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Commission Directive 81/680/EEC of 30 July 1981 amending Directives 71/250/EEC, 71/393/EEC, 72/199/EEC, 73/46/EEC, 74/203/EEC, 75/84/EEC, 76/372/EEC and 78/633/EEC establishing Community methods of analysis for the official control of feedingstuffs Official Journal L 246 , 29/08/1981 P. 0032 - 0035 Finnish special edition: Chapter 3 Volume 13 P. 0225 Spanish special edition: Chapter 03 Volume 23 P. 0057 Swedish special edition: Chapter 3 Volume 13 P. 0225 Portuguese special edition Chapter 03 Volume 23 P. 0057

COMMISSION DIRECTIVE of 30 July 1981 amending Directives 71/250/EEC, 71/393/EEC, 72/199/EEC, 73/46/EEC, 74/203/EEC, 75/84/EEC, 76/372/EEC and 78/633/EEC establishing Community methods of analysis for the official control of feedingstuffs (81/680/EEC) THE COMMISSION OF THE EUROPEAN COMMUNITIES, Having regard to the Treaty establishing the European Economic Community, Having regard to Council Directive 70/373/EEC of 20 July 1970 on the introduction of Community methods of sampling and analysis for the official control of feedingstuffs (1), as last amended by the Act of Accession of Greece, and in particular Article 2 thereof, Whereas the Annex to the First Commission Directive 71/250/EEC of 15 June 1971 establishing Community methods of analysis for the official control of feedingstuffs (2) sets out the general rules for applying the methods of analysis described in that Directive and in Commission Directives 71/393/EEC (3), 72/199/EEC (4), 73/46/EEC (5), 74/203/EEC (6), 75/84/EEC (7), 76/372/EEC (8) and 78/633/EEC (9) establishing Community methods of analysis for the official control of feedingstuffs ; whereas, however, some of the abovementioned Directives provide that those general rules are not to apply to the methods of analysis relating to additives in feedingstuffs; Whereas there is a need to adjust the general rules so that they apply without distinction to the analysis of all the constituents of feedingstuffs ; whereas the provisions of the Directives in question should therefore be amended; Whereas the measures provided for in this Directive are in accordance with the opinion of the Standing Committee for Feedingstuffs, HAS ADOPTED THIS DIRECTIVE: Article 1 First Commission Directive 71/250/EEC is hereby amended as follows: 1. The following paragraph is added to Article 1: "The general rules contained in Part 1 of the Annex shall apply to the methods of analysis adopted pursuant to Council Directive 70/373/EEC." 2. In the Annex, Part 1 "Introduction" is replaced by the Annex to this Directive. Article 2 In Article 1 of Second Commission Directive 71/393/EEC the second paragraph is deleted. Article 3 In Articles 1 and 2 of Third Commission Directive 72/199/EEC the second paragraph is deleted. Article 4 In Articles 1 and 2 of Fourth Commission Directive 73/46/EEC the second paragraph is deleted. Article 5 In Articles 1 and 2 of Fifth Commission Directive 74/203/EEC the second paragraph is deleted. Article 6 In Article 1 of Sixth Commission Directive 75/84/EEC the second paragraph is deleted. Article 7 In Article 1 of Seventh Commission Directive 76/372/EEC the second paragraph is deleted. Article 8 In Article 1 of Eighth Commission Directive 78/633/EEC the second paragraph is deleted. (1) OJ No L 170, 3.8.1970, p. 2. (2) OJ No L 155, 12.7.1971, p. 13. (3) OJ No L 279, 20.12.1971, p. 7. (4) OJ No L 123, 29.5.1972, p. 6. (5) OJ No L 83, 30.3.1973, p. 21. (6) OJ No L 108, 22.4.1974, p. 7. (7) OJ No L 32, 5.2.1975, p. 26. (8) OJ No L 102, 15.4.1976, p. 8. (9) OJ No L 206, 29.7.1978, p. 43. Article 9 The Member States shall bring into force the laws, regulations or administrative provisions necessary to comply with this Directive on 1 December 1981 and shall forthwith inform the Commission thereof. Article 10 This Directive is addressed to the Member States. Done at Brussels, 30 July 1981. For the Commission The President Gaston THORN ANNEX "ANNEX 1. GENERAL PROVISIONS ON METHODS OF ANALYSIS FOR FEEDINGSTUFFS A. PREPARATION OF SAMPLES FOR ANALYSIS 1. Purpose The procedures described below concern the preparation for analysis of final samples, sent to the control laboratories after sampling in accordance with the provisions laid down by First Commission Directive 76/371/EEC of 1 March 1976 establishing Community methods of sampling for the official control of feedingstuffs (1). These samples must be prepared in such a way that the amounts weighed out, as provided for in the methods of analysis, are homogeneous and representative of the final samples. 