Official Journal L 221. of the European Communities. Legislation. Volume August Contents. Acts whose publication is not obligatory

Transcription

1 Official Journal of the European Communities ISSN L 221 Volume August 2002 English edition Legislation Contents I Acts whose publication is obligatory Commission Regulation (EC) No 1481/2002 of 16 August 2002 establishing the standard import values for determining the entry price of certain fruit and vegetables... 1 Commission Regulation (EC) No 1482/2002 of 16 August 2002 amending Regulations (EC) No 1938/2001, (EC) No 1939/2001 and (EC) No 1940/2001 on the opening of standing invitations to tender for the resale on the Community internal market of rice held by the Spanish, Greek and Italian intervention agencies for use in animal feed... 3 Commission Regulation (EC) No 1483/2002 of 16 August 2002 suspending the buying-in of butter in certain Member States... 4 Commission Regulation (EC) No 1484/2002 of 16 August 2002 amending the import duties in the cereals sector... 5 II Acts whose publication is not obligatory Commission 2002/657/EC: Commission Decision of 12 August 2002 implementing Council Directive 96/ 23/EC concerning the performance of analytical methods and the interpretation of results ( 1 ) (notified under document number C(2002) 3044) /658/EC: Commission Decision of 14 August 2002 allowing Member States to extend provisional authorisations granted for the new active substances benzoic acid, carvone, mepanipyrim, oxadiargyl and trifloxystrobin ( 1 ) (notified under document number C(2002) 3048) ( 1 ) Text with EEA relevance EN Acts whose titles are printed in light type are those relating to day-to-day management of agricultural matters, and are generally valid for a limited period. The titles of all other acts are printed in bold type and preceded by an asterisk.

2 EN L 221/1 I (Acts whose publication is obligatory) COMMISSION REGULATION (EC) No 1481/2002 of 16 August 2002 establishing the standard import values for determining the entry price of certain fruit and vegetables THE COMMISSION OF THE EUROPEAN COMMUNITIES, Having regard to the Treaty establishing the European Community, Having regard to Commission Regulation (EC) No 3223/94 of 21 December 1994 on detailed rules for the application of the import arrangements for fruit and vegetables ( 1 ), as last amended by Regulation (EC) No 1498/98 ( 2 ), and in particular Article 4(1) thereof, Whereas: (1) Regulation (EC) No 3223/94 lays down, pursuant to the outcome of the Uruguay Round multilateral trade negotiations, the criteria whereby the Commission fixes the standard values for imports from third countries, in respect of the products and periods stipulated in the Annex thereto. (2) In compliance with the above criteria, the standard import values must be fixed at the levels set out in the Annex to this Regulation, HAS ADOPTED THIS REGULATION: Article 1 The standard import values referred to in Article 4 of Regulation (EC) No 3223/94 shall be fixed as indicated in the Annex hereto. Article 2 This Regulation shall enter into force on 17 August This Regulation shall be binding in its entirety and directly applicable in all Member States. Done at Brussels, 16 August For the Commission J. M. SILVA RODRÍGUEZ Agriculture Director-General ( 1 ) OJ L 337, , p. 66. ( 2 ) OJ L 198, , p. 4.

3 L 221/2 EN ANNEX to the Commission Regulation of 16 August 2002 establishing the standard import values for determining the entry price of certain fruit and vegetables (EUR/100 kg) CN code Third country code ( 1 ) Standard import value , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , ,1 ( 1 ) Country nomenclature as fixed by Commission Regulation (EC) No 2020/2001 (OJ L 273, , p. 6). Code 999 stands for of other origin.

4 EN L 221/3 COMMISSION REGULATION (EC) No 1482/2002 of 16 August 2002 amending Regulations (EC) No 1938/2001, (EC) No 1939/2001 and (EC) No 1940/2001 on the opening of standing invitations to tender for the resale on the Community internal market of rice held by the Spanish, Greek and Italian intervention agencies for use in animal feed THE COMMISSION OF THE EUROPEAN COMMUNITIES, Having regard to the Treaty establishing the European Community, Having regard to Council Regulation (EC) No 3072/95 of 22 December 1995 on the common organisation of the market in rice ( 1 ), as last amended by Commission Regulation (EC) No 411/2002 ( 2 ), and in particular Article 8(b) thereof, Whereas: (1) Commission Regulation (EEC) No 75/91 ( 3 ) lays down the procedures and conditions for the disposal of paddy rice held by intervention agencies. (2) The current tendering procedure has not yet resulted in the disposal of the quantity put up for sale. It is therefore necessary to set a later date for the final partial invitation to tender under Commission Regulations (EC) No 1938/ 2001 ( 4 ), (EC) No 1939/2001 ( 5 ) and (EC) No 1940/ 2001 ( 6 ), as last amended by Regulation (EC) No 1101/ 2002 ( 7 ). (3) The measures provided for in this Regulation are in accordance with the opinion of the Management Committee for Cereals, HAS ADOPTED THIS REGULATION: Article 1 Regulations (EC) No 1938/2001, (EC) No 1939/2001 and (EC) No 1940/2001 are amended as follows: In Article 5(3), the date 28 August 2002 is replaced by 27 November Article 2 This Regulation shall enter into force on the day of its publication in the. This Regulation shall be binding in its entirety and directly applicable in all Member States. Done at Brussels, 16 August For the Commission Franz FISCHLER Member of the Commission ( 1 ) OJ L 329, , p. 18. ( 2 ) OJ L 62, , p. 27. ( 3 ) OJ L 9, , p. 15. ( 4 ) OJ L 263, , p. 11. ( 5 ) OJ L 263, , p. 15. ( 6 ) OJ L 263, , p. 19. ( 7 ) OJ L 166, , p. 16.

