol/l solution.

3.3. Hydrochloric acid 0,5 mol/l solution.

3.4. Ammonium nitrate.

3.5. Hydrogen peroxide, 30 % w/v

3.6. Copper solution(2) (stock): weigh, to the nearest 0,001 gram, 1 gram of pure copper, dissolve in 25 ml 6 mol/l hydrochloric acid solution (3.2), add 5 ml of hydrogen peroxide (3.5) in portions and dilute to 1 litre with water. 1 ml of this solution contains 1000 µg of copper (Cu).

3.6.1. Copper solution (dilute): dilute 10 ml of stock solution (3.6) to 100 ml with water and then dilute 10 ml of the resulting solution, to 100 ml with water, 1 ml of the final dilution contains 10 µg of copper (Cu).

Prepare this solution at the time of use.

4. Apparatus

Atomic absorption spectrophotometer with a copper lamp (324,8 nm).

5. Procedure

5.1. Preparation of the solution for analysis

Weigh, to the nearest 0,001 gram, 25 grams of the sample, place it in a 400-ml beaker, add carefully 20 ml of hydrochloric acid (3.1) (there may be a vigorous reaction due to carbon dioxide formation). Add more hydrochloric acid, if necessary. When effervescence has stopped, evaporate to dryness on a steam bath, stirring occasionally with a glass rod. Add 15 ml 6 mol/l hydrochloric acid solution (3.2) and 120 ml of water. Stir with the glass rod, which should be left in the beaker, and cover the beaker with a watch glass. Boil the solution gently until dissolution is complete and then cool.

Transfer the solution quantitatively into a 250-ml graduated flask, by washing the beaker with 5 ml 6 mol/l hydrochloric acid (3.2), and twice with 5 ml of boiling water, make up to the mark with 0,5 mol/l hydrochloric acid (3.3) and mix carefully.

Filter through a copper-free filter paper(3), discarding the first 50 ml.

5.2. Blank solution

Prepare a blank solution from which only the sample has been omitted and allow for this in the calculation of the final results.

5.3. Determination

5.3.1. Preparation of sample and blank test solutions

Dilute the sample solution (5.1) and the blank test solution (5.2) with 0,5 mol/l hydrochloric acid solution (3.3) to a concentration of copper within the optimal measuring range of the spectrophotometer. Normally no dilution is needed.

5.3.2. Preparation of the calibration solutions

By diluting the standard solution (3.6.1) with 0,5 mol/l hydrochloric acid solution (3.3), prepare at least five standard solutions corresponding to the optimal measuring range of the spectrophotometer (0 to 5,0 mg/l Cu). Before making up to the mark, add to every solution ammonium nitrate (3.4) to give concentration of 100 mg per ml.

5.4. Measurement

Set up the spectrophotometer (4) at a wavelength of 324,8 nm. Use an oxidising air-acetylene flame. Spray successively, in triplicate, the calibration solution (5.3.2), the sample solution and the blank solution (5.3.1), washing the instrument through with distilled water between each spraying. Plot the calibration curve using the mean absorbances of every standard used as the ordinates and the corresponding concentrations of copper in µg/ml as the abscissae.

Determine the concentration of copper in the final sample and blank solutions by reference to the calibration curve.

6. Expression of the results

Calculate the copper content of the sample taking into account the mass of the test sample, the dilutions carried out in the course of the analysis and the value of the blank. Express the result as mg Cu/kg.

4. Determination of resistance to detonation

4.1. Scope and field of application

This document defines the procedure for the determination or resistance to detonation of ammonium nitrate fertilisers of high nitrogen content.

4.2. Principle

The test sample is confined in a steel tube and subjected to detonation shock from an explosive booster charge. Propagation of the detonation is determined from the degree of crushing of lead cylinders on which the tube rests horizontally during the test.

4.3. Materials

4.3.1. Plastic explosive containing 83 to 86 % penthrite

Density: 1500 to 1600 kg/m3

Detonation velocity: 7300 to 7700 m/s

Mass: 500 (± 1) gram.