2. Precautions to be taken All the necessary operations must be performed in such a way as to avoid as far as possible contamination of the sample and changes of its composition. Grinding, mixing and sieving should be carried out as quickly as possible with minimal exposure of the sample to the air and light. Mills and grinders likely to appreciably heat the sample should not be used. Manual grinding is recommended for feedingstuffs which are particularly sensitive to heat. Care should also be taken to ensure that the apparatus itself is not a source of contamination of trace elements. If the preparation cannot be carried out without significant changes in the moisture content of the sample, determine the moisture content before and after preparation according to the method laid down in Part 1 of the Annex to Second Commission Directive 71/393/EEC of 18 November 1971 establishing Community methods of analysis for the official control of feedingstuffs (2), as amended by Commission Directive 73/47/EEC of 5 December 1972 (3). 3. Procedure Mix thoroughly the final sample either mechanically or manually. Divide the sample into two equal portions (the quartering method should be used where applicable). Keep one of the portions in a suitable clean, dry container, fitted with an air-tight stopper, and prepare the other portion or a representative part of it, of at least 100 g, as indicated below. 3.1. Feedingstuffs which can be ground as such Unless otherwise specified in the methods of analysis, sieve the whole sample through a sieve with a square mesh of 1 mm side (in accordance with recommendation ISO R565) after grinding, if necessary. Avoid any overgrinding. Mix the sieved sample and collect it in a suitable clean, dry container fitted with an air-tight stopper. Mix again, immediately before weighing out the amount for analysis. 3.2. Feedingstuffs which can be ground after drying Unless otherwise specified in the methods of analysis, dry the sample to bring its moisture content down to a level of 8 to 12 %, according to the preliminary drying procedure described under point 4.3 of the method of determination of moisture mentioned in section 2 above. Then proceed as indicated in section 3.1. (1) OJ No L 102, 15.4.1976, p. 1. (2) OJ No L 279, 20.12.1971, p. 7. (3) OJ No L 83, 30.3.1973, p. 35. 3.3. Liquid or semi-liquid feedingstuffs Collect the sample in a suitable clean, dry container, fitted with an air-tight stopper. Mix thoroughly immediately before weighing out the amount for analysis. 3.4. Other feedingstuffs Samples which cannot be prepared according to one of the above procedures should be treated by any other procedure which ensures that the amounts weighed out for the analysis are homogeneous and representative of the final samples. 4. Storage of samples Samples must be stored at a temperature that will not alter their composition. Samples intended for the analysis of vitamins or substances which are particularly sensitive to light should be stored in brown glass containers. B. PROVISIONS RELATING TO REAGENTS AND APPARATUS USED IN METHODS OF ANALYSIS 1. Unless otherwise specified in the methods of analysis, all analytical reagents must be analytically pure (a.p.). When determining trace elements, the purity of the reagents must be checked by a blank test. Depending upon the results obtained, further purification of the reagents may be required. 2. Any operation involving preparation of solutions, dilution, rinsing or washing, mentioned in the methods of analysis without indication as to the nature of the solvent or diluent employed, implies that water must be used. As a general rule, water should be demineralized or distilled. In particular cases, which are indicated in the methods of analysis, it must be submitted to special procedures of purification. 3. In view of the equipment normally found in control laboratories, only those instruments and apparatus which are special or require specific usage are referred to in the methods of analysis. They must be clean, especially when very small amounts of substances have to be determinded. C. APPLICATION OF METHODS OF ANALYSIS AND EXPRESSION OF THE RESULTS 1. In general a single method of analysis is established for the determination of each substance in feedingstuffs. Where several methods are given, the particular method used by the control laboratory must be indicated on the analysis report. 2. The result given in the analysis report shall be the average value obtained from at least two determinations, carried out on separate portions of the sample, and of satisfactory repeatability. This result shall be expressed in the manner laid down in the method of analysis to an appropriate number of significant figures and shall be corrected, if necessary, to the moisture content of the final sample prior to preparation.

