ANNEX I

DEFINITIONS AND ABBREVIATIONS

I.   DEFINITIONS

For the purposes of this Regulation the definitions laid down in Annex I to Commission Decision 2002/657/EC of 14 August 2002 implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretation of results (1) shall apply.

Further to these definitions, the following definitions shall apply for the purposes of this Regulation:

1.1.	‘Action level’ means the level of a given substance, as laid down in Annex to Recommendation 2013/711/EU, which triggers investigations to identify the source of that substance in cases where increased levels of the substance are detected.

1.2.

‘Screening methods’ means methods used for selection of those samples with levels of PCDD/Fs and dioxin-like PCBs that exceed the maximum levels or the action levels. They shall allow a cost-effective high sample-throughput, thus increasing the chance to discover new incidents with high exposure and health risks to consumers. Screening methods shall be based on bioanalytical or GC-MS methods. Results from samples exceeding the cut-off value to check compliance with the maximum level shall be verified by a full re-analysis from the original sample by a confirmatory method.

1.3.

‘Confirmatory methods’ means methods that provide full or complementary information enabling the PCDD/Fs and dioxin-like PCBs to be identified and quantified unequivocally at the maximum or in case of need at the action level. Such methods utilise gas chromatography/high resolution mass spectrometry (GC-HRMS) or gas chromatography/tandem mass spectrometry (GC-MS/MS).

1.4.

‘Bioanalytical methods’ means methods based on the use of biological principles like cell-based assays, receptor-assays or immunoassays. They do not give results at the congener level but merely an indication (2) of the TEQ level, expressed in Bioanalytical Equivalents (BEQ) to acknowledge the fact that not all compounds present in a sample extract that produce a response in the test may obey all requirements of the TEQ-principle.

1.5.

‘Bioassay apparent recovery’ means the BEQ level calculated from the TCDD or PCB 126 calibration curve corrected for the blank and then divided by the TEQ level determined by the confirmatory method. It attempts to correct factors like the loss of PCDD/PCDFs and dioxin-like compounds during the extraction and clean-up steps, co-extracted compounds increasing or decreasing the response (agonistic and antagonistic effects), the quality of the curve fit, or differences between the TEF and the REP values. The bioassay apparent recovery is calculated from suitable reference samples with representative congener patterns around the maximum or action level.

1.6.	‘Semi-quantitative methods’ means methods which give an approximate indication of the concentration of the putative analyte, while the numerical result does not meet the requirements for quantitative methods.

1.7.

‘Accepted specific limit of quantification of an individual congener in a sample’ means the lowest content of the analyte that can be measured with reasonable statistical certainty, fulfilling the identification criteria as described in internationally recognised standards, for example, in standard EN 16215:2012 (Animal feed — Determination of dioxins and dioxin-like PCBs by GC/HRMS and of indicator PCBs by GC/HRMS) and/or in EPA methods 1613 and 1668 as revised. The limit of quantification of an individual congener may be identified as (a) the concentration of an analyte in the extract of a sample which produces an instrumental response at two different ions to be monitored with a S/N (signal/noise) ratio of 3:1 for the less intensive raw data signal; or, if for technical reasons the signal-to-noise calculation does not provide reliable results, (b) The lowest concentration point on a calibration curve that gives an acceptable (≤ 30 %) and consistent (measured at least at the start and at the end of an analytical series of samples) deviation to the average relative response factor calculated for all points on the calibration curve in each series of samples (3).

1.8.	‘Upper-bound’ means the concept which requires using the limit of quantification for the contribution of each non-quantified congener.

1.9.	‘Lower-bound’ means the concept which requires using zero for the contribution of each non-quantified congener.

1.10.

‘Medium-bound’ means the concept which requires using half of the limit of quantification calculating the contribution of each non-quantified congener.

1.11.

‘Lot’ means an identifiable quantity of food delivered at one time and determined by the official to have common characteristics, such as origin, variety, type of packing, packer, consignor or markings. In the case of fish and fishery products, also the size of fish shall be comparable. In case the size and/or weight of the fish is not comparable within a consignment, the consignment may still be considered as a lot but a specific sampling procedure has to be applied.

1.12.

‘Sublot’ means designated part of a large lot in order to apply the sampling method on that designated part. Each sublot must be physically separated and identifiable.

1.13.

‘Incremental sample’ means a quantity of material taken from a single place in the lot or sublot.

1.14.

‘Aggregate sample’ means the combined total of all the incremental samples taken from the lot or sublot.

1.15.

‘Laboratory sample’: a representative part/quantity of the aggregate sample intended for the laboratory.

II.   ABBREVIATIONS USED

BEQ	Bioanalytical Equivalents
GC	Gas chromatography
HRMS	High resolution mass spectrometry
LRMS	Low resolution mass spectrometry
MS/MS	Tandem mass spectrometry
PCB	Polychlorinated biphenyls
PCDD	Polychlorinated dibenzo-p-dioxins
PCDF	Polychlorinated dibenzofurans
QC	Quality control
REP	Relative potency
TEF	Toxic Equivalency Factor
TEQ	Toxic Equivalents
TCDD	Tetrachlorodibenzodioxin
U	Expanded measurement uncertainty

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(1)  Commission Decision 2002/657/EC of 14 August 2002 implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretation of results (OJ L 221, 17.8.2002, p. 8).

(2)  Bioanalytical methods are not specific to those congeners included in the TEF-scheme. Other structurally related AhR-active compounds may be present in the sample extract which contribute to the overall response. Therefore, bioanalytical results cannot be an estimate but rather an indication of the TEQ level in the sample.

(3)  The LOQ is calculated from the lowest concentration point taking into account the recovery of internal standards and sample intake.

ANNEX II

METHODS OF SAMPLING FOR OFFICIAL CONTROL OF LEVELS OF DIOXINS (PCDD/PCDF), DIOXIN-LIKE PCBs AND NON-DIOXIN-LIKE PCBs IN CERTAIN FOODSTUFFS

I.   SCOPE

Samples intended for the official control of the levels of dioxins (PCDD/PCDF), dioxin-like PCBs and non-dioxin-like PCBs, hereafter referred to as dioxins and PCBs, in foodstuffs shall be taken according to the methods described in this Annex. Aggregate samples thus obtained shall be considered as representative of the lots or sublots from which they are taken. Compliance with maximum levels laid down in Regulation (EC) No 1881/2006 setting maximum levels for certain contaminants in foodstuffs shall be established on the basis of the levels determined in the laboratory samples.

II.   GENERAL PROVISIONS

1.   Personnel

Sampling shall be performed by an authorised person as designated by the Member State.

2.   Material to be sampled

Each lot or sublot, which is to be examined, shall be sampled separately.

3.   Precautions to be taken

In the course of sampling and preparation of the samples, precautions shall be taken to avoid any changes, which would affect the content of dioxins and PCBs, adversely affect the analytical determination or make the aggregate samples unrepresentative.

4.   Incremental samples

As far as possible incremental samples shall be taken at various places distributed throughout the lot or sublot. Departure from such procedure shall be recorded in the record provided for under point II.8 of this Annex.

5.   Preparation of the aggregate sample

The aggregate sample shall be made up by combining the incremental samples. It shall be at least 1 kg unless not practical, e.g. when a single package has been sampled or when the product has a very high commercial value.

6.   Replicate samples

The replicate samples for enforcement, defence and reference purposes shall be taken from the homogenised aggregate sample, unless such procedure conflicts with Member States' rules as regard the rights of the food business operator. The size of the laboratory samples for enforcement shall be sufficient to allow at least for duplicate analyses.

