Proposal for a REGULATION OF THE EUROPEAN PARLIAMENT AND OF THE COUNCIL relating to fertilizers

(presented by the Commission)

TABLE OF CONTENTS

EXPLANATORY MEMORANDUM

1. General Comments

1.1. Policy

1.2. Directives concerned

1.3. Drafting Methodology and Structure

1.3.1. SLIM recommendations

1.3.2. Structure

1.4. Cadmium

1.4.1. The problem

1.4.2. Strategy

2. Specific Comments

REGULATION OF THE EUROPEAN PARLIAMENT AND OF THE COUNCIL

relating to fertilizers

ANNEX I - List of types of EC fertilizers

A. Inorganic straight primary nutrient fertilizers

A.1. Nitrogenous fertilizers

A.2. Phosphatic fertilizers

A.3. Potassic fertilizers

B. Inorganic compound primary nutrient fertilizers

B.1. NPK fertilizers

B.2. NP fertilizers

B.3. NK fertilizers

B.4. PK fertilizers

C. Inorganic fluid fertilizers

C.1. Straight fluid fertilizers

C.2. Compound fluid fertilizers

D. Inorganic secondary nutrient fertilizers

E. Inorganic micro-nutrient fertilizers

E.1. Fertilizers containing only one micro-nutrient

E.1.1. Boron...

E.1.2. Cobalt..

E.1.3. Copper.

E.1.4 Iron.....

E.1.5. Manganese

E.1.6. Molybdenum

E.1.7. Zinc.....

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

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

ANNEX II - Tolerances

1. Inorganic straight primary nutrient fertilizers - absolute value in percentage by mass expressed as N, P2O5, K2O, mgo, Cl

2. INORGANIC COMPOUND PRIMARY NUTRIENT FERTILIZERS

3. SECONDARY NUTRIENTS IN FERTILIZERS

4. MICRO-NUTRIENTS IN FERTILIZERS

ANNEX III - Technical provisions for Ammonium Nitrate Fertilizers of High Nitrogen Content

1. CHARACTERISTICS OF AND LIMITS FOR STRAIGHT AMMONIUM NITRATE FERTILIZERS OF HIGH NITROGEN CONTENT

2. DESCRIPTION OF THE TEST OF RESISTANCE TO DETONATION CONCERNING AMMONIUM NITRATE FERTILIZERS OF HIGH NITROGEN CONTENT

3. METHODS OF CHECKING COMPLIANCE WITH THE LIMITS SPECIFIED

IN ANNEXES III-1 and III-2

4. DETERMINATION OF RESISTANCE TO DETONATION

ANNEX IV - Methods of Sampling and Analysis

A. METHOD OF SAMPLING FOR THE CONTROL OF FERTILIZERS

1. PURPOSE AND SCOPE

2. SAMPLING OFFICERS

3. DEFINITIONS

4. APPARATUS

5. QUANTITATIVE REQUIREMENTS

6. INSTRUCTIONS FOR TAKING, PREPARING AND PACKAGING THE SAMPLES

7. PACKAGING OF FINAL SAMPLES

8. SAMPLING RECORD

9. DESTINATION OF SAMPLES

B. METHODS FOR THE ANALYSIS OF FERTILIZERS

GENERAL OBSERVATIONS

GENERAL PROVISIONS RELATING TO METHODS OF ANALYZING FERTILIZERS

Method 1 - PREPARATION OF THE SAMPLE FOR ANALYSIS

Methods 2 - NITROGEN

Method 2.1 - DETERMINATION OF AMMONIACAL NITROGEN

Methods 2.2 - DETERMINATION OF NITRIC AND AMMONIACAL NITROGEN

Method 2.2.1 - DETERMINATION OF NITRIC AND AMMONIACAL NITROGEN

ACCORDING TO ULSCH

Method 2.2.2 - DETERMINATION OF NITRIC AND AMMONIACAL NITROGEN ACCORDING TO ARND

Method 2.2.3 - DETERMINATION OF NITRIC AND AMMONIACAL NITROGEN ACCORDING TO DEVARDA

Method 2.3 - DETERMINATION OF TOTAL NITROGEN

Method 2.3.1 - DETERMINATION OF THE TOTAL NITROGEN IN CALCIUM CYANAMIDE NITRATE FREE

Method 2.3.2 - DETERMINATION OF TOTAL NITROGEN IN CALCIUM CYANAMIDE

CONTAINING NITRATES

Method 2.3.3 - DETERMINATION OF TOTAL NITROGEN IN UREA

Method 2.4 - DETERMINATION OF CYANAMIDE NITROGEN

Method 2.5 - SPECTROPHOTOMETRIC DETERMINATION OF BIURET IN UREA

Methods 2.6 - DETERMINATION OF DIFFERENT FORMS OF NITROGEN IN THE SAME

SAMPLE

Method 2.6.1 - DETERMINATION OF DIFFERENT FORMS OF NITROGEN IN THE SAME SAMPLE IN FERTILIZERS CONTAINING NITROGEN AS NITRIC, AMMONIACAL, UREA AND CYANAMIDE NITROGEN

Method 2.6.2 - DETERMINATION OF DIFFERENT FORMS OF NITROGEN IN FERTILIZERS CONTAINING NITROGEN ONLY AS NITRIC AMMONIACAL AND UREA NITROGEN

Methods 3 - PHOSPHORUS

Methods 3.1 - EXTRACTIONS

Method 3.1.1 - EXTRACTION OF PHOSPHORUS SOLUBLE IN MINERAL ACIDS

Method 3.1.2 - EXTRACTION OF THE PHOSPHORUS SOLUBLE IN 2 % FORMIC ACID (20 g per litre)