5 L 221/4 EN COMMISSION REGULATION (EC) No 1483/2002 of 16 August 2002 suspending the buying-in of butter in certain Member States THE COMMISSION OF THE EUROPEAN COMMUNITIES, Having regard to the Treaty establishing the European Community, Having regard to Council Regulation (EC) No 1255/1999 of 17 May 1999 on the common organisation of the market in milk and milk products ( 1 ), as last amended by Commission Regulation (EC) No 509/2002 ( 2 ), Having regard to Commission Regulation (EC) No 2771/1999 of 16 December 1999 laying down detailed rules for the application of Council Regulation (EC) No 1255/1999 as regards intervention on the market in butter and cream ( 3 ), as last amended by Regulation (EC) No 1614/2001 ( 4 ), and in particular Article 2 thereof, Whereas: (1) Article 2 of Regulation (EC) No 2771/1999 lays down that buying-in by invitation to tender is to be opened or suspended by the Commission in a Member State, as appropriate, once it is observed that, for two weeks in succession, the market price in that Member State is below or equal to or above 92 % of the intervention price. (2) Commission Regulation (EC) No 1430/2002 suspending the buying-in of butter in certain Member States ( 5 ) establishes the most recent list of Member States in which intervention is suspended. This list must be adjusted as a result of the market prices communicated by Belgium, Luxembourg and the Netherlands under Article 8 of Regulation (EC) No 2771/1999. In the interests of clarity, the list in question should be replaced and Regulation (EC) No 1430/2002 should be repealed, HAS ADOPTED THIS REGULATION: Article 1 Buying-in of butter by invitation to tender as provided for in Article 6(1) of Regulation (EC) No 1255/1999 is hereby suspended in Denmark, Greece, the Netherlands and Austria. Article 2 Regulation (EC) No 1430/2002 is hereby repealed. Article 3 This Regulation shall enter into force on 17 August This Regulation shall be binding in its entirety and directly applicable in all Member States. Done at Brussels, 16 August For the Commission Franz FISCHLER Member of the Commission ( 1 ) OJ L 160, , p. 48. ( 2 ) OJ L 79, , p. 15. ( 3 ) OJ L 333, , p. 11. ( 4 ) OJ L 214, , p. 20. ( 5 ) OJ L 206, , p. 14.

6 EN L 221/5 COMMISSION REGULATION (EC) No 1484/2002 of 16 August 2002 amending the import duties in the cereals sector THE COMMISSION OF THE EUROPEAN COMMUNITIES, Having regard to the Treaty establishing the European Community, Having regard to Council Regulation (EEC) No 1766/92 of 30 June 1992 on the common organisation of the market in cereals ( 1 ), as last amended by Regulation (EC) No 1666/ 2000 ( 2 ), Having regard to Commission Regulation (EC) No 1249/96 of 28 June 1996 laying down detailed rules for the application of Council Regulation (EEC) No 1766/92 as regards import duties in the cereals sector ( 3 ), as last amended by Regulation (EC) No 597/2002 ( 4 ), and in particular Article 2(1) thereof, Whereas: (1) The import duties in the cereals sector are fixed by Commission Regulation (EC) No 1478/2002 ( 5 ). (2) Article 2(1) of Regulation (EC) No 1249/96 provides that if during the period of application, the average import duty calculated differs by EUR 5 per tonne from the duty fixed, a corresponding adjustment is to be made. Such a difference has arisen. It is therefore necessary to adjust the import duties fixed in Regulation (EC) No 1478/2002, HAS ADOPTED THIS REGULATION: Article 1 Annexes I and II to Regulation (EC) No 1478/2002 are hereby replaced by Annexes I and II to this Regulation. Article 2 This Regulation shall enter into force on 17 August This Regulation shall be binding in its entirety and directly applicable in all Member States. Done at Brussels, 16 August For the Commission J. M. SILVA RODRÍGUEZ Agriculture Director-General ( 1 ) OJ L 181, , p. 21. ( 2 ) OJ L 193, , p. 1. ( 3 ) OJ L 161, , p ( 4 ) OJ L 91, , p. 9. ( 5 ) OJ L 220, , p. 11.