4.3.2. Seven lengths of flexible detonating cord with non-metallic sleeve

Filling mass: 11 to 13 g/m

Length of each cord: 400 (± 2) mm.

4.3.3. Compressed pellet of secondary explosive, recessed to receive detonator

Explosive: hexogen/wax 95/5 or tetryl or similar secondary explosive, with or without added graphite.

Density: 1500 to 1600 kg/m3

Diameter: 19 to 21 mm

Height: 19 to 23 mm

Central recess to receive detonator: diameter 7 to 7,3 mm, depth 12 mm.

4.3.4. Seamless steel tube as specified in ISO 65 - 1981 - Heavy Series, with nominal dimensions DN 100 (4'')

Outside diameter: 113,1 to 115,0 mm

Wall thickness: 5,0 to 6,5 mm

Length: 1005 (± 2) mm.

4.3.5. Bottom place

Material: steel of good weldable quality

Dimensions: 160 × 160 mm

Thickness: 5 to 6 mm

4.3.6. Six lead cylinders

Diameter: 50 (± 1) mm

Height: 100 to 101 mm

Materials: soft lead, at least 99,5 % purity.

4.3.7. Steel block

Length: at least 1000 mm

Width: at least 150 mm

Height: at least 150 mm

Mass: at least 300 kg if there is no firm base for the steel block.

4.3.8. Plastic or cardboard cylinder for booster charge

Wall thickness: 1,5 to 2,5 mm

Diameter: 92 to 96 mm

Height: 64 to 67 mm

4.3.9. Detonator (electric or non-electric) with initiation force 8 to 10

4.3.10. Wooden disc

Diameter: 92 to 96 mm. Diameter to be matched to the internal diameter of the plastic or cardboard cylinder (4.3.8)

Thickness: 20 mm

4.3.11. Wooden rod of same dimensions as detonator (4.3.9)

4.3.12. Dressmaking pins (maximum length 20 mm)

4.4. Procedure

4.4.1. Preparation of booster charge for insertion into steel tube

There are two methods of initiation of the explosive in the booster charge, depending on the availability of equipment.

4.4.1.1. Seven-point simultaneous initiation

The booster charge prepared for use is shown in Figure 1.

4.4.1.1.1. Drill holes in the wooden disc (4.3.10) parallel to the axis of the disc through the centre and through six points symmetrically distributed around a concentric circle 55 mm in diameter. The diameter of the holes must be 6 to 7 mm (see Section A-B in Figure 1), depending on the diameter of the detonating cord used (4.3.2).

4.4.1.1.2. Cut seven lengths of flexible detonating cord (4.3.2) each 400 mm long, avoiding any loss of explosive at each end by making a clean cut and immediately sealing the end with adhesive. Push each of the seven lengths through the seven holes in the wooden disc (4.3.10) until their ends project a few centimetres on the other side of the disc. Then insert a small dressmaking pin (4.3.12) transversally into the textile sleeve of each length of cord 5 to 6 mm from the end and apply adhesive around the outside of the lengths of cord in a band 2 cm wide adjacent to the pin. Finally, pull the long piece of each cord to bring the pin into contact with the wooden disc.

4.4.1.1.3. Shape the plastic explosive (4.3.1) to form a cylinder 92 to 96 mm in diameter, depending on the diameter of the cylinder (4.3.8). Stand this cylinder upright on a level surface and insert the shaped explosive. Then insert the wooden disc(4) carrying the seven lengths of detonating cord into the top of the cylinder and press it down onto the explosive. Adjust the height of the cylinder (64 to 67 mm) so that its top edge does not extend beyond the level of the wood. Finally, fix the cylinder to the wooden disc for instance with staples or small nails, around its entire circumference.

4.4.1.1.4. Group the free ends of the seven lengths of detonating cord around the circumference of the wooden rod (4.3.11) so that their ends are all level in a plane perpendicular to the rod. Secure them in a bundle around the rod by means of adhesive tape(5).