Method 3.1.3 - EXTRACTION OF PHOSPHORUS SOLUBLE IN 2 % CITRIC ACID (20 g per litre)

Method 3.1.4 - EXTRACTION OF PHOSPHORUS WHICH IS SOLUBLE IN NEUTRAL

AMMONIUM CITRATE

Methods 3.1.5 - EXTRACTION BY ALKALINE AMMONIUM CITRATE

Method 3.1.5.1 - Extraction of soluble phosphorus according to Petermann at 65 °C

Method 3.1.5.2 - Extraction of the soluble phosphorus according to Petermann at ambient temperature

Method 3.1.5.3 - Extraction of the phosphorus soluble in Joulie's alkaline ammonium citrate

Method 3.1.6 - EXTRACTION OF WATER SOLUBLE PHOSPHORUS

Method 3.2 - DETERMINATION OF EXTRACTED PHOSPHORUS (Gravimetric Method using quinoline phosphomolybdate)

Method 4 - POTASSIUM

Method 4.1 - DETERMINATION OF THE WATER SOLUBLE POTASSIUM CONTENT

Method 5

Method 6 - CHLORINE

Method 6.1 - DETERMINATION OF CHLORIDES IN THE ABSENCE OF ORGANIC

MATERIAL

Methods 7 - FINENESS OF GRINDING

Method 7.1 - DETERMINATION OF FINENESS OF GRINDING (dry procedure)

Method 7.2 - DETERMINATION OF THE FINENESS OF GRINDING OF SOFT NATURAL

PHOSPHATES

Methods 8 - SECONDARY NUTRIENTS

Method 8.1 - EXTRACTION OF TOTAL CALCIUM, TOTAL MAGNESIUM, TOTAL

SODIUM AND TOTAL SULPHUR IN THE FORM OF SULPHATES

Method 8.2 - EXTRACTION OF TOTAL SULPHUR PRESENT IN VARIOUS FORMS

Method 8.3 - EXTRACTION OF WATER-SOLUBLE CALCIUM, MAGNESIUM, SODIUM AND SULPHUR (in the form of sulphates)

Method 8.4 - EXTRACTION OF WATER-SOLUBLE SULPHUR WHERE THE SULPHUR

IS IN VARIOUS FORMS

Method 8.5 - EXTRACTION AND DETERMINATION OF ELEMENTAL SULPHUR

Method 8.6 - MANGANIMETRIC DETERMINATION OF EXTRACTED CALCIUM FOLLOWING PRECIPITATION IN THE FORM OF OXALATE

Method 8.7 - DETERMINATION OF MAGNESIUM BY ATOMIC ABSORPTION SPECTROMETRY

Method 8.8 - DETERMINATION OF MAGNESIUM BY COMPLEXOMETRY

Method 8.9 - DETERMINATION OF SULPHATES

Method 8.10 - DETERMINATION OF THE SODIUM EXTRACTED

Methods 9 - MICRO-NUTRIENTS at a concentration of less than or equal to 10%

Method 9.1 - EXTRACTION OF TOTAL MICRO-NUTRIENTS

Method 9.2 - EXTRACTION OF WATER-SOLUBLE MICRO-NUTRIENTS

Method 9.3 - REMOVAL OF ORGANIC COMPOUNDS FROM FERTILIZER EXTRACTS

Method 9.4 - DETERMINATION OF MICRO-NUTRIENTS IN FERTILIZER EXTRACTS BY ATOMIC ABSORPTION SPECTROMETRY (general procedure)

Method 9.5 - DETERMINATION OF BORON IN FERTILIZER EXTRACTS BY MEANS OF SPECTROMETRY WITH AZOMETHINE-H

Method 9.6 - DETERMINATION OF COBALT IN FERTILIZER EXTRACTS BY ATOMIC ABSORPTION SPECTROMETRY

Method 9.7 - DETERMINATION OF COPPER IN FERTILIZER EXTRACTS BY ATOMIC ABSORPTION SPECTROMETRY

Method 9.8 - DETERMINATION OF IRON IN FERTILIZER EXTRACTS BY ATOMIC ABSORPTION SPECTROMETRY

Method 9.9 - DETERMINATION OF MANGANESE IN FERTILIZER EXTRACTS BY ATOMIC ABSORPTION SPECTROMETRY

Method 9.10 - DETERMINATION OF MOLYBDENUM IN FERTILIZER EXTRACTS BY SPECTROMETRY OF A COMPLEX WITH AMMONIUM THIOCYANATE

Method 9.11 - DETERMINATION OF ZINC IN FERTILIZER EXTRACTS BY ATOMIC ABSORPTION SPECTROMETRY

Methods 10 - MICRO-NUTRIENTS AT A CONCENTRATION GREATER THAN 10 %

Method 10.1 - EXTRACTION OF TOTAL MICRO-NUTRIENTS

Method 10.2 - EXTRACTION OF WATER-SOLUBLE MICRO-NUTRIENTS

Method 10.3 - REMOVAL OF ORGANIC COMPOUNDS FROM FERTILIZER EXTRACTS

Method 10.4 - DETERMINATION OF MICRO-NUTRIENTS IN FERTILIZER EXTRACTS

BY ATOMIC ABSORPTION SPECTROMETRY (general procedure)