7 L 221/6 EN ANNEX I Import duties for the products covered by Article 10(2) of Regulation(EEC) No 1766/92 CN code Description Import duty ( 2 ) (EUR/tonne) Durum wheat high quality 0,00 medium quality ( 1 ) 0, Common wheat seed 0, Common high quality wheat other than for sowing ( 3 ) 0,00 medium quality 0,00 low quality 9, Rye 23, Barley, seed 23, Barley, other ( 4 ) 23, Maize seed other than hybrid 37, Maize other than seed ( 5 ) 37, Grain sorghum other than hybrids for sowing 33,84 ( 1 ) In the case of durum wheat not meeting the minimum quality requirements for durum wheat of medium quality, referred to in Annex I to Regulation (EC) No 1249/96, the duty applicable is that fixed for low-quality common wheat. ( 2 ) For goods arriving in the Community via the Atlantic Ocean or via the Suez Canal (Article 2(4) of Regulation (EC) No 1249/96), the importer may benefit from a reduction in the duty of: EUR 3 per tonne, where the port of unloading is on the Mediterranean Sea, or EUR 2 per tonne, where the port of unloading is in Ireland, the United Kingdom, Denmark, Sweden, Finland or the Atlantic coasts of the Iberian peninsula. ( 3 ) The importer may benefit from a flat-rate reduction of EUR 14 per tonne, where the conditions laid down in Article 2(5) of Regulation (EC) No 1249/96 are met. ( 4 ) The importer may benefit from a flat-rate reduction of EUR 8 per tonne, where the conditions laid down in Article 2(5) of Regulation (EC) No 1249/96 are met. ( 5 ) The importer may benefit from a flat-rate reduction of EUR 24 per tonne, where the conditions laid down in Article 2(5) of Regulation (EC) No 1249/96 are met.

8 EN L 221/7 ANNEX II 1. Averages over the two-week period preceding the day of fixing: Factors for calculating duties (period from 14 August to 16 August 2002) Exchange quotations Minneapolis Kansas City Chicago Chicago Minneapolis Minneapolis Minneapolis Product (% proteins at 12 % humidity) HRS2. 14 % HRW2. 11,5 % SRW2 YC3 HAD2 Medium quality (*) US barley 2 Quotation (EUR/t) 146,16 143,12 128,84 109,33 187,63 (**) 177,63 (**) 109,98 (**) Gulf premium (EUR/t) 22,45 7,18 8,13 Great Lakes premium (EUR/t) 19,51 (*) A discount of 10 EUR/t (Article 4(1) of Regulation (EC) No 1249/96). (**) Fob Duluth. 2. Freight/cost: Gulf of Mexico Rotterdam: 11,78 EUR/t; Great Lakes Rotterdam: 23,30 EUR/t. 3. Subsidy within the meaning of the third paragraph of Article 4(2) of Regulation (EC) No 1249/96: 0,00 EUR/t (HRW2) 0,00 EUR/t (SRW2).

9 L 221/8 EN II (Acts whose publication is not obligatory) COMMISSION COMMISSION DECISION of 12 August 2002 implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretation of results (notified under document number C(2002) 3044) (Text witheea relevance) (2002/657/EC) THE COMMISSION OF THE EUROPEAN COMMUNITIES, Having regard to the Treaty establishing the European Community, Having regard to Council Directive 96/23/EC of 29 April 1996 on measures to monitor certain substances and residues thereof in live animals and animal products and repealing Directives 85/358/EEC and 86/469/EEC and Decisions 89/187/EEC and 91/664/EEC ( 1 ), and in particular the second subparagraph of Article 15(1) thereof, Whereas: (1) The presence of residues in products of animal origin is a matter of concern for public health. (2) Commission Decision 98/179/EC of 23 February 1998 laying down detailed rules on official sampling for the monitoring of certain substances and residues thereof in live animals and animal products ( 2 ) provides that the analysis of samples is to be carried out exclusively by laboratories approved for official residue control by the competent national authority. (3) It is necessary to ensure the quality and comparability of the analytical results generated by laboratories approved for official residue control. This should be achieved by using quality assurance systems and specifically by applying of methods validated according to common procedures and performance criteria and by ensuring traceability to common standards or standards commonly agreed upon. (4) Council Directive 93/99/EEC of 29 October 1993 on the subject of additional measures concerning the official control of foodstuffs and Decision 98/179/EC ( 3 ) require ( 1 ) OJ L 125, , p. 10. ( 2 ) OJ L 65, , p. 31. ( 3 ) OJ L 290, , p. 14. official control laboratories to be accredited according to ISO (1) from January 2002 onwards. Pursuantto Decision 98/179/EC, participation in an internationally recognised external quality control assessment and accreditation scheme is required for approved laboratories. Moreover, approved laboratories must prove their competence by regular and successful participation in adequate proficiency testing schemes recognised or organised by the national or Community reference laboratories. (5) A network of Community reference laboratories, national reference laboratories and national control laboratories operates under Directive 96/23/EC to enhance coordination. (6) As a result of advances in analytical chemistry since the adoption of Directive 96/23/EC the concept of routine methods and reference methods has been superseded by criteria approach, in which performance criteria and procedures for the validation of screening and confirmatory methods are established. (7) It is necessary to determine common criteria for the interpretation of test results of official control laboratories in order to ensure a harmonised implementation of Directive 96/23/EC. (8) It is necessary to provide for the progressive establishmentof minimum required performance limits (MRPL) of analytical method for substances for which no permitted limit has been established and in particular for those substances whose use is not authorised, or is specifically prohibited in the Community, in order to ensure harmonised implementation of Directive 96/23/EC.