7.   Packaging and transmission of samples

Each sample shall be placed in a clean, inert container offering adequate protection from contamination, from loss of analytes by adsorption to the internal wall of the container and against damage in transit. All necessary precautions shall be taken to avoid any change in composition of the sample, which might arise during transportation or storage.

8.   Sealing and labelling of samples

Each sample taken for official use shall be sealed at the place of sampling and identified following the rules of the Member States.

A record shall be kept of each sampling, permitting each lot to be identified unambiguously and giving the date and place of sampling together with any additional information likely to be of assistance to the analyst.

III.   SAMPLING PLAN

The sampling method applied shall ensure that the aggregate sample is representative for the (sub)lot that is to be controlled.

1.   Division of lots into sublots

Large lots shall be divided into sublots on condition that the sublot can be separated physically. For products traded in large bulk consignments (e.g. vegetable oils) Table 1 shall apply. For other products Table 2 shall apply. Taking into account that the weight of the lot is not always an exact multiple of the weight of the sublots, the weight of the sublot may exceed the mentioned weight by a maximum of 20 %.

Table 1

Subdivision of lots into sublots for products traded in bulk consignments

Lot weight (ton)	Weight or number of sublots
≥ 1 500	500 tonnes
> 300 and < 1 500	3 sublots
≥ 50 and ≤ 300	100 tonnes
< 50	—

Table 2

Subdivision of lots into sublots for other products

Lot weight (ton)	Weight or number of sublots
≥ 15	15-30 tonnes
<15	—

2.   Number of incremental samples

The aggregate sample uniting all incremental samples shall be at least 1 kg (see point II.5 of this Annex).

The minimum number of incremental samples to be taken from the lot or sublot shall be as given in Tables 3 and 4.

In the case of bulk liquid products the lot or sublot shall be thoroughly mixed insofar as possible and insofar it does not affect the quality of the product, by either manual or mechanical means immediately prior to sampling. In this case, a homogeneous distribution of contaminants is assumed within a given lot or sublot. It is therefore sufficient to take three incremental samples from a lot or sublot to form the aggregate sample.

The incremental samples shall be of similar weight. The weight of an incremental sample shall be at least 100 grams.

Departure from this procedure must be recorded in the record provided for under point II.8 of this Annex. In accordance with the provisions of Decision 97/747/EC fixing the levels and frequencies of sampling provided for by Directive 96/23/EC for the monitoring of certain substances and residues thereof in certain animal products, the aggregate sample size for hen eggs is at least 12 eggs (for bulk lots as well for lots consisting of individual packages, tables 3 and 4 shall apply).

Table 3

Minimum number of incremental samples to be taken from the lot or sublot

Weight or volume of lot/sublot (in kg or litre)	Minimum number of incremental samples to be taken
< 50	3
50 to 500	5
> 500	10

If the lot or sublot consists of individual packages or units, then the number of packages or units which shall be taken to form the aggregate sample is given in Table 4.

Table 4

Number of packages or units (incremental samples) which shall be taken to form the aggregate sample if the lot or sublot consists of individual packages or units

Number of packages or units in the lot/sublot	Number of packages or units to be taken
1 to 25	at least 1 package or unit
26 to 100	about 5 %, at least 2 packages or units
> 100	about 5 %, at maximum 10 packages or units

3.   Specific provisions for the sampling of lots containing whole fishes of comparable size and weight

Fishes are considered as being of comparable size and weight in case the difference in size and weight does not exceed about 50 %.

The number of incremental samples to be taken from the lot are defined in Table 3. The aggregate sample uniting all incremental samples shall be at least 1 kg (see point II.5).

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In case the lot to be sampled contains small fishes (individual fishes weighing < about 1 kg), the whole fish is taken as incremental sample to form the aggregate sample. In case the resulting aggregate sample weighs more than 3 kg, the incremental samples may consist of the middle part, weighing each at least 100 grams, of the fishes forming the aggregate sample. The whole part to which the maximum level is applicable is used for homogenisation of the sample. The middle part of the fish is where the centre of gravity is. This is located in most cases at the dorsal fin (in case the fish has a dorsal fin) or halfway between the gill opening and the anus.

—

In case the lot to be sampled contains larger fishes (individual fishes weighing more than about 1 kg), the incremental sample consists of the middle part of the fish. Each incremental sample weighs at least 100 grams. For fishes of intermediate size (about 1-6 kg) the incremental sample is taken as a slice of the fish from backbone to belly in the middle part of the fish. For very large fishes (e.g. > about 6 kg), the incremental part is taken from the right side (frontal view) dorso-lateral muscle meat in the middle part of the fish In case the taking of such a piece of the middle part of the fish would result in a significant economic damage, taking of three incremental samples of at least 350 grams each may be considered as being sufficient, independently of the size of the lot or alternatively an equal part of the muscled meat close to the tail part and the muscle meat close to the head part of one fish may be taken to form the incremental sample being representative for the level of dioxins in the whole fish.

4.   Sampling of lots of fish containing whole fishes of different size and/or weight

—	The provisions of point III.3 as regards sample constitution shall apply.

—	In case a size or weight class/category is predominant (about 80 % or more of the lot), the sample is taken from fishes with the predominant size or weight. This sample is to be considered as being representative for the whole lot.

—	In case no particular size or weight class/category predominates, then it must be ensured that the fishes selected for the sample are representative for the lot. Specific guidance for such cases is provided in ‘Guidance on sampling of whole fishes of different size and/or weight’ (1).

5.   Sampling at retail stage

Sampling of foodstuffs at retail stage shall be done where possible in accordance with the sampling provisions set out in point III.2 of this Annex.

Where this is not possible, an alternative method of sampling at retail stage may be used provided that it ensures sufficient representativeness for the sampled lot or sublot.

IV.   COMPLIANCE OF THE LOT OR SUBLOT WITH THE SPECIFICATION

1.   As regards non-dioxin-like PCBs

The lot is accepted, if the analytical result does not exceed the maximum level of non-dioxin-like PCBs as laid down in Regulation (EC) No 1881/2006 taking into account the measurement uncertainty.

The lot is non-compliant with the maximum level as laid down in Regulation (EC) No 1881/2006, if the upperbound analytical result confirmed by duplicate analysis (2), exceeds the maximum level beyond reasonable doubt taking into account the measurement uncertainty. The mean of the two determinations, taking into account the measurement uncertainty is used for verification of compliance.

The measurement uncertainty may be taken into account according to one of the following approaches:

—	by calculating the expanded uncertainty, using a coverage factor of 2 which gives a level of confidence of approximately 95 %. A lot or sublot is non-compliant if the measured value minus U is above the established permitted level,

—	by establishing the decision limit (CCα) according to the provisions of Commission Decision 2002/657/EC (point 3.1.2.5 of the Annex I to that Decision — the case of substances with an established permitted level). A lot or sublot is non-compliant if the measured value is equal to or above the CCα.

The abovementioned rules shall apply for the analytical result obtained on the sample for official control. In case of analysis for defence or reference purposes, the national rules apply.

2.   As regards dioxins (PCDD/PCDF) and dioxin-like PCBs

The lot is accepted, if the result of a single analysis

—	performed by a screening method with a false-compliant rate below 5 % indicates that the level does not exceed the respective maximum level of PCDD/Fs and the sum of PCDD/Fs and dioxin-like PCBs as laid down in Regulation (EC) No 1881/2006,

—	performed by a confirmatory method does not exceed the respective maximum level of PCDD/Fs and the sum of PCDD/Fs and dioxin-like PCBs as laid down in Regulation (EC) No 1881/2006 taking into account the measurement uncertainty.

For screening assays a cut-off value shall be established for the decision on the compliance with the respective maximum levels set for either PCDD/Fs, or for the sum of PCDD/Fs and dioxin-like PCBs.