Method 10.5 - DETERMINATION OF BORON IN FERTILIZER EXTRACTS BY MEANS

OF ACIDIMETRIC TITRATION

Method 10.6 - DETERMINATION OF COBALT IN FERTILIZER EXTRACTS BY THE GRAVIMETRIC METHOD WITH 1-NITROSO-2-NAPHTHOL

Method 10.7 - DETERMINATION OF COPPER IN FERTILIZER EXTRACTS BY THE TITRIMETRIC METHOD

Method 10.8 - DETERMINATION OF IRON IN FERTILIZER EXTRACTS BY ATOMIC ABSORPTION SPECTROMETRY

Method 10.9 - DETERMINATION OF MANGANESE IN FERTILIZER EXTRACTS BY TITRATION

Method 10.10 - DETERMINATION OF MOLYBDENUM IN FERTILIZER EXTRACTS BY THE GRAVIMETRIC METHOD WITH 8-HYDROXYQUINOLINE

Method 10.11 - DETERMINATION OF ZINC IN FERTILIZER EXTRACTS BY ATOMIC ABSORPTION SPECTROMETRY

ANNEX V

A. List of documents to be consulted by manufacturers or their representatives in order to compile a technical file for a new type of fertilizers to be added to annex I of this regulation

B. Standards of accreditation concerning the laboratories that are competent and authorised to provide the necessary service for checking compliance of EC fertilizers with the requirements of this Regulation and its annexes

IMPACT ASSESSMENT FORM - DRAFT OF THE IMPACT OF THE PROPOSAL ON BUSINESS WITH SPECIAL REFERENCE TO SMALL AND MEDIUM-

SIZED ENTERPRISES (SMEs)

EXPLANATORY MEMORANDUM

1. General Comments

1.1. Policy

In the context of a people's Europe, the Commission attaches great importance to simplifying and clarifying Community law so as to make it more accessible to the ordinary citizen, thus giving him new opportunities and the chance to make use of the specific rights it gives him.

This aim cannot be achieved as long as numerous provisions that have been amended several times remain scattered, so that they must be sought partly in the original instrument and partly in later amending ones. Considerable research work, comparing many different instruments, is thus needed to identify the current rules.

For this reason, a consolidation of rules that have frequently been amended is essential if Community law is to be clear and transparent.

1.2. Directives concerned

The attached proposal of the Commission is a recast of Council and Commission Directives on the approximation of the laws of the Member States relating to fertilizers. It integrates within a single text the following Directives:

- Council Directive 76/116/EEC of 18 December 1975 on the approximation of the laws of the Member States relating to fertilizers;

- Council Directive 80/876/EEC of 15 July 1980 on the approximation of the laws of the Member States relating to straight ammonium nitrate fertilizers on high nitrogen content;

- 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 fertilizers of high nitrogen content;

- 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 fertilizers,

and the various amendments and adaptations to technical progress to these directives (see first whereas of the attached proposal).

1.3. Drafting Methodology and Structure

1.3.1. SLIM recommendations

Recommendations on what to include into the simplification of the fertilizer legislation were given by the Commission's SLIM II working group in its final report dated 27 October 1997. This, as well as all other points of relevance have been discussed in detail by the Commission's fertilizer working group (here: the working group), where experts from Member States and Industry gave their advice in altogether 13 days of meetings between March 1998 and December 2000. Implementation of this advice had to be guided by scientific, legal and pragmatic considerations. In particular, the SLIM group's recommendations to address certain issues in the recast have been taken into account as follows:

(a) Establishment of an ad-hoc group to advise the Commission For largest possible flexibility it is proposed to leave this to be organised by the Commission's working group on fertilizers on a case by case basis. Article 32 of the recast gives information on how to submit a proposal concerning fertilizers to the Commission.

(b) Criteria for the decision on new types of fertilizers (incl. organic). See Article 14.

(c) Requirements for types fertilizers to be added to the list. See Article 14.

(d) Requirement for mixtures of fertilizers according to compatibility. This is implicitly included in Article 14.

(e) Requirements for peer-reviewing of dossiers of new types of fertilizers with health and safety concerns. This is implicitly part of Article 14. The working group has agreed to decide on a case by case basis to ask for peer-reviewing of proposals.

(f) Conditions for adding new fertilizer groups. The working group has agreed that types of fertilizers of new fertilizer groups (e.g. organic) will only be considered after adoption of this recast and Article 14 provides for the necessity to define test methods.

(g) Controls by network of accredited laboratories and reports. Provisions are in Article 30, and whereas No 9.

(h) Study group on cadmium. This group has been established independently of the recast work, within the framework of the working group related to fertilizers, to permit consultations and discussions with Member States and interested parties. See transitional provisions, Article 33.

(i) Mixture of fertilizers. See Article 9a, last indent. Technical provisions for the identification of nutrients apply.

1.3.2. Structure

This recast has been structured in such a way as to exclude as far as possible all technical specifications from the legal text and instead include them into the annexes. Hence, as a guiding rule, the legal text was kept as general as possible. Undoubtedly, a "new approach" recast would have made things even easier. But that was neither the advice of the SLIM group, nor does it seem that there is, for the time being, enough common understanding on all the necessary standards for analysis. However, provisions [Article 29(4)] have been included to stimulate future adaptation to technical progress to be made in accordance with the "new approach".

In this draft, common provisions are separated from specific provisions. The latter ones are being ordered according to the main groups of fertilizers that are currently included in the legislation. This provides a rather simple way of using this legislation and adding other possible groups of fertilizers (e.g. organic fertilizers) without the need to restructure the whole instrument again.

The technical annexes have been compiled from the original Directives and rearranged. The working group has reviewed the annexes and has introduced some changes, however of a rather minor nature. In particular, technical specifications on nutrient contents have not been changed and tolerance levels have all been put into the annex. It was agreed that in the future a more detailed review of the specific technical requirements of the annexes would be needed in order to bring them up to date with state of the art analysis technology on fertilizers. However, experience of some Member Sates with their national fertilizer legislation showed that this would require several years. It was therefore decided to separate that work from this work on the recast.