4.4.1.2. Central initiation by a compressed pellet

The booster charge prepared for use is shown in Figure 2.

4.4.1.2.1. Preparing a compressed pellet

Taking the necessary safety precautions, place 10 grams of a secondary explosive (4.3.3) in a mould with an inside diameter of 19 to 21 mm and compress to the correct shape and density.

(The ratio of diameter: height should be roughly 1:1).

In the centre of the bottom of the mould there is a peg, 12 mm in height and 7,0 to 7,3 mm in diameter (depending on the diameter of the detonator used), which forms a cylindrical recess in the compressed cartridge for subsequent insertion of the detonator.

4.4.1.2.2. Preparing the booster charge

Place the explosive (4.3.1) into the cylinder (4.3.8) standing upright on a level surface, then press it down with a wooden die to give the explosive a cylindrical shape with a central recess. Insert the compressed pellet into this recess. Cover the cylindrically shaped explosive containing the compressed pellet with a wooden disc (4.3.10) having a central hole 7,0 to 7,3 mm in diameter for insertion of a detonator. Fix the wooden disc and the cylinder together with a cross of adhesive tape. Ensure that the hole drilled in the disc and the recess in the compressed pellet are coaxial by inserting the wooden rod (4.3.11).

4.4.2. Preparing steel tubes for the detonation tests

At one end of the steel tube (4.3.4), drill two diametrically opposed holes 4 mm in diameter perpendicularly through the side wall at a distance of 4 mm from the edge.

Butt weld the bottom plate (4.3.5) to the opposite end of the tube, completely filling the right angle between the bottom place and the wall of the tube with weld metal around the entire circumference of the tube.

4.4.3. Filling and charging the steel tube

See Figures 1 and 2.

4.4.3.1. The test sample, the steel tube and the booster charge must be conditioned to temperatures of 20 (± 5) °C. 16 to 18 kg of the test sample are needed for two detonation tests.

4.4.3.2. Place the tube upright with its square bottom place resting on a firm, flat surface, preferably concrete. Fill the tube to about one-third of its height with the test sample and drop it 10 cm vertically onto the floor five times to compact the prills or granules as densely as possible in the tube. To accelerate compaction, vibrate the tube by striking the side wall with a 750 to 1000-gram hammer between drops for a total of 10 times.

Repeat this charging method with another portion of the test sample. Finally, a further addition shall be made such that, after compaction by raising and dropping the tube 10 times and a total of 20 intermittent hammer blows, the charge fills the tube to a distance of 70 mm from its orifice.

The filling height of the sample must be adjusted in the steel tube so that the booster charge (4.4.1.1 or 4.4.1.2) to be inserted later will be in close contact with the sample over its entire surface.

4.4.3.3. Insert the booster charge into the tube so that it is in contact with the sample; the top surface of the wooden disc must be 6 mm below the end of the tube. Ensure essential close contact between explosive and test sample by adding or removing small quantities of sample. As shown in Figures 1 and 2, split pins should be inserted through the holes near the open end of the tube and their legs opened flat against the tube.

4.4.4. Positioning of the steel tube and lead cylinders (see figure 3)

4.4.4.1. Number the bases of the lead cylinders (4.3.6) 1 to 6. Make six marks 150 mm apart on the centre line of a steel block (4.3.7) lying on a horizontal base, with the first mark at least 75 mm from the edge of the block. Place a lead cylinder upright on each of these marks, with the base of each cylinder centred on its mark.

4.4.4.2. Lay the steel tube prepared according to 4.4.3 horizontally on the lead cylinders so that the axis of the tube is parallel to the centre line of the steel block and the welded end of the tube extends 50 mm beyond lead cylinder No 6. To prevent the tube from rolling, insert small wooden wedges between the tops of the lead cylinders and the tube wall (one on each side) or place a cross of wood between the tube and the steel block.