The lot is non-compliant with the maximum level as laid down in Regulation (EC) No 1881/2006, if the upperbound analytical result obtained with a confirmatory method and confirmed by duplicate analysis (3), exceeds the maximum level beyond reasonable doubt taking into account the measurement uncertainty. The mean of the two determinations, taking into account the measurement uncertainty is used for verification of compliance.

The measurement uncertainty may be taken into account according to one of the following approaches:

—

by calculating the expanded uncertainty, using a coverage factor of 2 which gives a level of confidence of approximately 95 %. A lot or sublot is non-compliant if the measured value minus U is above the established permitted level. In case of a separate determination of PCDD/Fs and dioxin-like-PCBs the sum of the estimated expanded uncertainty of the separate analytical results of PCDD/Fs and dioxin-like PCBs has to be used for the estimated expanded uncertainty of the sum of PCDD/Fs and dioxin-like PCBs,

—	by establishing the decision limit (CCα) according to the provisions of Decision 2002/657/EC (point 3.1.2.5 of the Annex I to that Decision — the case of substances with established permitted level) a lot or sublot is non-compliant if the measured value is equal to or above the CCα.

The abovementioned rules shall apply for the analytical result obtained on the sample for official control. In case of analysis for defence or reference purposes, the national rules apply.

V.   EXCEEDANCE OF ACTION LEVELS

Action levels serve as tool for selection of samples in those cases where it is appropriate to identify a source of contamination and to take measures for its reduction or elimination. Screening methods shall establish appropriate cut-off values for selection of these samples. In case significant efforts are necessary to identify a source and to reduce or eliminate the contamination, it might be appropriate to confirm exceedance of the action level by duplicate sample analysis using a confirmatory method and taking into account the measurement uncertainty (3).

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(1)  http://ec.europa.eu/food/food/chemicalsafety/contaminants/dioxins_en.htm

(2)  The duplicate analysis is necessary if the result of the first determination applying confirmatory methods with the use of 13C-labelled internal standard for the relevant analytes is not compliant. The duplicate analysis is necessary to exclude the possibility of internal cross-contamination or an accidental mix-up of samples. In case the analysis is performed in the frame of a contamination incident, confirmation by duplicate analysis might be omitted in case the samples selected for analysis are through traceability linked to the contamination incident and the level found is significantly above the maximum level.

(3)  Identical explanation and requirements for duplicate analysis for control of action levels as in footnote (*) for maximum levels.

ANNEX III

SAMPLE PREPARATION AND REQUIREMENTS FOR METHODS OF ANALYSIS USED IN CONTROL OF THE LEVELS OF DIOXINS (PCDD/PCDF) AND DIOXIN-LIKE PCBS IN CERTAIN FOODSTUFFS

1.   FIELD OF APPLICATION

The requirements set out in this Annex shall be applied where foodstuffs are analysed for the official control of the levels of 2,3,7,8-substituted polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofurans (PCDD/Fs) and dioxin-like polychlorinated biphenyls (dioxin-like PCBs) and for other regulatory purposes.

Monitoring for the presence of PCDD/Fs and dioxin-like PCBs in foodstuffs may be performed with two different types of analytical methods:

(a)

Screening methods The goal of screening methods is to select those samples with levels of PCDD/Fs and dioxin-like PCBs that exceed the maximum levels or the action levels. Screening methods should allow cost-effective high sample-throughput, thus increasing the chance to discover new incidents with high exposure and health risks of consumers. Their application should aim at avoiding false-compliant results. They may comprise bioanalytical and GC/MS methods. Screening methods compare the analytical result with a cut-off value, providing a yes/no-decision over possible exceedance of the maximum or action level. The concentration of PCDD/Fs and the sum of PCDD/Fs and dioxin-like PCBs in samples suspected to be non-compliant with the maximum level must be determined/confirmed by a confirmatory method. In addition, screening methods may give an indication of the levels of PCDD/Fs and dioxin-like PCBs present in the sample. In case of application of bioanalytical screening methods the result is expressed as Bioanalytical Equivalents (BEQ), whereas in case of application of physico-chemical GC-MS methods it is expressed as Toxic Equivalents (TEQ). The numerically indicated results of screening methods are suitable for demonstrating compliance or suspected non-compliance or exceedance of action levels and give an indication of the range of levels in case of follow-up by confirmatory methods. They are not suitable for purposes such as evaluation of background levels, estimation of intake, following of time trends in levels or re-evaluation of action and maximum levels.

(b)

Confirmatory methods Confirmatory methods allow the unequivocal identification and quantification of PCDD/Fs and dioxin-like PCBs present in a sample and provide full information on congener basis. Therefore, these methods allow the control of maximum and action levels, including the confirmation of results obtained by screening methods. Furthermore, results may be used for other purposes such as determination of low background levels in food monitoring, following of time trends, exposure assessment of the population and building of database for possible re-evaluation of action and maximum levels. They are also important for establishing congener patterns in order to identify the source of a possible contamination. Such methods utilise GC-HRMS. For confirming compliance or non-compliance with the maximum level, also GC-MS/MS can be used.

2.   BACKGROUND

For calculation of Toxic Equivalents (TEQ) concentrations, the concentrations of the individual substances in a given sample shall be multiplied by their respective Toxic Equivalency Factor (TEF), as established by the World Health Organization and listed in the Appendix to this Annex, and subsequently summed to give the total concentration of dioxin-like compounds expressed as TEQs.

Screening and confirmatory methods may only be applied for control of a certain matrix if the methods are sensitive enough to detect levels reliably at the maximum or action level.

3.   QUALITY ASSURANCE REQUIREMENTS

—	Measures must be taken to avoid cross-contamination at each stage of the sampling and analysis procedure.

—	The samples must be stored and transported in glass, aluminium, polypropylene or polyethylene containers suitable for storage without any influence on the levels of PCDD/Fs and dioxin-like PCBs in the samples. Traces of paper dust must be removed from the sample container.

—	The sample storage and transportation has to be performed in a way that maintains the integrity of the foodstuff sample.

—	Insofar as relevant, finely grind and mix thoroughly each laboratory sample using a process that has been demonstrated to achieve complete homogenisation (e.g. ground to pass a 1 mm sieve); samples have to be dried before grinding if moisture content is too high.

—	Control of reagents, glassware and equipment for possible influence of TEQ- or BEQ-based results is of general importance.

—	A blank analysis shall be performed by carrying out the entire analytical procedure omitting only the sample.

—

For bioanalytical methods, it is of great importance that all glassware and solvents used in analysis shall be tested to be free of compounds that interfere with the detection of target compounds in the working range. Glassware shall be rinsed with solvents or/and heated at temperatures suitable to remove traces of PCDD/Fs, dioxin-like compounds and interfering compounds from its surface.

—	Sample quantity used for the extraction must be sufficient to fulfil the requirements with respect to a sufficiently low working range including the concentrations of maximum or action levels.

—	The specific sample preparation procedures used for the products under consideration shall follow internationally accepted guidelines.

—

In the case of fish, the skin has to be removed as the maximum level applies to muscle meat without skin. However it is necessary that all remaining muscle meat and fat tissue on the inner side of the skin are carefully and completely scraped off from the skin and added to the sample to be analysed.

4.   REQUIREMENTS FOR LABORATORIES

—

In accordance with the provisions of Regulation (EC) No 882/2004 of the European Parliament and of the Council (1), laboratories shall be accredited by a recognised body operating in accordance with ISO Guide 58 to ensure that they are applying analytical quality assurance. Laboratories shall be accredited following the EN ISO/IEC 17025 standard.