10 EN L 221/9 (9) Commission Decision 90/515/EEC of 26 September 1990 laying down the reference methods for detecting residues of heavy metals and arsenic ( 1 ), Commission Decision 93/256/EEC of 14 May 1993 laying down the methods to be used for detecting residues of substances having a hormonal or a thyrostatic action ( 2 ), and of Commission Decision 93/257/EEC of 15 April 1993 laying down the reference methods and the list of the national reference laboratories for detecting residues ( 3 ), as lastamended by Decision 98/536/EC ( 4 ) have been reexamined before in order to take account of developments in scientific and technical knowledge, have been found outdated in their scope and provisions and should accordingly be repealed with this Decision. (10) In order to allow methods for the analysis of official samples to be adapted to the provisions of this Decision, a transitional period should be laid down. (11) The measures provided for in this Decision are in accordance with the opinion of the Standing Committee on the Food Chain and Animal Health, (d) comply with the relevant minimum required performance limits (MRPL) to be established in accordance with Article 4. Article 4 Minimum required performance limits The present Decision shall be reviewed to progressively establish the minimum required performance limits (MRPL) of analytical methods to be used for substances for which no permitted limithas been established. Article 5 Quality control The Member States shall ensure the quality of the results of the analysis of samples taken pursuant to Directive 96/23/EC, in particular by monitoring tests and/or calibration results according to Chapter 5.9 of ISO (1). HAS ADOPTED THIS DECISION: Article 1 Subject matter and scope This Decision provides rules for the analytical methods to be used in the testing of official samples taken pursuant to Article 15(1), second sentence, of Directive 96/23/EC and specifies common criteria for the interpretation of analytical results of official control laboratories for such samples. This Decision shall not apply to substances for which more specific rules have been laid down in other Community legislation. Article 2 Definitions For the purpose of this Decision the definitions in Directive 96/ 23/EC and in the Annex to this decision shall apply. Article 3 Analytical methods The Member States shall ensure that official samples taken pursuant to Directive 96/23/EC are analysed using methods that: (a) are documented in test instructions, preferably according to ISO 78-2 (6); (b) comply with Part 2 of the Annex to this Decision; (c) have been validated according to the procedures described in Part3 of the Annex; ( 1 ) OJ L 286, , p. 33. ( 2 ) OJ L 118, , p. 64. ( 3 ) OJ L 118, , p. 75. ( 4 ) OJ L 251, , p. 39. Article 6 Interpretation of results 1. The resultof an analysis shall be considered noncompliant if the decision limit of the confirmatory method for the analyte is exceeded. 2. If a permitted limit has been established for a substance, the decision limit is the concentration above which it can be decided with a statistical certainty of 1 α that the permitted limithas been truly exceeded. 3. If no permitted limit has been established for a substance, the decision limit is the lowest concentration level at which a method can discriminate with a statistical certainty of 1 α that the particular analyte is present. 4. For substances listed in Group A of Annex I to Directive 96/23/EC, the α error shall be 1 % or lower. For all other substances, the α error shall be 5 % or lower. Article 7 Repeal Decisions 90/515/EEC, 93/256/EEC and 93/257/EEC are repealed. Article 8 Transitional provisions The methods for the analysis of official samples of substances listed in Group A of Annex I to Directive 96/23/EC, which satisfy the criteria set out in Decisions 90/515/EEC, 93/256/ EEC and 93/257/EEC may be used for up to two years after this Decision enters into force. Methods currently applied for substances listed in Group B of Annex I to Directive 96/23/EC shall comply with this Decision at the latest five years after the date of application of this Decision.

11 L 221/10 EN Article 9 Date of application This Decision shall apply from 1 September Article 10 Addressees This Decision is addressed to the Member States. Done atbrussels, 12 August2002. For the Commission David BYRNE Member of the Commission

12 EN L 221/11 ANNEX PERFORMANCE CRITERIA, OTHER REQUIREMENTS AND PROCEDURES FOR ANALYTICAL METHODS 1. DEFINITIONS 1.1. Accuracy means the closeness of agreement between a test result and the accepted reference value (2). It is determined by determining trueness and precision Alpha (α) error means the probability that the tested sample is compliant, even though a non-compliant measurementhas been obtained (false non-compliantdecision) Analyte means the substance that has to be detected, identified and/or quantified and derivatives emerging during its analysis Beta (β) error means the probability that the tested sample is truly non-compliant, even though a compliant measurementhas been obtained (false compliantdecision) Bias means the difference between the expectation of the test result and an accepted reference value (2) Calibration standard means a device for measurements that represents the quantity of substance of interest in a way that ties its value to a reference base Certified reference material (CRM) means a material that has had a specified analyte content assigned to it Co-chromatography means a procedure in which the extract prior to the chromatographic step(s) is divided into two parts. Part one is chromatographed as such. Part two is mixed with the standard analyte that is to be measured. Then this mixture is also chromatographed. The amount of added standard analyte has to be similar to the estimated amount of the analyte in the extract. This method is designed to improve the identification of an analyte when chromatographic methods are used, especially when no suitable internal standard can be used Collaborative study means analysing the same sample by the same method to determine the performance characteristics of the method. The study covers random measurement error and laboratory bias Confirmatory method means methods that provide full or complementary information enabling the substance to be unequivocally identified and if necessary quantified at the level of interest Decision limit(ccα) means the limit at and above which it can be concluded with an error probability of α that a sample is non-compliant Detection capability (CCβ) means the smallest content of the substance that may be detected, identified and/or quantified in a sample with an error probability of β. In the case of substances for which no permitted limit has been established, the detection capability is the lowest concentration at which a method is able to detect truly contaminated samples with a statistical certainty of 1 β. In the case of substances with an established permitted limit, this means that the detection capability is the concentration at which the method is able to detect permitted limit concentrations with a statistical certainty of 1 β Fortified sample material means a sample enriched with a known amount of the analyte to be detected Interlaboratory study (comparison) means organisation, performance and evaluation of tests on the same sample by two or more laboratories in accordance with predetermined conditions to determine testing performance. According to the purpose the study can be classified as collaborative study or proficiency study Internal Standard (IS) means a substance not contained in the sample with physical-chemical properties as similar as possible to those of the analyte that has to be identified and which is added to each sample as well as to each calibration standard Laboratory sample means a sample prepared for sending to a laboratory and intended for inspection or testing Level of interest means the concentration of substance or analyte in a sample that is significant to determine its compliance with legislation Minimum required performance limit(mrpl) means minimum contentof an analyte in a sample, which atleasthas to be detected and confirmed. It is intended to harmonise the analytical performance of methods for substances for which no permitted limited has been established.