Note:

Make sure that the tube is in contact with all six lead cylinders; a slight curvature of the tube surface can be compensated for by rotating the tube about its longitudinal axis; if any of the lead cylinders is too tall, tap the cylinder in question carefully with a hammer until it is the required height.

4.4.5. Preparation for detonation

4.4.5.1. Set up the apparatus according to the 4.4.4 in a bunker or suitably prepared underground site (e.g. mine or tunnel). Ensure that the temperature of the steel tube is kept at 20 (± 5) °C before detonation.

Note:

Should such firing sites not be available, the work can, if necessary, be done in a concrete-lined pit covered over with wooden beams. Detonation can cause steel fragments to be projected with high kinetic energy, therefore, firing must be carried out at a suitable distance from dwellings or thoroughfares.

4.4.5.2. If the booster charge with seven-point initiation is used, ensure that the detonation cords are stretched out as described in the footnote to 4.4.1.1.4 and arranged as horizontally as possible.

4.4.5.3. Finally, remove the wooden rod and replace with the detonator. Do not carry out firing until the danger zone has been evacuated and the test personnel have taken cover.

4.4.5.4. Detonate the explosive.

4.4.6. Allow sufficient time for the fumes (gaseous and sometimes toxic decomposition products such as nitrous gases) to disperse, then collect the lead cylinders and measure their heights with a Vernier caliper

Record for each of the marked lead cylinders, the degree of crushing expressed as a percentage of the original height of 100 mm. If the cylinders are crushed obliquely, record the highest and the lowest values and calculate the average.

4.4.7. A probe for continuous measurement of the detonation velocity can be used; the probe should be inserted longitudinally to the axis of the tube or along its side wall

4.4.8. Two detonation tests per sample are to be carried out

4.5. Test report

Values for the following parameters are to be given in the test report for each of the detonation tests:

- the values actually measures for the outside diameter of the steel tube and for the wall thickness,

- the Brinell hardness of the steel tube,

- the temperature of the tube and the sample shortly before firing,

- the packing density (kg/m3) of the sample in the steel tube,

- the height of each lead cylinder after firing, specifying the corresponding cylinder number,

- method of initiation employed for the booster charge.

4.5.1. Evaluation of test results

If, in each firing, the crushing of at least one lead cylinder is less than 5 %, the test shall be considered conclusive and the sample in conformity with the requirements of Annex III.2.

Figure 1

>PIC FILE= "L_2003304EN.007001.TIF">

Figure 2

>PIC FILE= "L_2003304EN.007101.TIF">

Figure 3

>PIC FILE= "L_2003304EN.007201.TIF">

(1) 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.

(2) Commercially available standard copper solution may be used.

(3) Whatman 541 or equivalent.

(4) The diameter of the disc must always correspond to the inside diameter of the cylinder.

(5) NB:

When the six peripheral lengths of cord are taut after assembly, the central cord must remain slightly slack.

ANNEX IV

METHODS OF SAMPLING AND ANALYSIS

A. METHOD OF SAMPLING FOR THE CONTROL OF FERTILISERS

INTRODUCTION

Correct sampling is a difficult operation which requires the greatest of care. The need to obtain a sufficiently representative sample for the official testing of fertilisers cannot, therefore, be stressed too much.

The sampling method described below must be applied with strict accuracy by specialists with experience of the conventional sampling procedure.

1. Purpose and scope

Samples intended for the official control of fertilisers, for quality and composition, shall be taken according to the methods described below. Samples thus obtained shall be considered as representative of the sampled portions.

2. Sampling officers

The samples shall be taken by specialist officers authorised for that purpose by the Member States.

3. Definitions

Sampled portion: A quantity of product constituting a unit, and having characteristics presumed to be uniform.

Incremental sample: A quantity taken from one point in the sampled portion.

Aggregate sample: An aggregate of incremental samples taken from the same sampled portion.

Reduced sample: A representative part of the aggregate sample, obtained from the latter by a process of reduction.