—	Laboratory proficiency shall be proven by the continuous successful participation in interlaboratory studies for the determination of PCDD/Fs and dioxin-like PCBs in relevant food matrices and concentration ranges.

—	Laboratories applying screening methods for routine control of samples shall establish a close cooperation with laboratories applying the confirmatory method, both for quality control and confirmation of the analytical result of suspected samples.

5.   BASIC REQUIREMENTS TO BE MET BY ANALYTICAL PROCEDURE FOR DIOXINS (PCDD/FS) AND DIOXIN-LIKE PCBS

5.1.   Low working range and limits of quantification

—

For PCDD/Fs, detectable quantities have to be in the upper femtogram (10– 15 g) range because of extreme toxicity of some of these compounds. For most PCB congeners limit of quantification in the nanogram (10– 9 g) range is already sufficient. However, for the measurement of the more toxic dioxin-like PCB congeners (in particular non-ortho substituted congeners) the lower end of the working range must reach the low picogram (10– 12 g) levels.

5.2.   High selectivity (specificity)

—

A distinction is required between PCDD/Fs and dioxin-like PCBs and a multitude of other, coextracted and possibly interfering compounds present at concentrations up to several orders of magnitude higher than those of the analytes of interest. For gas chromatography/mass spectrometry (GC-MS) methods, a differentiation among various congeners is necessary, such as between toxic (e.g. the seventeen 2,3,7,8-substituted PCDD/Fs, and twelve dioxin-like PCBs) and other congeners.

—	Bioanalytical methods shall be able to detect the target compounds as the sum of PCDD/Fs, and/or dioxin-like PCBs. Sample clean-up shall aim at removing compounds causing false-non-compliant results or compounds that may decrease the response, causing false-compliant results.

5.3.   High accuracy (trueness and precision, bioassay apparent recovery)

—

For GC-MS methods, the determination shall provide a valid estimate of the true concentration in a sample. High accuracy (accuracy of the measurement: the closeness of the agreement between the result of a measurement with the true or assigned value of the measurand) is necessary to avoid the rejection of a sample analysis result on the basis of poor reliability of the determined TEQ level. Accuracy is expressed as trueness (difference between the mean value measured for an analyte in a certified material and its certified value, expressed as percentage of this value) and precision (RSDR relative standard deviation calculated from results generated under reproducibility conditions).

—	For bioanalytical methods, the bioassay apparent recovery shall be determined.

5.4.   Validation in the range of maximum level and general quality control measures

—	Laboratories shall demonstrate the performance of a method in the range of the maximum level, e.g. 0,5 ×, 1 × and 2 × the maximum level with an acceptable coefficient of variation for repeated analysis, during the validation procedure and/or during routine analysis.

—

Regular blank controls and spiking experiments or analysis of control samples (preferably, if available, certified reference material) shall be performed as internal quality control measures. Quality control (QC) charts for blank controls, spiking experiments or analysis of control samples shall be recorded and checked to make sure the analytical performance is in accordance with the requirements.

5.5.   Limit of quantification

—

For a bioanalytical screening method, establishment of the LOQ is not an indispensable requirement but the method shall prove that it can differentiate between the blank and the cut-off value. When providing a BEQ-level, a reporting level shall be established to deal with samples showing a response below this level. The reporting level shall be demonstrated to be different from procedure blank samples at least by a factor of three, with a response below the working range. It shall therefore be calculated from samples containing the target compounds around the required minimum level, and not from a S/N ratio or an assay blank.

—	Limit of quantification (LOQ) for a confirmatory method shall be about one fifth of the maximum level.

5.6.   Analytical criteria

—

For reliable results from confirmatory or screening methods, the following criteria must be met in the range of the maximum level or action level for the TEQ value respectively the BEQ value, whether determined as total TEQ (as sum of PCDD/F and dioxin-like PCBs) or separately for PCDD/F and dioxin-like PCBs.   Screening with bioanalytical or physico-chemical methods Confirmatory methods False-compliant rate (2) < 5 %   Trueness   – 20 % to + 20 % Repeatability (RSDr) < 20 %   Within-laboratory reproducibility (RSDR) < 25 % < 15 %

5.7.   Specific requirements for screening methods

—	Both GC-MS and bioanalytical methods may be used for screening. For GC-MS methods the requirements as laid down in point 6 of this Annex are to be used. For cell based bioanalytical methods specific requirements are laid down in point 7 of this Annex.

—	Laboratories applying screening methods for routine control of samples shall establish a close cooperation with laboratories applying the confirmatory method.

—	Performance verification of the screening method is required during routine analysis, by analytical quality control and on-going method validation. There must be a continuous programme for control of compliant results.

—

Check on possible suppression of the cell response and cytotoxicity 20 % of the sample extracts shall be measured in routine screening without and with 2,3,7,8-TCDD added corresponding to the maximum or action level, to check if the response is possibly suppressed by interfering substances present in the sample extract. The measured concentration of the spiked sample is compared to the sum of the concentration of the unspiked extract plus the spiking concentration. If this measured concentration is more than 25 % lower than the calculated (sum) concentration, this is an indication of a potential signal suppression and the respective sample must be submitted to confirmatory analysis. Results shall be monitored in quality control charts.

—	Quality control on compliant samples Approximately 2 to 10 % of the compliant samples, depending on sample matrix and laboratory experience, shall be confirmed.

—

Determination of false-compliant rates from QC data The rate of false-compliant results from screening of samples below and above the maximum level or the action level shall be determined. Actual false-compliant rates shall be below 5 %. After a minimum of 20 confirmed results per matrix/matrix group is available from the quality control of compliant samples, conclusions on the false-compliant rate shall be drawn from this database. The results from samples analysed in ring trials or during contamination incidents, covering a concentration range up to e.g. 2 × the maximum level (ML), may also be included in the minimum of 20 results for evaluation of the false-compliant rate. The samples shall cover most frequent congener patterns, representing various sources. Although screening assays shall preferentially aim at detecting samples exceeding the action level, the criterion for determining false-compliant rates is the maximum level, taking into account the measurement uncertainty of the confirmatory method.

—

Potential non-compliant results from screening shall always be verified by a full re-analysis of the original sample by a confirmatory method. These samples may also be used to evaluate the rate of false-non-compliant results. For screening methods, the rate of ‘false-non-compliant results’ is the fraction of results confirmed to be compliant from confirmatory analysis, while in previous screening the sample had been declared to be suspected to be non-compliant. However, evaluation of the advantageousness of the screening method shall be based on comparison of false-non-compliant samples with the total number of samples checked. This rate shall be low enough to make the use of a screening tool advantageous.

—	At least under validation conditions, bioanalytical methods shall provide a valid indication of the TEQ level, calculated and expressed as BEQ.

—	Also for bioanalytical methods carried out under repeatability conditions, the intra-laboratory RSDr would typically be smaller than the reproducibility RSDR.

6.   SPECIFIC REQUIREMENTS FOR GC-MS METHODS TO BE COMPLIED WITH FOR SCREENING OR CONFIRMATORY PURPOSES

6.1.   Acceptable differences between upperbound and lowerbound WHO-TEQ levels

—	The difference between upperbound level and lowerbound level shall not exceed 20 % for confirmation of the exceedance of maximum or in case of need of action levels.

6.2.   Control of recoveries

—

Addition of 13C-labelled 2,3,7,8-chlorine substituted internal PCDD/F standards and of 13C-labelled internal dioxin-like PCB standards must be carried out at the very beginning of the analytical method e.g. prior to extraction in order to validate the analytical procedure. At least one congener for each of the tetra- to octa-chlorinated homologous groups for PCDD/Fs and at least one congener for each of the homologous groups for dioxin-like PCBs must be added (alternatively, at least one congener for each mass spectrometric selected ion recording function used for monitoring PCDD/Fs and dioxin-like PCBs). In case of confirmatory methods, all 17 13C-labelled 2,3,7,8-substituted internal PCDD/F standards and all 12 13C-labelled internal dioxin-like PCB standards shall be used.