The legal instrument chosen is that of a regulation. This is justified by the many adaptations to technical progress that this legislation has been and will be subjected to. In addition, a regulation imposes directly on manufacturers precise requirements to be implemented at the same time and in the same manner throughout the Community. Thus, it facilitates the tasks of the Member States and the economic operators and promotes a uniform application in the internal market.

1.4. Cadmium

1.4.1. The problem

Unintentional cadmium content in mineral fertilizers is a concern, in particular for Austria, Finland and Sweden who, since their accession to the Community, are allowed until 31 December 2001 to restrict the placing on the market of EC-fertilizers with a cadmium content above their national thresholds. No limit values exist on the European level and hence the European fertilizer legislation is currently not fully harmonised. The Commission has committed itself in 1998 to solve this problem by the end of 2001 and has together with the Member States initiated and conducted a risk assessment programme of cadmium in fertilizers.

1.4.2. Strategy

When the risk assessment programme is terminated, the Commission will make a proposal on what measures should be taken, if any, at Community level.

The current recast does therefore not address the cadmium issue, it is limited to the more technical process of recasting the present law. It should therefore be possible to adopt it rapidly. This is all the more necessary as it provides for a transitory period of two years during which the problem of cadmium can be resolved. Afterwards, a similar review on other contaminants will be performed in case that their presence would adversely affect human, animal or plant health, or the environment.

2. Specific Comments

The structure of the recast is indicated by its table of contents.

Much of the text has been copied from the old directives, but rearranged to fit to the structure. Use was made of all the articles of the old directives except in cases of redundancy. Whenever possible, the wording of the old directives has been used.

Article 2 For the most important terms definitions have been introduced, most of them are equivalent to those used by CEN, some have been altered following the advice of the expert working group.

Articles 3 The designation "EC fertilizer" is reserved for those fertilizers complying with this Regulation.

Article 4 Emphasis was put on ensuring that the responsibilities of the person who places the fertilizer on the market are clearly spelled out.

Article 5 This Article enunciates the principle of free circulation in the internal market.

Article 6 Articles of the old directives defining general requirements for the declarations of all types of nutrients have been integrated in this article.

Articles 7-12 Labelling and packaging requirements were taken over almost unchanged from the old directives.

Article 13 This Article relates to the tolerances for the declared contents of nutrients. In Annex II of this Regulation it is made clear that the tolerances are meant to be negative values only. Paragraph 2 specifies the obligations of the manufacturers. Paragraph 3 was copied from the technical Annex III of Directive 76/116/EEC.

Article 14 This Article defines the general requirements that a type of fertilizer must fulfil for Annex I inclusion, introducing explicitly the notion of presenting analysis methods in a proposal.

Article 15 The safeguard clause was hitherto only part of Directive 80/876/EEC concerning the approximation of the laws of the Member Sates relating to straight ammonium nitrate fertilizers of high nitrogen content. It is now applicable to the entire EC fertilizer legislation.

Articles 16-19 Scope, declaration and identification provisions have been included here for the specific types of fertilizers as indicated. They have been copied from the old directives with changes in order to simplify and improve clarity.

Articles 20, 21 Similar as in Articles 16-19, specific requirements for these particular types of fertilizers are defined.

Articles 22, 23 Ibid.

Article 24 As in the previous Directive

Articles 25-28 The scope has been expanded from straight to compound ammonium nitrate fertilizers, of high nitrogen content in order to take into account the new market situation. According to the old legislation compounds would not be subject to detonation tests thus creating a loop hole that Members States wanted to close because of safety and security reasons.

Hence the detonation test can now be required by Member States also for compound Ammonium Nitrate fertilizer of high nitrogen content. If an EC fertilizer satisfies the requirement of the test of resistance to detonation mentioned in Annex III of this Regulation, it should be subject to less stringent national provisions, in particular as regards storage.

Article 29 This Article on compliance provisions includes provisions to use, whenever possible, European standards for adaptation to technical progress of analysis methods, introducing the new approach to future legislation in this sector.

Article 30 This is new and provides for a better framework for analysis and testing. The SLIM group and Member States saw the need to introduce a quality assurance scheme for laboratories. Because of the diverse situation in Member states transitional measure have been introduced as well (see Article 34).

Article 31 Provisions are defined on what to do when applying for Annex I inclusion of a new type of fertilizer.

Article 32 The relevant Comitology according to Council Decision 1999/468/EC.

Articles 33, 34 Transitional provisions, partly from existing directives and partly as indicated under Article 30. The derogation for Austria, Finland and Sweden mentioned in Article 33 has been prolonged till 31 December 2004 in order to allow sufficient time for Community measures on cadmium to be decided.

Articles 35-38 Final provisions.

2001/0212 (COD)

Proposal for a

REGULATION OF THE EUROPEAN PARLIAMENT AND OF THE COUNCIL

relating to fertilizers

(Text with EEA relevance)

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],

[1] OJ C

Having regard to the opinion of the Economic and Social Committee [2],

[2] OJ C

Acting in accordance with the procedure laid down in Article 251 of the Treaty [3],

[3] OJ C

Whereas:

(1) Council Directive 76/116/EEC of 18 December 1975 on the approximation of the laws of the Member States relating to fertilizers [4], as last amended by Directive 98/97/EC of the European Parliament and the Council [5], Council Directive 80/876/EEC of 15 July 1980 on the approximation of the laws of the Member States relating to straight ammonium nitrate fertilizers of high nitrogen content [6], as amended by Directive 97/63/EC of the European Parliament and the Council [7], 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 fertilizers of high nitrogen content [8], as amended by Directive 88/126/EEC [9] 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 fertilizers [10], as last amended by Directive 95/8/EC [11], have been substantially amended several times. In accordance with the communication from the Commission to the Council and the European Parliament "Simpler legislation for the internal market" [12] (SLIM) and the Action Plan for the Single Market [13] those Directives should be repealed and replaced by a single legal instrument, in the interests of clarity.