Final sample: A representative part of the reduced sample.

4. Apparatus

4.1. The sampling apparatus must be made of materials which cannot affect the characteristics of the products to be sampled. Such apparatus may be officially approved by the Member States.

4.2. Apparatus recommended for the sampling of solid fertilisers

4.2.1. Manual sampling

4.2.1.1. Flat-bottomed shovel with vertical sides.

4.2.1.2. Sampling spear with a long split or compartments. The dimensions of the sampling spear must be appropriate to the characteristics of the sampled portion (depth of container, dimensions of sack, etc.) and to the particle size of the fertiliser.

4.2.2. Mechanical sampling

Approved mechanical apparatus may be used for the sampling of moving fertilisers.

4.2.3. Divider

Apparatus designed to divide the sample into equal parts may be used for taking incremental samples and for the preparation of reduced and final samples.

4.3. Apparatus recommended for the sampling of fluid fertilisers

4.3.1. Manual sampling

Open tube, probe, bottle or another appropriate equipment able to take samples at random from the sampled portion.

4.3.2. Mechanical sampling

Approved mechanical apparatus may be used for sampling of moving fluid fertilisers.

5. Quantitative requirements

5.1. Sampled portion

The size of the sampled portion must be such that each of its constituent parts can be sampled.

5.2. Incremental samples

5.2.1. Loose solid fertilisers or fluid fertilisers in containers exceeding 100 kg

5.2.1.1. Sampled portions not exceeding 2,5 tonnes:

Minimum number of incremental samples: seven

5.2.1.2. Sampled portions exceeding 2,5 tonnes and up to 80 tonnes:

Minimum number of incremental samples:

>REFERENCE TO A GRAPHIC>

5.2.1.3. Sampled portions exceeding 80 tonnes:

Minimum number of incremental samples: 40

5.2.2. Packaged solid fertilisers or fluid fertilisers in containers (= packages each not exceeding 100 kg)

5.2.2.1. Packages of more than 1 kg

5.2.2.1.1. Sampled portions of less than five packages:

Minimum number of packages to be sampled(2): all packages.

5.2.2.1.2. Sampled portions of five to 16 packages:

Minimum number of packages to be sampled(3): four.

5.2.2.1.3. Sampled portions of 17 to 400 packages:

Minimum number of packages to be sampled(4):

>REFERENCE TO A GRAPHIC>

5.2.2.1.4. Sampled portions exceeding 400 packages:

Minimum number of packages to be sampled(6): 20.

5.2.2.2. Packages not exceeding 1 kg:

Minimum number of packages to be sampled(7): four.

5.3. Aggregate sample

A single aggregate sample per sampled portion is required. The total mass of the incremental samples making up the aggregate sample shall be not less than the following:

5.3.1. Loose solid fertilisers or fluid fertilisers in containers exceeding 100 kg: 4 kg.

5.3.2. Packaged solid fertilisers or fluid fertilisers in containers (= packages) each not exceeding 100 kg

5.3.2.1. Packages of more than 1 kg: 4 kg

5.3.2.2. Packages not exceeding 1 kg: mass of the contents of four original packages.

5.3.3. Ammonium nitrate fertiliser sample for tests according to Annex III.2: 75 kg

5.4. Final samples

The aggregate sample gives the final samples on reduction when necessary. Analysis of at least one final sample is required. The mass of the sample for analysis shall not be less than 500 g.

5.4.1. Solid and fluid fertilisers

5.4.2. Ammonium nitrate fertiliser sample for tests

The aggregate sample gives the final sample for tests on reduction when necessary.

5.4.2.1. Minimum final sample mass for Annex III.1 tests: 1 kg

5.4.2.2. Minimum final sample mass for Annex III.2 tests: 25 kg

6. Instructions for taking, preparing and packaging the samples

6.1. General

The samples must be taken and prepared as quickly as possible bearing in mind the precautions necessary to ensure that they remain representative of the fertiliser sampled. Instruments and also surfaces and containers intended to receive samples must be clean and dry.