—	Relative response factors shall also be determined for those congeners for which no 13C-labelled analogue is added by using appropriate calibration solutions.

—

For foodstuffs of plant origin and foodstuffs of animal origin containing less than 10 % fat, the addition of the internal standards is mandatory prior to extraction. For foodstuffs of animal origin containing more than 10 % fat, the internal standards may be added either before or after fat extraction. An appropriate validation of the extraction efficiency shall be carried out, depending on the stage at which internal standards are introduced and on whether results are reported on product or fat basis.

—	Prior to GC-MS analysis, 1 or 2 recovery (surrogate) standard(s) must be added.

—

Control of recovery is necessary. For confirmatory methods, the recoveries of the individual internal standards shall be in the range of 60 to 120 %. Lower or higher recoveries for individual congeners, in particular for some hepta- and octa- chlorinated dibenzo-p-dioxins and dibenzofurans, are acceptable on the condition that their contribution to the TEQ value does not exceed 10 % of the total TEQ value (based on sum of PCDD/F and dioxin-like PCBs). For GC-MS screening methods, the recoveries shall be in the range of 30 to 140 %.

6.3.   Removal of interfering substances

—	Separation of PCDD/Fs from interfering chlorinated compounds such as non-dioxin-like PCBs and chlorinated diphenyl ethers shall be carried out by suitable chromatographic techniques (preferably with a florisil, alumina and/or carbon column).

—	Gas-chromatographic separation of isomers shall be sufficient (< 25 % peak to peak between 1,2,3,4,7,8-HxCDF and 1,2,3,6,7,8-HxCDF).

6.4.   Calibration with standard curve

—	The range of the calibration curve shall cover the relevant range of maximum or action levels.

6.5.   Specific criteria for confirmatory methods

—

For GC-HRMS: — In HRMS, the resolution shall typically be greater than or equal to 10 000 for the entire mass range at 10 % valley. — Fulfilment of further identification and confirmation criteria as described in internationally recognised standards, for example, in standard EN 16215:2012 (Animal feed — Determination of dioxins and dioxin-like PCBs by GC/HRMS and of indicator PCBs by GC/HRMS) and/or in EPA methods 1613 and 1668 as revised.

—

For GC-MS/MS: — Monitoring of at least 2 specific precursor ions, each with one specific corresponding transition product ion, for all labelled and unlabelled analytes in the scope of analysis. — Maximum permitted tolerance of relative ion intensities of ± 15 % for selected transition product ions in comparison to calculated or measured values (average from calibration standards), applying identical MS/MS conditions, in particular collision energy and collision gas pressure, for each transition of an analyte. — Resolution for each quadrupole to be set equal to or better than unit mass resolution (unit mass resolution: sufficient resolution to separate two peaks one mass unit apart) in order to minimise possible interferences on the analytes of interest. — Fulfilment of the further criteria as described in internationally recognised standards, for example, in standard EN 16215:2012 (Animal feed — Determination of dioxins and dioxin-like PCBs by GC/HRMS and of indicator PCBs by GC/HRMS) and/or in EPA methods 1613 and 1668 as revised, except the obligation to use GC-HRMS.

7.   SPECIFIC REQUIREMENTS FOR BIOANALYTICAL METHODS

Bioanalytical methods are methods based on the use of biological principles like cell-based assays, receptor-assays or immunoassays. This point 7 establishes requirements for bioanalytical methods in general.

A screening method in principle classifies a sample as compliant or suspected to be non-compliant. For this, the calculated BEQ level is compared to the cut-off value (see 7.3). Samples below the cut-off value are declared compliant, samples equal or above the cut-off value as suspected to be non-compliant, requiring analysis by a confirmatory method. In practice, a BEQ level corresponding to 2/3 of the maximum level may serve as cut-off value provided that a false-compliant rate below 5 % and an acceptable rate for false-non-compliant results are ensured. With separate maximum levels for PCDD/Fs and for the sum of PCDD/Fs and dioxin-like PCBs, checking compliance of samples without fractionation requires appropriate bioassay cut-off values for PCDD/Fs. For checking of samples exceeding the action levels, an appropriate percentage of the respective action level would suit as cut-off value.

Furthermore, in the case of certain bioanalytical methods, an indicative level expressed in BEQs may be given for samples in the working range and exceeding the reporting limit (see 7.1.1 and 7.1.6).

7.1.   Evaluation of the test response

7.1.1.   General requirements

—

When calculating the concentrations from a TCDD calibration curve, values at the lower and higher end of the curve will show a high variation (high coefficient of variation (CV)). The working range is the area where this CV is smaller than 15 %. The lower end of the working range (reporting limit) must further be set significantly (at least by a factor of three) above the procedure blanks. The upper end of theworking range is usually represented by the EC70 value (70 % of maximal effective concentration), but lower if the CV is higher than 15 % in this range. The working range shall be established during validation. Cut-off values (7.3) must be well within the working range.

—	Standard solutions and sample extracts shall be tested at least in duplicate. When using duplicates, a standard solution or a control extract tested in 4 to 6 wells divided over the plate shall produce a response or concentration (only possible in the working range) based on a CV < 15 %.

7.1.2.   Calibration

7.1.2.1.   Calibration with standard curve

—	Levels in samples may be estimated by comparison of the test response with a calibration curve of TCDD (or PCB 126 or a PCDD/F/dioxin-like PCB standard mixture) to calculate the BEQ level in the extract and subsequently in the sample.

—

Calibration curves shall contain 8 to 12 concentrations (at least in duplicates), with enough concentrations in the lower part of the curve (working range). Special attention shall be paid to the quality of the curve-fit in the working range. As such, the R2 value is of little or no value in estimating the goodness of fit in non-linear regression. A better fit will be achieved by minimising the difference between calculated and observed levels in the working range of the curve (e.g. by minimising the sum of squared residuals).

—

The estimated level in the sample extract is subsequently corrected for the BEQ level calculated for a matrix/solvent blank sample (to account for impurities from solvents and chemicals used), and the apparent recovery (calculated from the BEQ level of suitable reference samples with representative congener patterns around the maximum or action level). For performing a recovery correction, the apparent recovery must always be within the required range (see point 7.1.4). Reference samples used for recovery correction must comply with requirements as given in point 7.2.

7.1.2.2.   Calibration with reference samples

Alternatively, a calibration curve prepared from at least 4 reference samples (see point 7.2): one matrix blank, plus three reference samples at 0,5 ×, 1,0 × and 2,0 × the maximum or action level may be used, eliminating the need to correct for blank and recovery. In this case, the test response corresponding to 2/3 of the maximum level (see 7.3) may be calculated directly from these samples and used as cut-off value. For checking of samples exceeding the action levels, an appropriate percentage of these action levels would suit as cut-off value.

7.1.3.   Separate determination of PCDD/Fs and dioxin-like PCBs

Extracts may be split into fractions containing PCDD/Fs and dioxin-like PCBs, allowing a separate indication of PCDD/Fs and dioxin-like PCB TEQ levels (in BEQs). A PCB 126 standard calibration curve shall preferentially be used to evaluate results for the fraction containing dioxin-like PCBs.