COMMISSION DIRECTIVE of 30 July 1981 amending Directives 71/250/EEC, 71/393/EEC, 72/199/EEC, 73/46/EEC, 74/203/EEC, 75/84/EEC, 76/372/EEC and 78/633/EEC establishing Community methods of analysis for the official control of feedingstuffs (81/680/EEC)

THE COMMISSION OF THE EUROPEAN COMMUNITIES,

Having regard to the Treaty establishing the European Economic Community,

Having regard to Council Directive 70/373/EEC of 20 July 1970 on the introduction of Community methods of sampling and analysis for the official control of feedingstuffs (1), as last amended by the Act of Accession of Greece, and in particular Article 2 thereof,

Whereas the Annex to the First Commission Directive 71/250/EEC of 15 June 1971 establishing Community methods of analysis for the official control of feedingstuffs (2) sets out the general rules for applying the methods of analysis described in that Directive and in Commission Directives 71/393/EEC (3), 72/199/EEC (4), 73/46/EEC (5), 74/203/EEC (6), 75/84/EEC (7), 76/372/EEC (8) and 78/633/EEC (9) establishing Community methods of analysis for the official control of feedingstuffs ; whereas, however, some of the abovementioned Directives provide that those general rules are not to apply to the methods of analysis relating to additives in feedingstuffs;

Whereas there is a need to adjust the general rules so that they apply without distinction to the analysis of all the constituents of feedingstuffs ; whereas the provisions of the Directives in question should therefore be amended;

Whereas the measures provided for in this Directive are in accordance with the opinion of the Standing Committee for Feedingstuffs,

HAS ADOPTED THIS DIRECTIVE:

First Commission Directive 71/250/EEC is hereby amended as follows: 1. The following paragraph is added to Article 1:

"The general rules contained in Part 1 of the Annex shall apply to the methods of analysis adopted pursuant to Council Directive 70/373/EEC."

2. In the Annex, Part 1 "Introduction" is replaced by the Annex to this Directive.

Article 2

In Article 1 of Second Commission Directive 71/393/EEC the second paragraph is deleted.

Article 3

In Articles 1 and 2 of Third Commission Directive 72/199/EEC the second paragraph is deleted.

Article 4

In Articles 1 and 2 of Fourth Commission Directive 73/46/EEC the second paragraph is deleted.

Article 5

In Articles 1 and 2 of Fifth Commission Directive 74/203/EEC the second paragraph is deleted.

Article 6

In Article 1 of Sixth Commission Directive 75/84/EEC the second paragraph is deleted.

Article 7

In Article 1 of Seventh Commission Directive 76/372/EEC the second paragraph is deleted.

Article 8

In Article 1 of Eighth Commission Directive 78/633/EEC the second paragraph is deleted.

(1) OJ No L 170, 3.8.1970, p. 2. (2) OJ No L 155, 12.7.1971, p. 13. (3) OJ No L 279, 20.12.1971, p. 7. (4) OJ No L 123, 29.5.1972, p. 6. (5) OJ No L 83, 30.3.1973, p. 21. (6) OJ No L 108, 22.4.1974, p. 7. (7) OJ No L 32, 5.2.1975, p. 26. (8) OJ No L 102, 15.4.1976, p. 8. (9) OJ No L 206, 29.7.1978, p. 43.

Article 9

The Member States shall bring into force the laws, regulations or administrative provisions necessary to comply with this Directive on 1 December 1981 and shall forthwith inform the Commission thereof.

Article 10

This Directive is addressed to the Member States.

Done at Brussels, 30 July 1981.

For the Commission

The President

Gaston THORN

ANNEX

"ANNEX 1. GENERAL PROVISIONS ON METHODS OF ANALYSIS FOR FEEDINGSTUFFS

A. PREPARATION OF SAMPLES FOR ANALYSIS

1. Purpose

The procedures described below concern the preparation for analysis of final samples, sent to the control laboratories after sampling in accordance with the provisions laid down by First Commission Directive 76/371/EEC of 1 March 1976 establishing Community methods of sampling for the official control of feedingstuffs (1).