[4] OJ L 24, 30.1.1976, p. 21.

[5] OJ L 18, 23.1.1999, p. 60.

[6] OJ L 250, 23.9.1980, p. 7.

[7] OJ L 335, 6.12.1997, p. 15.

[8] OJ L 38, 7.2.1987, p. 1.

[9] OJ L 63, 9.3.1988, p. 12.

[10] OJ L 213, 22.8.1977, p. 1.

[11] OJ L 86, 20.4. 1995,p. 41.

[12] COM(96) 204 final.

[13] CSE(97) 1 final.

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

(3) In each Member State fertilizers must display certain technical characteristics laid down by mandatory provisions. These provisions, concerning more particularly the composition and definition of fertilizers types, 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. They should therefore be harmonised.

(4) Since the objectives of the proposed action namely to ensure the internal market in fertilizers, 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 those objectives.

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

(6) Community rules on the identification and labelling of these fertilizers, 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 fertilizers.

(8) The production of fertilizers 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 fertilizers with requirements of this Regulation concerning quality and composition should be carried out by competent laboratories.

(10) Ammonium nitrate is the essential ingredient of a variety of products, some of which are intended for use as fertilizers and others as explosives. I It is necessary, having regard to the particular nature of ammonium nitrate fertilizers of high nitrogen content and to the requirements it entails regarding public safety, health and protection of workers, to lay down additional Community rules for EC fertilizers 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. Member States should therefore not be prevented from taking appropriate steps to avoid such use.

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

(13) Ammonium nitrate EC fertilizers of high nitrogen content should conform to certain characteristics to ensure that they are harmless. Member States should be able to subject such fertilizers to a test of resistance to detonation before or after they are placed on the market. If an EC fertilizer satisfies the requirement of the test of resistance to detonation, it should be subject to less stringent national provisions, in particular as regards storage.

(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) Fertilizers can be contaminated by substances that can potentially pose a risk to human and animal health and the environment. The issue of unintentional cadmium content in mineral fertilizers is the first of these substances that will be addressed by the Commission. 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 his representative wanting to include a new type of fertilizer into Annex I in order to apply to a fertilizer the marking "EC FERTILIZER". This procedure should include the submission of a technical file to a Member State authority which will act as rapporteur for the file.

(17) Since the measures necessary for the implementation of this Regulation are measures of general scope within the meaning of Article 2 of Council Decision 1999/468/EC of 28 June 1999 laying down the procedures for the exercise of implementing powers conferred on the Commission [14], they should be adopted by use of the regulatory procedure provided for in Article 5 of that Decision.

[14] OJ L 184, 17.7.1999, p. 23.

(18) Member States should lay down penalties in respect of infringements to the provisions of this Regulation,

HAVE ADOPTED THIS REGULATION:

TItLE I General provisions

Chapter I Scope and Definitions

Article 1

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

Article 2

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

(a) Fertilizer 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 small compared to those of primary and secondary nutrients.

(e) Inorganic fertilizer means a fertilizer in which the declared nutrients are in the form of minerals obtained by physical and/or chemical industrial processes. Calcium cyanamide, urea and its condensation and association products may, by convention, be classed as inorganic fertilizers.

(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 fertilizers means fertilizers with a common type designation as indicated in Annex I.

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

(j) Compound fertilizer means a fertilizer 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 fertilizer means a compound fertilizer, 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 Fertilizer means a fertilizer obtained by dry mixing of several fertilizers, with no chemical reaction.

(m) Foliar fertilizer means a fertilizer designed for application to and nutrient uptake by the foliage of a crop.

(n) Fluid fertilizer means fertilizers in suspension or solution.

(o) Solution fertilizer means a fluid fertilizer, that is free of solid particles.

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

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

(r) Declarable content means the content of a nutrient, or its oxide, which according to Community legislation, may or shall be given on a label or document associated with an EC fertilizer.

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

(t) Harmonised 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 fertilizers and holding not more than 1 000 kg.

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

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

(x) Manufacturer means the natural or legal person, including importers, placing a fertilizer on the market.

Chapter ii Placing on the market

Article 3

A fertilizer belonging to a type of fertilizers listed in Annex I and which complies with the conditions laid down in this Regulation, may be designated "EC fertilizer".

The manufacturer shall not use the designation "EC fertilizer" for fertilizers that do not comply with this Regulation.

Article 4

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

Article 5

1. Without prejudice to the provisions of Article 15 and of 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 fertilizers marked "EC fertilizer" which comply with the provisions of this Regulation.

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

Article 6

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 fertilizers placed on their market is to be expressed in the following way:

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

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

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

(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 read as being in elemental form and the numerical values 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 fertilizers and, where the conditions of Article 17 are fulfilled, of primary nutrient fertilizers placed on their markets are to be expressed:

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

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

(c) or 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. The Member States cannot prevent a manufacturer from choosing to label an "EC fertilizer" in both of the forms mentioned in paragraphs 1 and 2 respectively.