7.1.4.   Bioassay apparent recoveries

The ‘bioassay apparent recovery’ shall be calculated from suitable reference samples with representative congener patterns around the maximum or action level and expressed as percentage of the BEQ level in comparison to the TEQ level. Depending on the type of assay and TEFs (3) used, the differences between TEF and REP factors for dioxin-like PCBs may cause low apparent recoveries for dioxin-like PCBs in comparison to PCDD/Fs. Therefore, if a separate determination of PCDD/Fs and dioxin-like PCBs is performed, bioassay apparent recoveries shall be: for dioxin-like PCBs 20 % to 60 %, for PCDD/Fs 50 % to 130 % (ranges apply for TCDD calibration curve). As the contribution of dioxin-like PCBs to the sum of PCDD/Fs and dioxin-like PCBs may vary between different matrices and samples, bioassay apparent recoveries for the sum parameter reflect these ranges and shall be between 30 % to 130 %.

7.1.5.   Control of recoveries for clean-up

The loss of compounds during the clean-up shall be checked during validation. A blank sample spiked with a mixture of the different congeners shall be submitted to clean-up (at least n=3) and the recovery and variability checked by a confirmatory method. The recovery shall be within 60 to 120 % especially for congeners contributing more than 10 % to the TEQ-level in various mixtures.

7.1.6.   Reporting Limit

When reporting BEQ levels, a reporting limit shall be determined from relevant matrix samples involving typical congener patterns, but not from the calibration curve of the standards due to low precision in the lower range of the curve. Effects from extraction and clean-up must be taken into account. The reporting limit must be set significantly (at least by a factor of three) above the procedure blanks.

7.2.   Use of reference samples

—	Reference samples shall represent sample matrix, congener patterns and concentration ranges for PCDD/Fs and dioxin-like PCBs around the maximum or action level.

—

A procedure blank, or preferably a matrix blank, and a reference sample at the maximum or action level have to be included in each test series. These samples must be extracted and tested at the same time under identical conditions. The reference sample must show a clearly elevated response in comparison to the blank sample, thus ensuring the suitability of the test. These samples may be used for blank and recovery corrections.

—	Reference samples chosen for performing a recovery correction shall be representative for the test samples, meaning that congener patterns shall not lead to an underestimation of levels.

—

Extra reference samples at e.g. 0,5 × and 2 × the maximum or action level may be included to demonstrate the proper performance of the test in the range of interest for the control of the maximum or action level. Combined, these samples may be used for calculating the BEQ-levels in test samples (7.1.2.2).

7.3.   Determination of cut-off values

The relationship between bioanalytical results in BEQ and results from confirmatory methods in TEQ shall be established (e.g. by matrix-matched calibration experiments, involving reference samples spiked at 0, 0,5 ×, 1 × and 2 × the maximum level (ML), with 6 repetitions on each level (n=24)). Correction factors (blank and recovery) may be estimated from this relationship but shall be checked in each test series by including procedure/matrix blanks and recovery samples (7.2).

Cut-off values shall be established for decision over sample compliance with maximum levels or for control of action levels, if of interest, with the respective maximum or action levels set for either PCDD/Fs and dioxin-like PCBs alone, or for the sum of PCDD/Fs and dioxin-like PCBs. They are represented by the lower endpoint of the distribution of bioanalytical results (corrected for blank and recovery) corresponding to the decision limit of the confirmatory method based on a 95 % level of confidence, implying a false-compliant rate < 5 %, and on a RSDR < 25 %. The decision limit of the confirmatory method is the maximum level, taking into account the measurement uncertainty.

In practice, the cut-off value (in BEQ) may be calculated from the following approaches (see Figure 1):

7.3.1.   Use of the lower band of the 95 % prediction interval at the decision limit of the confirmatory method

with:

BEQDL	BEQ corresponding to the decision limit of the confirmatory method, being the ML including measurement uncertainty
sy,x	residual standard deviation
tα,f=m – 2	Student factor (α = 5 %, f = degrees of freedom, single-sided)
m	total number of calibration points (index j)
n	number of repetitions on each level
x i	Sample concentration (in TEQ) of calibration point i determined by a confirmatory method
	mean of the concentrations (in TEQ) of all calibration samples

Qxx	=
i	=	index for calibration point i

7.3.2.   Calculation from bioanalytical results (corrected for blank and recovery) of multiple analyses of samples (n ≥ 6) contaminated at the decision limit of the confirmatory method, as the lower endpoint of the data distribution at the corresponding mean BEQ value:

with

SDR	standard deviation of bioassay results at BEQDL, measured under within-laboratory reproducibility conditions

7.3.3.   Calculation as mean value of bioanalytical results (in BEQ, corrected for blank and recovery) from multiple analysis of samples (n > 6) contaminated at 2/3 of the maximum or action level. This is based on the observation that this level will be around the cut-off determined under 7.3.1 or 7.3.2.

Figure 1

Calculation of cut-off values based on a 95 % level of confidence implying a false-compliant rate < 5 %, and a RSDR < 25 %:

1.	from the lower band of the 95 % prediction interval at the decision limit of the confirmatory method,

2.	from multiple analysis of samples (n ≥ 6) contaminated at the decision limit of the confirmatory method as the lower endpoint of the data distribution (represented in the figure by a bell-shaped curve) at the corresponding mean BEQ value.

7.3.4.   Restrictions to cut-off values:

BEQ-based cut-off values calculated from the RSDR achieved during validation using a limited number of samples with different matrix/congener patterns may be higher than the TEQ-based maximum or action levels due to a better precision than attainable in routine when an unknown spectrum of possible congener patterns has to be controlled. In such cases, cut-off values shall be calculated from an RSDR = 25 %, or two-thirds of the maximum or action level shall be preferred.

7.4.   Performance characteristics

—

Since no internal standards can be used in bioanalytical methods, tests on repeatability shall be carried out to obtain information on the standard deviation within and between test series. Repeatability shall be below 20 %, intra-laboratory reproducibility below 25 %. This shall be based on the calculated levels in BEQs after blank and recovery correction.

—	As part of the validation process, the test must be shown to discriminate between a blank sample and a level at the cut-off value, allowing the identification of samples above the corresponding cut-off value (see 7.1.2).

—	Target compounds, possible interferences and maximum tolerable blank levels shall be defined.

—	The percent standard deviation in the response or concentration calculated from the response (only possible in working range) of a triplicate determination of a sample extract shall not be above 15 %.

—	The uncorrected results of the reference sample(s) expressed in BEQs (blank and at the maximum or action level) shall be used for evaluation of the performance of the bioanalytical method over a constant time period.

—

Quality control (QC) charts for procedure blanks and each type of reference sample shall be recorded and checked to make sure the analytical performance is in accordance with the requirements, in particular for the procedure blanks with regard to the requested minimum difference to the lower end of the working range and for the reference samples with regard to within-laboratory reproducibility. Procedure blanks must be well controlled in order to avoid false-compliant results when subtracted.

—

The results from the confirmatory methods of suspected samples and 2 to 10 % of the compliant samples (minimum of 20 samples per matrix) shall be collected and used to evaluate the performance of the screening method and the relationship between BEQs and TEQs. This database might be used for re-evaluation of cut-off values applicable to routine samples for the validated matrices.

—

Successful method performance may also be demonstrated by participation in ring trials. The results from samples analysed in ring trials, covering a concentration range up to e.g. 2 × ML, may also be included in the evaluation of the false-compliant rate, if a laboratory is able to demonstrate its successful performance. The samples shall cover most frequent congener patterns, representing various sources.

—	During incidents, the cut-off values may be re-evaluated, reflecting the specific matrix and congener patterns of this single incident.

8.   REPORTING OF THE RESULT

Confirmatory methods

—

Insofar as the used analytical procedure makes it possible, the analytical results shall contain the levels of the individual PCDD/F and dioxin-like PCB congeners and be reported as lower-bound, upper-bound and medium-bound in order to include a maximum of information in the reporting of the results and thereby enabling the interpretation of the results according to specific requirements.