13 L 221/12 EN Performance characteristic means functional quality that can be attributed to an analytical method. This may be for instance specificity, accuracy, trueness, precision, repeatability, reproducibility, recovery, detection capability and ruggedness Performance criteria means requirements for a performance characteristic according to which it can be judged that the analytical method is fit for the purpose and generates reliable results Permitted limit means maximum residue limit, maximum level or other maximum tolerance for substances established elsewhere in Community legislation Precision means the closeness of agreement between independent test results obtained under stipulated (predetermined) conditions. The measure of precision usually is expressed in terms of imprecision and computed as standard deviation of the test result. Less precision is determined by a larger standard deviation (2) Proficiency study means analysing the same sample allowing laboratories to choose their own methods, provided these methods are used under routine conditions. The study has to be performed according to ISO guide 43-1 (3) and 43-2 (4) and can be used to assess the reproducibility of methods Qualitative method means an analytical method which identifies a substance on the basis of its chemical, biological or physical properties Quantitative method means an analytical method which determines the amount or mass fraction of a substance so that it may be expressed as a numerical value of appropriate units Reagent blank determination means the complete analytical procedure applied without the test portion or using an equivalent amount of suitable solvent in place of the test portion Recovery means the percentage of the true concentration of a substance recovered during the analytical procedure. It is determined during validation, if no certified reference material is available Reference material means a material of which one or several properties have been confirmed by a validated method, so that it can be used to calibrate an apparatus or to verify a method of measurement Repeatability means precision under repeatability conditions (2) Repeatability conditions means conditions where independent test results are obtained with the same method on identical test items in the same laboratory by the same operator using the same equipment (2) Reproducibility means precision under reproducibility conditions (2)(4) Reproducibility conditions means conditions where test results are obtained with the same method on identical test items in different laboratories with different operators using different equipment (2)(4) Ruggedness means the susceptibility of an analytical method to changes in experimental conditions which can be expressed as a list of the sample materials, analytes, storage conditions, environmental and/or sample preparation conditions under which the method can be applied as presented or with specified minor modifications. For all experimental conditions which could in practice be subject to fluctuation (e.g. stability of reagents, composition of the sample, ph, temperature) any variations which could affect the analytical result should be indicated Sample blank determination means the complete analytical procedure applied to a test portion taken from a sample from which the analyte is absent Screening method means methods that are used to detect the presence of a substance or class of substances at the level of interest. These methods have the capability for a high sample throughput and are used to sift large numbers of samples for potential non-compliant results. They are specifically designed to avoid false compliant results Single laboratory study (in-house validation) means an analytical study involving a single laboratory using one method to analyse the same or different test materials under different conditions over justified long time intervals Specificity means the ability of a method to distinguish between the analyte being measured and other substances. This characteristic is predominantly a function of the measuring technique described, but can vary according to class of compound or matrix.