4. The content of one or more of the micro-nutrients boron, cobalt, copper, iron, manganese, molybdenum, or zinc in the EC fertilizers belonging to the types of fertilizers 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 fertilizer 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 fertilizers belonging to the types of fertilizers 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 fertilizers 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 fertilizers belonging to the types of fertilizers listed in sections A, B, C and D of Annex I by indicating:

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

(ii) the water-soluble content, expressed as a percentage of the fertilizer 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 present in the fertilizer 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

1. Manufacturers shall provide EC fertilizers with the identification markings listed in Article 9.

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

Article 8

Member States may require on their territory without impeding trade and under the responsibility of the manufacturer, that an indication be given of the dose rates and conditions of use suitable for the soil and crop conditions under which the fertilizer is used. This information must be clearly separated from the compulsory indications provided for in Articles 9, 19, 21 and 23.

Article 9

1. Without prejudice to other Community rules, the only statutory markings relating to fertilizers and permitted on the packages, labels and accompanying documents referred to in Article 7 shall be the following indications:

(a) Compulsory identification

- The words "EC FERTILIZER" in capital letters;

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

- Quantities of fluid fertilizers, expressed by mass. The expression of quantities of fluid fertilizers 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 fertilizers;

- If the gross mass/volume is given, the tare mass/volume must be indicated beside it;

- The name or trade name or trade mark and the address of the manufacturer;

- For blended fertilizers the marking "blend" after the designation of the type.

(b) Optional identification

- As listed in Annex I;

- The specific directions for the use, storage, and handling of the fertilizer;

- The manufacturer's own mark, the trademark of the product and the trade description of the product.

The characteristics 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 fertilizers may be placed on the market only if suitable additional instructions are provided by the manufacturer. These instructions shall cover, in particular, storage temperature and prevention of accidents during storage.

Article 10

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

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

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

Article 11

Member States may require that on their territory the label, the markings on the package and the accompanying documents shall appear in at least their national language or languages.

Article 12

In the case of packaged EC fertilizers, 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

1. The declared contents of nutrients of EC fertilizers shall comply with the tolerance limits established in Annex II.

2. A 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

A type of fertilizer shall only be included into Annex I if:

(a) Under normal conditions of use it does not adversely affect human, animal, or plant health, or the environment;

(b) It provides nutrients in an effective manner;

(c) Relevant sampling, analysis, and if required, test methods are being provided.

Article 15

1. Where a Member State has justifiable grounds for believing that a specific EC fertilizer, although satisfying the requirements of this Regulation, constitutes a risk to safety or health of humans or of animals or a risk to the environment, it may temporarily prohibit the placing on the market of that fertilizer 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, within six weeks from the receipt of the information, consult the Member States and if appropriate shall without undue delay consult the relevant technical or scientific committee of the Commission. The Commission shall inform the Member States about the conclusions of the said committee.

3. After consultation of the Member States, or if appropriate of the relevant technical or scientific committee of the Commission, a decision shall be taken on the matter within 90 days in accordance with the procedure referred to in Article 32(2).

4. The provisions of this Regulation shall not preclude the taking of measures which are justified on grounds of public security to prohibit, restrict or hinder the placing on the market of EC fertilizers.

Title II provisions for specific types of fertilizers

Chapter I Inorganic primary nutrient fertilizers

Article 16

This chapter shall apply to inorganic primary nutrient fertilizers, solid or fluid, straight or compound, including those containing secondary nutrients 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

1. A declaration of the calcium, magnesium, sodium and sulphur content as secondary nutrient content of the EC fertilizers belonging to the types of fertilizers listed in sections A, B and C of Annex I may be made, provided that the EC fertilizer continues to satisfy the requirements set out in those sections and 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.

2. Unless otherwise specified in Annex I a declaration of the calcium content shall only be made if it is soluble in water.

Article 18

The declaration of the calcium, magnesium, sodium and sulphur content of the fertilizers 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 fertilizer by mass;

(b) the total content and the content soluble in water, expressed as a percentage of the fertilizer 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.

Article 19

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

2. The designation of the type of fertilizer shall be stated, in accordance with Annex I with, in brackets and immediately following the chemical symbols of the primary nutrients, the chemical symbols of the declared secondary nutrients, which the fertilizer contains.

The nutrient content shall be given by:

(i) numbers indicating the primary nutrient content which, for compound fertilizers, should be in the order laid down by the said designation;

(ii) numbers, in brackets, indicating the contents for the declared secondary nutrients followed:

- by the words "with micro-nutrients" if there is a declared content of micro-nutrients, or

- by the word "with" followed by the name or names of the micro-nutrients present or by their chemical symbols.

Only numbers stating the contents of primary and secondary nutrients shall follow the type designation.

3. The declared content of primary nutrients and secondary nutrients shall be given as a percentage by mass, as whole numbers or, where necessary, to one decimal place.

For compound fertilizers 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 be given as a percentage by mass as specified in sections E.2.2 and E.2.3 of Annex I.

4. The forms and solubility of the nutrients shall also be expressed as a percentage by mass of fertilizer, 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 fertilizers

Article 20

This chapter shall apply to inorganic secondary nutrient fertilizers, 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

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

2. The designation of the type of fertilizer shall be stated in accordance with section D of Annex I.

The nutrient content shall be given by numbers indicating the contents of the declared secondary nutrients followed:

(i) by the words "with micro-nutrients" if there is a declared content of micro-nutrients, or

(ii) by the word "with" followed by the name or names of the micro-nutrients present or by their chemical symbols.

Only numbers stating the contents of secondary nutrients shall follow the type designation.

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

For compound fertilizers 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 be given as a percentage by mass as specified in sections E.2.2 and E.2.3 of Annex I.