—

The report shall also include the method used for extraction of PCDD/Fs, dioxin-like PCBs and lipids. The lipid content of the sample shall be determined and reported for food samples with maximum levels expressed on fat basis and an expected fat concentration in the range of 0 — 2 % (in correspondence to existing legislation), for other samples is the determination of the lipid content optional.

—	The recoveries of the individual internal standards must be made available in case the recoveries are outside the range mentioned in point 6.2, in case the maximum level is exceeded (in this case, the recoveries for one of the two duplicate analysis) and in other cases upon request.

—

As the uncertainty of measurement is to be taken into account when deciding about the compliance of a sample, this parameter shall also be made available. Thus, analytical results shall be reported as x +/– U whereby x is the analytical result and U is the expanded measurement uncertainty using a coverage factor of 2 which gives a level of confidence of approximately 95 %. In case of a separate determination of PCDD/Fs and dioxin-like-PCBs the sum of the estimated expanded uncertainty of the separate analytical results of PCDD/Fs and dioxin-like PCBs has to be used for the sum of PCDD/Fs and dioxin-like PCBs.

—	If the uncertainty of measurement is taken into account by applying CCα (as described in Annex II, point IV.2), this parameter shall be reported.

—	The results shall be expressed in the same units and with (at least) the same number of significant figures as the maximum levels laid down in Regulation (EC) No 1881/2006.

Bioanalytical screening methods

—	The result of the screening shall be expressed as compliant or suspected to be non-compliant (suspected).

—	In addition, a result for PCDD/F and/or dioxin-like PCBs expressed in Bioanalytical Equivalents (BEQ) (not TEQ) may be given (see Annex III, point 1). Samples with a response below the reporting limit shall be expressed as lower than the reporting limit.

—	For each type of sample matrix, the report shall mention the maximum or action level on which the evaluation is based.

—	The report shall mention the type of test applied, the basic test principle and kind of calibration.

—

The report shall also include the method used for extraction of PCDD/Fs, dioxin-like PCBs and lipids. The lipid content of the sample shall be determined and reported for food samples with maximum or action levels expressed on fat basis and an expected fat concentration in the range of 0 — 2 % (in correspondence to existing legislation), for other samples is the determination of the lipid content optional.

—	In case of samples suspected to be non-compliant, the report needs to include a note on the action to be taken. The concentration of PCDD/Fs and the sum of PCDD/Fs and dioxin-like PCBs in those samples with elevated levels has to be determined/confirmed by a confirmatory method.

---

(1)  Regulation (EC) No 882/2004 of the European Parliament and of the Council of 29 April 2004 on official controls performed to ensure the verification of compliance with feed and food law, animal health and animal welfare rules (OJ L 165, 30.4.2004, p. 1).

(2)  With respect to the maximum levels.

(3)  Current requirements are based on the TEFs published in: M. Van den Berg et al, Toxicol Sci 93 (2), 223–241 (2006).

ANNEX IV

SAMPLE PREPARATION AND REQUIREMENTS FOR METHODS OF ANALYSIS USED IN CONTROL OF THE LEVELS OF NON-DIOXIN-LIKE PCBS (PCB # 28, 52, 101, 138, 153, 180) IN CERTAIN FOODSTUFFS

The requirements set out in this Annex shall be applied where foodstuffs are analysed for the official control of the levels of non-dioxin-like polychlorinated biphenyls (non-dioxin-like PCBs) and for other regulatory purposes.

1.   Applicable detection methods:

Gas Chromatography/Electron Capture Detection (GC-ECD), GC-LRMS, GC-MS/MS, GC-HRMS or equivalent methods.

2.   Identification and confirmation of analytes of interest:

—	Relative retention time in relation to internal standards or reference standards (acceptable deviation of +/– 0,25 %).

—

Gas chromatographic separation of all six indicator PCBs (PCB 28, PCB 52, PCB 101, PCB 138, PCB 153 and PCB 180) from interfering substances, especially co-eluting PCBs, in particular if levels of samples are in the range of legal limits and non-compliance is to be confirmed. (Congeners often found to co-elute are e.g. PCB 28/31, PCB 52/69 and PCB 138/163/164. For GC-MS also possible interferences from fragments of higher chlorinated congeners have to be considered.)

—

For GC-MS techniques: — Monitoring of at least: — two specific ions for HRMS, — two specific ions of m/z > 200 or three specific ions of m/z >100 for LRMS, — 1 precursor and 2 product ions for MS-MS. — Maximum permitted tolerances for abundance ratios for selected mass fragments: Relative deviation of abundance ratio of selected mass fragments from theoretical abundance or calibration standard for target ion (most abundant ion monitored) and qualifier ion(s): Relative intensity of qualifier ion(s) compared to target ion GC-EI-MS (relative deviation) GC-CI-MS, GC-MSn (relative deviation) > 50 % ± 10 % ± 20 % > 20 % to 50 % ± 15 % ± 25 % > 10 % to 20 % ± 20 % ± 30 % ≤ 10 % ± 50 % (1) ± 50 % (1)

—	For GC-ECD: Confirmation of results exceeding the tolerance with two GC columns with stationary phases of different polarity.

3.   Demonstration of performance of method:

Validation in the range of the maximum level (0,5 to 2 times the maximum level) with an acceptable coefficient of variation for repeated analysis (see requirements for intermediate precision in point 8).

4.   Limit of quantification:

The blank values shall not be higher than 30 % of the level of contamination corresponding to the maximum level (2).

5.   Quality control:

Regular blank controls, analysis of spiked samples, quality control samples, participation in interlaboratory studies on relevant matrices.

6.   Control of recoveries:

—	Use of suitable internal standards with physico-chemical properties comparable to analytes of interest.

—	Addition of internal standards: — Addition to products (before extraction and clean-up process); — Addition also possible to extracted fat (before clean-up process), if maximum level is expressed on fat basis.

—

Requirements for methods using all six isotope-labelled indicator PCB congeners: — Correction of results for recoveries of internal standards; — Generally acceptable recoveries of isotope-labelled internal standards are between 50 and 120 %; — Lower or higher recoveries for individual congeners with a contribution to the sum of the six indicator PCBs below 10 % are acceptable.

—

Requirements for methods using not all six isotope-labelled internal standards or other internal standards: — Control of recovery of internal standard(s) for every sample; — Acceptable recoveries of internal standard(s) between 60 and 120 %; — Correction of results for recoveries of internal standards.

—	The recoveries of unlabelled congeners shall be checked by spiked samples or quality control samples with concentrations in the range of the maximum level. Acceptable recoveries for these congeners are between 70 and 120 %.

7.   Requirements for laboratories:

In accordance with the provisions of Regulation (EC) No 882/2004, laboratories shall be accredited by a recognised body operating in accordance with ISO Guide 58 to ensure that they are applying analytical quality assurance. Laboratories shall be accredited following the EN ISO/IEC 17025 standard.

8.   Performance characteristics: Criteria for the sum of the six indicator PCBs at the maximum level:

Trueness	– 30 to + 30 %
Intermediate precision (RSD%)	≤ 20 %
Difference between upper and lower bound calculation	≤ 20 %

9.   Reporting of results

—

Insofar as the used analytical procedure makes it possible, the analytical results shall contain the levels of the individual PCB congeners and be reported as lower-bound, upper-bound and medium-bound in order to include a maximum of information in the reporting of the results and thereby enabling the interpretation of the results according to specific requirements.

—

The report shall also include the method used for extraction of PCBs and lipids. The lipid content of the sample shall be determined and reported for food samples with maximum levels expressed on fat basis and an expected fat concentration in the range of 0 — 2 % (in correspondence to existing legislation), for other samples is the determination of the lipid content optional.