14 EN L 221/ Standard addition means a procedure in which the test sample is divided in two (or more) test portions. One portion is analysed as such and known amounts of the standard analyte are added to the other test portions before analysis. The amount of the standard analyte added has to be between two and five times the estimated amount of the analyte in the sample. This procedure is designed to determine the content of an analyte in a sample, taking account of the recovery of the analytical procedure Standard analyte means an analyte of known and certified content and purity to be used as a reference in the analysis Substance means matter of particular or definite chemical constitution and its metabolites Test portion means the quantity of material drawn from the test sample on which the test or observation is carried out Test sample means a sample prepared from a laboratory sample and from which test portions will be taken Trueness means the closeness of agreement between the average value obtained from a large series of test results and an accepted reference value. Trueness is usually expressed as bias (2) Units means those units described in ISO 31 (20) and Directive 71/354/EC (19) Validation means the confirmation by examination and the provision of effective evidence that the particular requirements of a specific intended use are fulfilled (1) Within-laboratory reproducibility means precision obtained in the same laboratory under stipulated (predetermined) conditions (concerning e.g. method, test materials, operators, environment) over justified long time intervals. 2. PERFORMANCE CRITERIA AND OTHER REQUIREMENTS FOR ANALYTICAL METHODS Analytical methods or combinations of methods other than those described below may only be used for screening or confirmatory purposes if it can be proven that they fulfil the relevant requirements established in this Decision GENERAL REQUIREMENTS Handling of samples Samples shall be obtained, handled and processed in such a way that there is a maximum chance of detecting the substance. Sample handling procedures shall prevent the possibility of accidental contamination or loss of analytes Performance of tests Recovery During the analysis of samples the recovery shall be determined in each batch of samples, if a fixed recovery correction factor is used. If the recovery is within limits, the fixed correction factor may then be used. Otherwise the recovery factor obtained for that specific batch shall be used, unless the specific recovery factor of the analyte in the sample is to be applied in which case the standard addition procedure (see 3.5) or an internal standard shall be used for the quantitative determination of an analyte in a sample Specificity A method shall be able to distinguish between the analyte and the other substances under the experimental conditions. An estimate to which extent this is possible has to be provided. Strategies to overcome any foreseeable interference with substances when the described measuring technique is used, e.g. homologues, analogues, metabolic products of the residue of interest have to be employed. It is of prime importance that interference, which might arise from matrix components, is investigated SCREENING METHODS Only those analytical techniques, for which it can be demonstrated in a documented traceable manner that they are validated and have a false compliant rate of < 5%(β-error) at the level of interest shall be used for screening purposes in conformity with Directive 96/23/EC. In the case of a suspected non-compliant result, this result shall be confirmed by a confirmatory method.

15 L 221/14 EN CONFIRMATORY METHODS FOR ORGANIC RESIDUES AND CONTAMINANTS Confirmatory methods for organic residues or contaminants shall provide information on the chemical structure of the analyte. Consequently methods based only on chromatographic analysis without the use of spectrometric detection are not suitable on their own for use as confirmatory methods. However, if a single technique lacks sufficient specificity, the desired specificity shall be achieved by analytical procedures consisting of suitable combinations of clean-up, chromatographic separation(s) and spectrometric detection. The following methods or method combinations are considered suitable for the identification of organic residues or contaminants for the substance groups indicated: Table 1 Suitable confirmatory methods for organic residues or contaminants Measuring technique Substances Annex 1 96/23/EC Limitations LC or GC with mass-spectrometric detection LC or GC with IR spectrometric detection Groups A and B Groups A and B Only if following either an on-line or an off-line chromatographic separation Only if full scan techniques are used or using atleast3 (group B) or 4 (group A) identification points for techniques that do not record the full mass spectra Specific requirements for absorption in IR spectrometry have to be met LC-full-scan DAD Group B Specific requirements for absorption in UV spectrometry have to be met LC -fluorescence Group B Only for molecules that exhibit native fluorescence and to molecules that exhibit fluorescence after either transformation or derivatisation 2-D TLC - full-scan UV/VIS Group B Two-dimensional HPTLC and co-chromatography are mandatory GC-Elektron capture detection Group B Only if two columns of different polarity are used LC-immunogram Group B Only if at least two different chromatographic systems or a second, independent detection method are used LC-UV/VIS (single wavelength) Group B Only if at least two different chromatographic systems or second, independent detection method are used Common performance criteria and requirements Confirmatory methods shall provide information on the chemical structure of the analyte. When more than one compound gives the same response, then the method cannot discriminate between these compounds. Methods based only on chromatographic analysis without the use of spectrometric detection are not suitable on their own for use as confirmatory methods. Where used in the method, a suitable internal standard shall be added to the test portion at the beginning of the extraction procedure. Depending on availability, either stable isotope-labelled forms of the analyte, which are particularly suited for mass-spectrometric detection, or compounds that are structurally related to the analyte shall be used. When no suitable internal standard can be used, the identification of the analyte shall be confirmed by co-chromatography. In this case only one peak shall be obtained, the enhanced peak height (or area) being equivalent to the amount of added analyte. With gas chromatography (GC) or liquid chromatography (LC), the peak width at half-maximum height shall be within the % range of the original width, and the retention times shall be identical within a margin of 5 %. For thin layer chromatography (TLC) methods, only the spot presumed to be due to the analyte shall be intensified; a new spot shall not appear and the visual appearance shall notchange.