These samples must be prepared in such a way that the amounts weighed out, as provided for in the methods of analysis, are homogeneous and representative of the final samples.

2. Precautions to be taken

All the necessary operations must be performed in such a way as to avoid as far as possible contamination of the sample and changes of its composition. Grinding, mixing and sieving should be carried out as quickly as possible with minimal exposure of the sample to the air and light. Mills and grinders likely to appreciably heat the sample should not be used. Manual grinding is recommended for feedingstuffs which are particularly sensitive to heat. Care should also be taken to ensure that the apparatus itself is not a source of contamination of trace elements.

If the preparation cannot be carried out without significant changes in the moisture content of the sample, determine the moisture content before and after preparation according to the method laid down in Part 1 of the Annex to Second Commission Directive 71/393/EEC of 18 November 1971 establishing Community methods of analysis for the official control of feedingstuffs (2), as amended by Commission Directive 73/47/EEC of 5 December 1972 (3).

3. Procedure

Mix thoroughly the final sample either mechanically or manually. Divide the sample into two equal portions (the quartering method should be used where applicable). Keep one of the portions in a suitable clean, dry container, fitted with an air-tight stopper, and prepare the other portion or a representative part of it, of at least 100 g, as indicated below. 3.1. Feedingstuffs which can be ground as such

Unless otherwise specified in the methods of analysis, sieve the whole sample through a sieve with a square mesh of 1 mm side (in accordance with recommendation ISO R565) after grinding, if necessary. Avoid any overgrinding.

Mix the sieved sample and collect it in a suitable clean, dry container fitted with an air-tight stopper. Mix again, immediately before weighing out the amount for analysis.

3.2. Feedingstuffs which can be ground after drying

Unless otherwise specified in the methods of analysis, dry the sample to bring its moisture content down to a level of 8 to 12 %, according to the preliminary drying procedure described under point 4.3 of the method of determination of moisture mentioned in section 2 above. Then proceed as indicated in section 3.1.

(1) OJ No L 102, 15.4.1976, p. 1. (2) OJ No L 279, 20.12.1971, p. 7. (3) OJ No L 83, 30.3.1973, p. 35. 3.3. Liquid or semi-liquid feedingstuffs

Collect the sample in a suitable clean, dry container, fitted with an air-tight stopper. Mix thoroughly immediately before weighing out the amount for analysis.

3.4. Other feedingstuffs

Samples which cannot be prepared according to one of the above procedures should be treated by any other procedure which ensures that the amounts weighed out for the analysis are homogeneous and representative of the final samples.

4. Storage of samples

Samples must be stored at a temperature that will not alter their composition. Samples intended for the analysis of vitamins or substances which are particularly sensitive to light should be stored in brown glass containers.

B. PROVISIONS RELATING TO REAGENTS AND APPARATUS USED IN METHODS OF ANALYSIS

1. Unless otherwise specified in the methods of analysis, all analytical reagents must be analytically pure (a.p.). When determining trace elements, the purity of the reagents must be checked by a blank test. Depending upon the results obtained, further purification of the reagents may be required.

2. Any operation involving preparation of solutions, dilution, rinsing or washing, mentioned in the methods of analysis without indication as to the nature of the solvent or diluent employed, implies that water must be used. As a general rule, water should be demineralized or distilled. In particular cases, which are indicated in the methods of analysis, it must be submitted to special procedures of purification.

3. In view of the equipment normally found in control laboratories, only those instruments and apparatus which are special or require specific usage are referred to in the methods of analysis. They must be clean, especially when very small amounts of substances have to be determinded.

C. APPLICATION OF METHODS OF ANALYSIS AND EXPRESSION OF THE RESULTS

1. In general a single method of analysis is established for the determination of each substance in feedingstuffs. Where several methods are given, the particular method used by the control laboratory must be indicated on the analysis report.

2. The result given in the analysis report shall be the average value obtained from at least two determinations, carried out on separate portions of the sample, and of satisfactory repeatability.

This result shall be expressed in the manner laid down in the method of analysis to an appropriate number of significant figures and shall be corrected, if necessary, to the moisture content of the final sample prior to preparation.