In the case of fluid fertilisers, if possible the sampled portion should be mixed prior to sampling.

6.2. Incremental samples

Incremental samples must be taken at random throughout the whole sampled portion and they must be of approximately equal sizes.

6.2.1. Loose solid fertilisers or fluid fertilisers in containers exceeding 100 kg

An imaginary division shall be made of the sampled portion into a number of approximately equal parts. A number of parts corresponding to the number of incremental samples required in accordance with 5.2 shall be selected at random and at least one sample taken from each of these parts. Where it is not possible to comply with the requirements of 5.1 when sampling bulk fertilisers or fluid fertilisers in containers exceeding 100 kg the sampling should be carried out when the sampled portion is being moved (loading or unloading). In this case samples shall be taken from the randomly selected notional parts as defined above while these are being moved.

6.2.2. Packaged solid fertilisers or fluid fertilisers in containers (= packages) each not exceeding 100 kg

Having selected the required number of packages for sampling as indicated in 5.2, part of the contents of each package shall be removed. Where necessary, the samples shall be taken after emptying the packages separately.

6.3. Preparation of aggregate sample

The incremental samples shall be mixed to form a single aggregate sample.

6.4. Preparation of the final sample

The material in the aggregate sample shall be carefully mixed(8).

If necessary the aggregate sample should first be reduced to at least 2 kg (reduced sample) either by using a mechanical divider or by the quartering method.

At least three final samples shall then be prepared, of approximately the same amount and conforming to the quantitative requirements of 5.4. Each sample shall be put into an appropriate air tight container. All necessary precautions shall be taken to avoid any change in the characteristics of the sample.

For the tests of Annex III, sections 1 and 2, the final samples shall be kept at a temperature between 0 °C and 25 °C.

7. Packaging of final samples

The containers or packages shall be scaled and labelled (the total label must be incorporated in the seal) in such a manner that they cannot be opened without damaging the seal.

8. Sampling record

A record must be kept of each sampling, permitting each sampled portion to be identified unambiguously.

9. Destination of samples

For each sample portion at least one final sample shall be sent as quickly as possible to an authorised analytical laboratory or to the test institution, together with the information necessary for the analysis or the test.

B. METHODS FOR THE ANALYSIS OF FERTILISERS

(See table of contents p. 2.)

General observations

Laboratory equipment

In the descriptions of the methods, general laboratory equipment has not been precisely defined, except that the sizes of flasks and pipettes are given. In all cases laboratory apparatus must be well cleaned, particularly when small quantities of elements are to be determined.

Control tests

Before analysis it is necessary to ensure that all apparatus functions well and that the analytical technique is carried out correctly, using where appropriate chemical compounds of known composition (e.g. ammonium sulphate, mono potassium phosphate, etc.). Nevertheless, the results from analysed fertilisers can indicate wrong chemical composition if the analytical technique is not rigorously followed. On the other hand, a certain number of determinations are empirical and are relative to products of complex chemical composition. It is recommended that where available, laboratories should make use of standard reference fertilisers of well defined composition.

General provisions relating to methods of analysing fertilisers

1. Reagents

Unless otherwise specified in the method of analysis, all of the reagents must be analysis-pur (a.p.). Where micro-nutrients are to be analysed the purity of the reagents must be checked by means of a blank test. Depending upon the result obtained, it might be necessary to conduct a further purification.

2. Water

Where dissolution, dilution, rinsing or washing operations referred to in the methods of analysis do not specify the nature of solvents or diluents the use of water is implied. Normally, the water will have to be demineralised or distilled. In these specific instances, as mentioned in the method of analysis, that water will have to be subjected to specific purification processes.

3. Laboratory equipment

In view of the equipment normally used in inspection laboratories, the apparatus described in the methods of analysis is restricted to special instruments and apparatus or to such demanded by any specific requirements. This equipment must be perfectly clean, above all where small quantit