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

• Published date: 22 August 1977
• Official Gazette Publication: Official Journal of the European Communities, L 213, 22 August 1977

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31977L0535

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

Official Journal L 213 , 22/08/1977 P. 0001 - 0090
Finnish special edition: Chapter 13 Volume 7 P. 0051
Greek special edition: Chapter 13 Volume 6 P. 0052
Swedish special edition: Chapter 13 Volume 7 P. 0051
Spanish special edition: Chapter 13 Volume 7 P. 0063
Portuguese special edition Chapter 13 Volume 7 P. 0063

COMMISSION DIRECTIVE of 22 June 1977 on the approximation of the laws of the Member States relating to methods of sampling and analysis for fertilizers (77/535/EEC)

THE COMMISSION OF THE EUROPEAN COMMUNITIES,

Having regard to the Treaty establishing the European Economic Community,

Having regard to Council Directive 76/116/EEC of 18 December 1975 on the approximation of the laws of the Member States relating to fertilizers (1), and in particular Article 9 (2) thereof,

Whereas that Directive provides for official controls for EEC fertilizers for the purpose of checking compliance with requirements arising under the Community provisions concerning the quality and composition of fertilizers;

Whereas the measures provided for in this Directive are in accordance with the Opinion of the Committee on the Adaptation to Technical Progress of the Directives for the Removal of Technical Barriers to Trade in Fertilizers,

HAS ADOPTED THIS DIRECTIVE:

Article 1

The Member States shall take the necessary measures to ensure that sampling and analyses for official controls of EEC fertilizers pursuant to Article 8 (1) and (2) of Council Directive 76/116/EEC of 18 December 1975 are carried out in accordance with the methods described in the Annex to this Directive.

Article 2

1. The Member States shall, not later than 19 December 1977, bring into force the laws, regulations or administrative provisions necessary to comply with this Directive. They shall forthwith notify the Commission thereof.

2. The Member States shall ensure that the texts of the provisions of national law which they adopt in the field covered by this Directive are communicated to the Commission.

Article 3

This Directive is addressed to the Member States.

Done at Brussels, 22 June 1977.

For the Commission

Étienne DAVIGNON

Member of the Commission (1)OJ No L 24, 30.1.1976, p. 21.

ANNEX I METHOD OF SAMPLING FOR THE CONTROL OF FERTILIZERS

INTRODUCTION

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

The sampling method described below must be applied with strict accuracy by specialists with experience of the conventional sampling procedure. 1. PURPOSE AND SCOPE

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

2. SAMPLING OFFICERS

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

3. DEFINITIONS

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

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

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

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

Final sample : A representative part of the reduced sample.

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

4.2. Apparatus recommended for the sampling of solid fertilizers 4.2.1. Manual sampling 4.2.1.1. Flat-bottomed shovel with vertical sides.

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

4.2.2. Mechanical sampling

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

4.2.3. Divider

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

5. QUANTITATIVE REQUIREMENTS 5.1. Sampled portion

The size of the sampled portion must be such that each of its constituent parts can be sampled. >PIC FILE= "T0010881">

6. INSTRUCTIONS FOR TAKING, PREPARING AND PACKAGING THE SAMPLES 6.1. General

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

6.2. Incremental samples

Incremental samples must be taken at random throughout the whole sampled portion and they must be of approximately equal sizes. 6.2.1. Loose fertilizers

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

6.2.2. Packaged fertilizers

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

6.3. Preparation of aggregate sample

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

6.4. Preparation of the final sample

The material in the aggregate sample shall be carefully mixed (1).

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

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

7. PACKAGING OF FINAL SAMPLES

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

8. SAMPLING RECORD

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

9. DESTINATION OF SAMPLES

For each sample portion at least one final sample shall be sent as quickly as possible to an authorized analytical laboratory, together with the information necessary for the analyst. (1)Any lumps shall be broken up (if necessary by separating them out and returning them to the sample).

ANNEX II

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GENERAL OBSERVATIONS

Laboratory equipment

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

Control tests

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

Method 1 PREPARATION OF THE SAMPLE FOR ANALYSIS

1. SCOPE

This document defines the procedure for the preparation of the sample for analysis, taken from the final sample.

2. PRINCIPLE

The preparation of a final sample received at the laboratory is a series of operations, usually sieving, grinding and mixing, carried out in such a way that: - on the one hand, the smallest amount weighed out laid down by the methods of analysis is representative of the laboratory sample,

- on the other hand, the fineness of the fertilizer cannot have been changed by the preparation to the extent that its solubility in the various extraction reagents is appreciably affected.

3. APPARATUS

Sample divider (optional).

Sieves with apertus of 0 72 and 0 75 mm.

250-ml flasks, stoppered.

Porcelain pestle and mortar or grinder.

4. CHOICE OF TREATMENT TO BE USED

Preliminary remark

If the product is suitable, only a representative part of the final sample need be kept. 4.1. Final samples which must not be ground

Calcium nitrate, calcium magnesium nitrate, sodium nitrate, Chile nitrate, calcium cyanamide, nitrogenous calcium cyanamide, ammonium sulphate, ammonium nitrates of over 30 % N, urea, basic slag, natural phosphate rendered partially soluble, precipitated dihydrated...