4. The forms and solubility of the nutrients shall also be expressed as a percentage by mass of fertilizer, 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 III Inorganic micro-nutrient fertilizers

Article 22

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

Article 23

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. The designation of the type of fertilizer shall be stated:

(a) either in accordance with section E.1 of Annex I, or

(b) as the type designation "mixture of micro-nutrients", followed by the names of the micro-nutrients present or their chemical symbols.

3. The declared micro-nutrient content shall be given as a percentage by mass, in whole numbers or, where necessary, to one decimal places for fertilizers containing only one micro-nutrient shown in section E.1 of Annex I.

Where fertilizers contain several micro-nutrients, the number of decimal places may, for a given element, be as set out in section E.2.1 of Annex I.

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

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

5. Below the obligatory or optional declarations the following shall be entered on the label and accompanying papers 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

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

Chapter IV Ammonium nitrate fertilizers of high nitrogen content

Article 25

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

This type of fertilizer may contain inorganic or inert substances.

Any substances that are used in the manufacturing of this type of fertilizers, must not increase its sensitivity to heat or its tendency to detonate.

Article 26

1. Manufacturers shall ensure that straight ammonium nitrate fertilizers 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 fertilizers 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.

Article 27

1. Without prejudice to the measures referred to in Article 26, Member States may require additional checks on ammonium nitrate EC fertilizers of high nitrogen content. Such checks may be carried out either before the fertilizers are placed on the market within their territories, or after marketing, or at both stages .

For these checks, only the test described in section 2 of Annex III shall be used.

2. EC fertilizers which satisfy the requirements of this chapter and, where required by the Member State, the test of resistance to detonation described in section 3 (Method 1, point 3) and 4 of Annex III, shall not be subject to national rules which apply to less safe fertilizers and their storage.

Article 28

Straight ammonium nitrate fertilizers of high nitrogen content shall be made available to the final user only in packaged form.

Title III conformity assessment of fertilizers

Article 29

1. Member States may subject fertilizers placed on the market with the marking "EC FERTILIZER" to official control measures, for the purpose of verifying that they comply with this Regulation. These control measures shall not oblige manufacturers to repeat tests made by laboratories fulfilling the conditions of Article 30 in so far as these tests have shown compliance of the fertilizer in question.

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

3. Compliance with this Regulation in respect of conformity to types of fertilizer 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 IV and taking into account the tolerances specified in Annex II.

4. Adaptation to technical progress of sampling and analysis methods shall follow the procedure referred to in Article 32(2), and shall, wherever possible, use Harmonised European Standards.

Article 30

1. Member States shall notify to the Commission those laboratories on their territories that are competent and authorised to provide the necessary services for checking compliance of EC fertilizers with the requirements of this Regulation

2. Member States shall demonstrate the competence of the notified laboratories referred to under Paragraph 1 either by accreditation, according to the standards mentioned in Annex V, or by certifying them to comply with the requirements of Council Directive 87/18/EEC [15].

[15] OJ L 15, 17.1. 1987, p. 29.

3. The Commission shall publish the list of notified laboratories in the Official Journal of the European Communities.

4. Where a Member State has justifiable grounds for believing that a notified laboratory does not possess the competence referred to in Paragraph 2 of this article, it shall raise this matter in the committee referred to in Article 32(1). Article 15(2) shall apply mutatis mutandis.

Title IV FINAL provisions

Chapter I Adaptation of the annexes

Article 31

1. The inclusion of a new type of fertilizer into Annex I of this Regulation shall be adopted in accordance with the procedure referred to in Article 32(2). This procedure requires the submission of a technical file to a Member State authority which will act as rapporteur for the file to the committee referred to in Article 32(1).

2. A manufacturer or its representative wanting to propose a new type of fertilizer to be added to Annex I and to this effect needs to compile a technical file, shall do so by taking into account the technical documents referred to in 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

1. The Commission shall be assisted by a committee, composed of representatives of the Member States and chaired by the representative of the Commission.

2. Where reference is made to this paragraph, the regulatory procedure laid down in Article 5 of Decision 1999/468/EC shall apply, in compliance with Article 7 and Article 8 thereof.

3. The period provided for in Article 5(6) of Decision 1999/468/EC shall be three months.

Chapter II Transitional provisions

Article 33

1. By way of derogation from Article 5, Austria, Finland and Sweden may prohibit the placing on the market on their territory of EC fertilizers containing cadmium at concentrations in excess of those which were fixed nationally at the date of Accession until 31 December 2004.

2. The Commission shall, in consultation with Member States and interested parties, review by 30 June 2002 at the latest the need for establishing provisions at Community level concerning the cadmium content of fertilizers.

Article 34

1. Without prejudice to the provisions of Article 30(2), Member States may, for a transitional period until 31 December 2006 continue to apply their national provisions for authorising competent laboratories to provide the necessary services for checking compliance of EC fertilizers with the requirements of this Regulation.

2. Member States shall notify these laboratories to the Commission, giving details of their authorisation scheme.

Chapter III Final provisions

Article 35

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

Article 36

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. The Member States shall notify those provisions to the Commission by 31 December 2003 at the latest and shall notify it without delay of any subsequent amendment affecting them.

Article 37

By 31 December 2006 at the latest, the Commission will review the way in which declarations have to be made under Article 6 with a view to proposing a single coherent system of declarations throughout the Community.

Article 38

This Regulation shall enter into force on the sixtieth day following that of its publication in the Official Journal of the European Communities.