16 EN L 221/15 Reference or fortified material containing known amounts of analyte, at or near either the permitted limit or the decision limit (non-compliant control sample) as well as compliant control materials and reagent blanks should preferably be carried through the entire procedure simultaneously with each batch of test samples analysed. The order for injecting the extracts into the analytical instrument is as follows: reagent blank, compliant control sample, sample(s) to be confirmed, compliant control sample again and finally non-compliant control sample. Any variation from this sequence shall be justified Additional performance criteria and other requirements for quantitative methods of analysis Trueness of quantitative methods In the case of repeated analyses of a certified reference material, the guideline ranges for the deviation of the experimentally determined recovery corrected mean mass fraction from the certified value are as follows: Table 2 Minimum trueness of quantitative methods Mass fraction Range 1 µg/kg 50 % to + 20 % > 1 µg/kg to 10 µg/kg 30 % to + 10 % 10 µg/kg 20%to+10% When no such CRMs are available, it is acceptable that trueness of measurements is assessed through recovery of additions of known amounts of the analyte(s) to a blank matrix. Data corrected with the mean recovery are only acceptable when they fall within the ranges shown in Table Precision of quantitative methods The inter-laboratory coefficient of variation (CV) for the repeated analysis of a reference or fortified material, under reproducibility conditions, shall not exceed the level calculated by the Horwitz Equation. The equation is: CV = 2 (1 0,5 log C) where C is the mass fraction expressed as a power (exponent) of 10 (e.g. 1 mg/g = 10-3 ). Examples are shown in the table 3. Table 3 Examples for reproducibility CVs for quantitative methods at a range of analyte mass fractions Mass fraction Reproducibility CV(%) 1 µg/kg (*) 10 µg/kg (*) 100 µg/kg µg/kg (1 mg/kg) 16 (*) For mass fractions lower than 100 µg/kg the application of the Horwitz Equation gives unacceptable high values. Therefore, the CVs for concentrations lower than 100 µg/kg shall be as low as possible. For analyses carried out under repeatability conditions, the intra-laboratory CV would typically be between one half and two thirds of the above values. For analyses carried out under within-laboratory reproducibility conditions, the within-laboratory CV shall not be greater than the reproducibility CV. In the case of substances with an established permitted limit, the method shall achieve within-laboratory reproducibility not greater than the corresponding reproducibility CV at a concentration of 0,5 the permitted limit.

17 L 221/16 EN Performance criteria and other requirements for mass spectrometric detection Mass spectrometric methods are suitable for consideration as confirmatory methods only following either an on-line or an off-line chromatographic separation Chromatographic separation For GC-MS procedures, the gas chromatographic separation shall be carried out using capillary columns. For LC-MS procedures, the chromatographic separation shall be carried out using suitable LC columns. In any case, the minimum acceptable retention time for the analyte under examination is twice the retention time corresponding to the void volume of the column. The retention time (or relative retention time) of the analyte in the test portion shall match that of the calibration standard within a specified retention time window. The retention time window shall be commensurate with the resolving power of the chromatographic system. The ratio of the chromatographic retention time of the analyte to that of the internal standard, i.e. the relative retention time of the analyte, shall correspond to that of the calibration solution at a tolerance of ± 0,5 % for GC and ± 2,5 % for LC Mass spectrometric detection Mass-spectrometric detection shall be carried out by employing MS-techniques such as recording of full mass spectra (full scans) or selected ion monitoring (SIM), as well as MS-MS n techniques such as Selected Reaction Monitoring (SRM), or other suitable MS or MS-MS n techniques in combination with appropriate ionisation modes. In high-resolution mass spectrometry (HRMS), the resolution shall typically be greater than for the entire mass range at 10 % valley. Full scan: When mass spectrometric determination is performed by the recording of full scan spectra, the presence of all measured diagnostic ions (the molecular ion, characteristic adducts of the molecular ion, characteristic fragment ions and isotope ions) with a relative intensity of more than 10 % in the reference spectrum of the calibration standard is obligatory. SIM: When mass spectrometric determination is performed by fragmentography, the molecular ion shall preferably be one of the selected diagnostic ions (the molecular ion, characteristic adducts of the molecular ion, characteristic fragment ions and all their isotope ions). The selected diagnostic ions should not exclusively originate from the same part of the molecule. The signal-to-noise ratio for each diagnostic ion shall be 3:1. Full scan and SIM: The relative intensities of the detected ions, expressed as a percentage of the intensity of the most intense ion or transition, shall correspond to those of the calibration standard, either from calibration standard solutions or from spiked samples, at comparable concentrations, measured under the same conditions, within the following tolerances: Table 4 Maximum permitted tolerances for relative ion intensities using a range of mass spectrometric techniques Relative intensity (% of base peak) EI-GC-MS (relative) CI-GC-MS, GC-MS n LC-MS, LC-MS n (relative) > 50 % ± 10 % ± 20 % > 20%to50% ± 15 % ± 25 % > 10%to20% ± 20 % ± 30 % 10 % ± 50 % ± 50 % Interpretation of mass spectral data: The relative intensities of the diagnostic ions and/or precursor/ product ion pairs have to be identified by comparing spectra or by integrating the signals of the single mass traces. Whenever background correction is applied, this shall be applied uniformly throughout the batch (see 2.3.1, paragraph 4) and shall be clearly indicated. Full scan: When full scan spectra are recorded in single mass spectrometry, a minimum of four ions shall be present with a relative intensity of 10 % of the base peak. The molecular ion shall be included if it is present in the reference spectrum with a relative intensity of 10 %. At least four ions shall lie within the maximum permitted tolerances for relative ion intensities (Table 5). Computer-aided library searching may be used. In this case, the comparison of mass spectral data in the test samples to that of the calibration solution has to exceed a critical match factor. This factor shall be determined during the validation process for every analyte on the basis of spectra for which the criteria described below are fulfilled. Variability in the spectra caused by the sample matrix and the detector performance shall be checked.

18 EN L 221/17 SIM: When mass fragments are measured using other than full-scan techniques, a system of identification points shall be used to interpret the data. For the confirmation of substances listed in Group A of Annex I of Directive 96/23/EC, a minimum of 4 identification points shall be required. For the confirmation of substances listed in Group B of Annex I of Directive 96/23/EC, a minimum of 3 identification points are required. The table below shows the number of identification points that each of the basic mass spectrometric techniques can earn. However, in order to qualify for the identification points required for confirmation and the sum of identification points to be calculated: (a) a minimum of atleastone ion ratio shall be measured, and (b) all relevant measured ion ratios shall meet the criteria described above, and (c) a maximum of three separate techniques can be combined to achieve the minimum number of identification points. Table 5 The relationship between a range of classes of mass fragment and identification points earned MS technique Identification points earned per ion Low resolution mass spectrometry (LR) 1,0 LR-MS n precursor ion 1,0 LR-MS n transition products 1,5 HRMS 2,0 HR- MS n precursor ion 2,0 HR-MS n transition products 2,5 Footnotes: (1) Each ion may only be counted once. (2) GC-MS using electron impact ionisation is regarded as being a different technique to GC-MS using chemical ionisation. (3) Different analytes can be used to increase the number of identification points only if the derivatives employ different reaction chemistries. (4) For substances in Group A of Annex 1 to Directive 96/23/EC, if one of the following techniques are used in the analytical procedure: HPLC coupled with full-scan diode array spectrophotometry (DAD); HPLC coupled with fluorescence detection; HPLC coupled to an immunogram; two-dimensional TLC coupled to spectrometric detection; a maximum of one identification point may be contributed, providing that the relevant criteria for these techniques are fulfilled. (5) Transition products include both daughter and granddaughter products. Table 6 Examples of the number of identification points earned for a range of techniques and combinations thereof (n = an integer) Technique(s) Number of ions Identification points GC-MS (EI or CI) N n GC-MS (EI and CI) 2 (EI) + 2 (CI) 4 GC-MS (EI or CI) 2 derivatives 2 (Derivative A) + 2 (Derivative B) 4 LC-MS N n GC-MS-MS 1 precursor and 2 daughters 4 LC-MS-MS 1 precursor and 2 daughters 4 GC-MS-MS 2 precursor ions, each with 1 daughter 5 LC-MS-MS 2 precursor ions, each with 1 daughter 5 LC-MS-MS-MS 1 precursor, 1 daughter and 2 granddaughters 5,5 HRMS N 2 n GC-MS and LC-MS GC-MS and HRMS

19 L 221/18 EN Performance criteria and other requirements for chromatography coupled to infrared detection Adequate peaks: Adequate peaks are absorption maxima in the infrared spectrum of a calibration standard fulfilling the following requirements Infra-red detection Absorption maximum: This shall be in the wavenumber range cm -1. Intensity of absorption: This shall not be less than either: (a) a specific molar absorbance of 40 with respect to peak base line; or (b) a relative absorbance of 12,5 % of the absorbance of the most intense peak in the region cm -1 when both are measured with respect to zero absorbance, and 5 % of the absorbance of the most intense peak in the region cm -1 when both are measured with respect to their peak base line. Note: Although adequate peaks according to (a) may be preferred from a theoretical point of view, those according to (b) are easier to determine in practice. The number of peaks in the infrared spectrum of the analyte whose frequencies correspond with an adequate peak in the spectrum of the calibration standard, within a margin of ±1cm -1 is determined Interpretation of infra-red spectral data Absorption shall be present in all regions of the analyte spectrum which correspond with an adequate peak in the reference spectrum of the calibration standard. A minimum of six adequate peaks is required in the infrared spectrum of the calibration standard. If there are less than six adequate peaks (7), the spectrum at issue cannot be used as a reference spectrum. The score, i.e. the percentage of the adequate peaks found in the infrared spectrum of the analyte, shall be at least 50. Where there is no exact match for an adequate peak, the relevant region of the analyte spectrum shall be consistent with the presence of a matching peak. The procedure is only applicable to absorption peaks in the sample spectrum with an intensity of a least three times the peak to peak noise Performance criteria and other requirements for the determination of an analyte using LC with other detection techniques Chromatographic separation An internal standard shall be used if a material suitable for this purpose is available. It shall preferably be a related standard with a retention time close to that of the analyte. The analyte shall elute at the retention time that is typical for the corresponding calibration standard under the same experimental conditions. The minimum acceptable retention time for an analyte shall be two times the retention time corresponding to the void volume of the column. The ratio of the retention time of the analyte to that of the internal standard, i.e. the relative retention time of the analyte, shall be the same as that of the calibration standard in the appropriate matrix, within a margin of ± 2,5 % Full-scan UV/VIS detection The performance criteria for LC methods have to be fulfilled. The absorption maxima in the spectrum of the analyte shall be at the same wavelengths as those of the calibration standard within a margin determined by the resolution of the detection system. For diode array detection, this is typically within ± 2 nm. The spectrum of the analyte above 220 nm shall, for those parts of the two spectra with a relative absorbance 10 %, not be visibly different from the spectrum of the calibration standard. This criterion is met when firstly the same maxima are present and secondly when the difference between the two spectra is at no point observed greater than 10 % of the absorbance of the calibration standard. In the case computer-aided library searching and matching are used, the comparison of the spectral data in the test samples to that of the calibration solution has to exceed a critical match factor. This factor shall be determined during the validation process for every analyte on the basis of spectra for which the criteria described above are fulfilled. Variability in the spectra caused by the sample matrix and the detector performance shall be checked.