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

Done at Brussels,

For the European Parliament For the Council

The President The President

ANNEX I List of types of EC fertilizers

A. Inorganic straight primary nutrient fertilizers

A.1. Nitrogenous fertilizers

>TABLE POSITION>

A.2. Phosphatic fertilizers

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

>TABLE POSITION>

A.3. Potassic fertilizers

>TABLE POSITION>

B. Inorganic compound primary nutrient fertilizers

B.1. NPK fertilizers

>TABLE POSITION>

>TABLE POSITION>

B.1. NPK fertilizer (continued)

>TABLE POSITION>

>TABLE POSITION>

B.2. NP fertilizers

>TABLE POSITION>

>TABLE POSITION>

B.2. NP fertilizers(continued)

>TABLE POSITION>

B.3. NK fertilizers

>TABLE POSITION>

>TABLE POSITION>

B.3. NK fertilizers (continued)

>TABLE POSITION>

>TABLE POSITION>

B.4. PK fertilizers

>TABLE POSITION>

>TABLE POSITION>

C. Inorganic fluid fertilizers

C.1. Straight fluid fertilizers

>TABLE POSITION>

C.2. Compound fluid fertilizers

>TABLE POSITION>

>TABLE POSITION>

C.2. Compound fluid fertilizers (continued)

>TABLE POSITION>

>TABLE POSITION>

C.2. Compound fluid fertilizers (continued)

>TABLE POSITION>

>TABLE POSITION>

C.2. Compound fluid fertilizers (continued)

>TABLE POSITION>

>TABLE POSITION>

C.2. Compound fluid fertilizers (continued)

>TABLE POSITION>

>TABLE POSITION>

C.2. Compound fluid fertilizers (continued)

>TABLE POSITION>

>TABLE POSITION>

C.2. Compound fluid fertilizers (continued)

>TABLE POSITION>

>TABLE POSITION>

C.2. Compound fluid fertilizers (continued)

>TABLE POSITION>

>TABLE POSITION>

D. Inorganic secondary nutrient fertilizers

>TABLE POSITION>

E. Inorganic micro-nutrient fertilizers

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. Fertilizers containing only one micro-nutrient

E.1.1. Boron

>TABLE POSITION>

E.1.2. Cobalt

>TABLE POSITION>

E.1.3. Copper

>TABLE POSITION>

E.1.4 Iron

>TABLE POSITION>

E.1.5. Manganese

>TABLE POSITION>

E.1.6. Molybdenum

>TABLE POSITION>

E.1.7. Zinc

>TABLE POSITION>

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

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

>TABLE POSITION>

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

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

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

>TABLE POSITION>

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

>TABLE POSITION>

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

Authorised products

E.3.1. Chelating agents

Sodium, potassium or ammonium acid or salts of:

>TABLE POSITION>

E.3.2. Complexing agents

List to be drawn up

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 fertilizer are as follows:

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

1.1. Nitrogenous fertilizers

>TABLE POSITION>

1.2. Phosphatic fertilizers

>TABLE POSITION>

1.3. Potassic fertilizers

>TABLE POSITION>

1.4. Other components

>TABLE POSITION>

2. INORGANIC COMPOUND PRIMARY NUTRIENT FERTILIZERS

2.1. Nutrient elements

>TABLE POSITION>

2.2. Total negative deviations from the declared value

>TABLE POSITION>

3. SECONDARY NUTRIENTS IN FERTILIZERS

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 FERTILIZERS

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 Fertilizers of High Nitrogen Content

1. CHARACTERISTICS OF AND LIMITS FOR STRAIGHT AMMONIUM NITRATE FERTILIZERS OF HIGH NITROGEN CONTENT

1.1. Porosity (oil retention)

The oil retention of the fertilizer, 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 fertilizers having a nitrogen content of at least 31.5 % by mass and must not exceed 0.4 % for fertilizers having a nitrogen content of at least 28 % but less than 31.5 % by mass.

1.3. pH

A solution of 10 g of fertilizer 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 fertilizer 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 FERTILIZERS OF HIGH NITROGEN CONTENT

The test must be carried out on a representative sample of fertilizer. 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 fertilizer must be subjected to the test of resistance to detonation in a horizontal steel tube under the following conditions:

- seamless steel tube,

- Tube length: 1 000 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 fertilizers of high nitrogen content and of the test on the resistance to detonation for both, straight and compound ammonium nitrate fertilizer 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 fertilizer.

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 fertilizers 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 fertilizer. 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

>REFERENCE TO A GRAPHIC>

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 fertilizers of high nitrogen content.

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

2. Definition

Oil retention of a fertilizer: the quantity of oil retained by the fertilizer 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 2,00 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:

>TABLE POSITION>

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 fertilizers 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 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 [16]. 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.

[16] 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.

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:

>TABLE POSITION>

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

>REFERENCE TO A GRAPHIC>

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 fertilizer 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 1 000-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 1 000-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 fertilizers 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 fertilizers 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 ((1E) of the potential E. In a fourth column, record the differences ((2E) positive or negative, between the potential increments ((1E). 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 (1E.

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

>TABLE POSITION>

where:

V0 is the total volume, in ml, of the silver nitrate solution immediately lower than the volume which gives the maximum increment of (1E,

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 (2E,

B is the sum of the absolute values of the last positive values of (2E and the first negative value of (2E (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:

V4 = 2V3 - V2

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 serves 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:

>TABLE POSITION>

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 POSITION>

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 fertilizers 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 [17] (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 1 000 µg of copper (Cu).

[17] Commercially available standard copper solution may be used.

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 [18], discarding the first 50 ml.

[18] Whatman 541 or equivalent.

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 fertilizers 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: 1 500 to 1 600 kg/m3

Detonation velocity: 7 300 to 7 700 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: 1 500 to 1 600 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: 1 005 (± 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 1 000 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 cm 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