—	The recoveries of the individual internal standards must be made available in case the recoveries are outside the range mentioned in point 6, in case the maximum level is exceeded and in other cases upon request.

—

As the uncertainty of measurement is to be taken into account when deciding about the compliance of a sample, this parameter shall also be made available. Thus, analytical results shall be reported as x +/– U whereby x is the analytical result and U is the expanded measurement uncertainty using a coverage factor of 2 which gives a level of confidence of approximately 95 %.

—	If the uncertainty of measurement is taken into account by applying CCα (as described in Annex II, point IV.1), this parameter shall be reported.

—	The results shall be expressed in the same units and with (at least) the same number of significant figures as the maximum levels laid down in Regulation (EC) No 1881/2006.

---

(1)  Sufficient number of mass fragments with relative intensity > 10 % available, therefore not recommendable to use qualifier ion(s) with a relative intensity of less than 10 % compared to the target ion.

(2)  It is highly recommendable to have a lower contribution of the reagent blank level to the level of a contaminant in a sample. It is in the responsibility of the laboratory to control the variation of blank levels, in particular, if the blank levels are subtracted.

ANNEX

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
0702 00 00	MK	64,8
	TR	64,5
	ZZ	64,7
0707 00 05	AL	25,2
	MK	40,7
	TR	121,6
	ZZ	62,5
0709 93 10	TR	114,5
	ZZ	114,5
0805 50 10	TR	121,8
	ZA	129,3
	ZZ	125,6
0808 10 80	AR	104,3
	BR	77,8
	CL	99,5
	CN	127,0
	NZ	137,5
	US	161,6
	UY	70,3
	ZA	120,5
	ZZ	112,3
0809 29 00	TR	444,9
	ZZ	444,9

---

(1)  Nomenclature of countries laid down by Commission Regulation (EC) No 1833/2006 (OJ L 354, 14.12.2006, p. 19). Code ‘ZZ’ stands for ‘of other origin’.

ANNEX

EU ECOLABEL CRITERIA AND ASSESSMENT AND VERIFICATION REQUIREMENTS

Criteria for awarding the EU Ecolabel to paints and varnishes:

1.	White pigment and wet scrub resistance

2.	Titanium dioxide

3.	Efficiency in use (a) Spreading rate (b) Resistance to water (c) Adhesion (d) Abrasion (e) Weathering (f) Water vapour permeability (g) Liquid water permeability (h) Fungal resistance (i) Crack bridging (j) Alkali resistance (k) Corrosion resistance

4.	Volatile and Semi-volatile Organic Compounds (VOCs, SVOCs)

5.	Restriction of hazardous substances and mixtures (a) Overall restrictions that apply to hazard classifications and risk phrases (b) Restrictions that apply to Substances of Very High Concern (c) Restrictions that apply to specific hazardous substances

6.	Consumer information

7.	Information appearing on the EU Ecolabel

The Ecolabel criteria reflect the best environmental performing products on the market of paints and varnishes. High quality and performance standards of the paint are required to ensure the longevity of the product and contribute that way to the significant reduction of the paints' overall life cycle impacts. Moreover, the criteria aim at minimizing the use of volatile and semi-volatile organic substances in the paint formulation.

Whilst the use of chemical products and release of pollutants is part of the production process, a product that bears the EU Ecolabel guarantees the consumer that the use of such substances has been limited to the extent technically possible without prejudice to its fitness for use. Moreover, the final paint or varnish product may not be classified as being an acute toxin or hazardous to the environment under European legislation on the labelling of products.

The criteria exclude whenever possible or restrict to a minimum the concentration (required for providing specific functions and properties) of a number of substances identified as hazardous to human health and the environment that may be used in the formulation of paints and varnishes. Only where a substance is required to meet consumer performance expectations or mandated requirements for the product (for instance paint preservation), and where there are no applied and tested available alternatives, derogation for such a substance to be used in the Ecolabel is granted.

Derogations are evaluated on the basis of the precautionary principle and scientific and technical evidence, especially if safer products are available on the market.

Testing of the final product for the presence of restricted hazardous substances may be requested in order to provide a high level of assurance to consumers.

Where appropriate, strict conditions are also imposed on the handling of substances in manufacturing processes for paints and varnishes to avoid workforce exposure. The verification of compliance with the criteria is formulated in a way that provides a high level of assurance to consumers, reflects the practical potential for applicants to obtain information from the supply chain and excludes the potential for ‘free riding’ by applicants.

Assessment and verification

(a)

Requirements The specific assessment and verification requirements are indicated within each criterion. Where the applicant is required to provide declarations, documentation, analyses, test reports, or other evidence to show compliance with the criteria, these may originate from the applicant and/or his supplier(s) and/or their supplier(s), as appropriate. In the case of changes such as in supplier, the paint formulation or an extension of a product range that results in a change in how the paint or varnish complies with one or more criteria (as relevant) then the licenseholder shall, in advance of any change, submit information to the relevant Competent Body demonstrating the products ongoing compliance as specified in the relevant criteria. Where appropriate, test methods other than those indicated for each criterion may be used if these are described in the user manual of the Ecolabel criteria application and the competent body assessing the application accepts their equivalence. Competent bodies shall preferentially recognise tests which are accredited according to ISO 17025 and verifications performed by bodies which are accredited under the EN 45011 standard or an equivalent international standard. Where appropriate, competent bodies may require supporting documentation and may carry out independent verifications.

(b)	Measurement thresholds Unless otherwise indicated compliance with the Ecolabel criteria is required for intentionally added substances and mixtures, as well as for by-products and impurities from raw materials, the concentration of which equals or exceeds 0,010 % by weight of final formulation.

(c)

The exact formulation of the product, including the function and the physical form of all ingredients identified within the criteria, as well as any additional functional ingredients, and their ingoing concentration shall be provided to the competent body. The chemical name, CAS number and CLP classification according to Regulation (EC) No 1272/2008 shall be provided for each ingredient. All ingredients identified within the criteria, as well as any additional functional ingredients and known impurities, that are present at concentrations in the product of greater than 0,010 % shall be reported unless a lower concentration is required in order to comply with a derogation requirement. Where ingredients are referred to in the criteria, this includes substances and preparations or mixtures. The definitions of ‘substances’ and ‘mixtures’ are given in Article 3 of Regulation (EC) No 1907/2006 of the European Parliament and of the Council (1) (‘the REACH Regulation’. Safety data sheets and/or CAS numbers and CLP classifications for each ingredient shall be submitted to the competent body in accordance with the REACH Regulation.

(d)

For all criteria, apart from Criterion 4 Volatile and Semi-volatile Organic Compounds (VOCs, SVOCs), the limits shall apply to the paint or varnish in its packaging. In line with Directive 2004/42/EC the VOC limits relate to the ready to use product and so the maximum VOC content shall be measured or calculated including any recommended additions such as colorants and/or thinners. For this calculation or measurement, data supplied by the raw material suppliers regarding solids content, VOC content and product density will be required. The above is also applicable in the measurement or calculation of SVOCs. Competent bodies may request testing for SVOC's in order to validate calculations.

Criterion 1. White pigment and Wet Scrub Resistance

1(a)   Minimum requirement for white pigment content

Indoor wall and ceiling paints for which Class 1 and 2 wet scrub resistance claims are made shall have a white pigment content (white inorganic pigments with a refractive index higher than 1,8) per m2 of dry film equal to or lower than that described in Table 1, with 98 % opacity. For tinting systems this requirement only applies to the base paint.

Table 1

Relationship between wet scrub resistance and TiO2 content for indoor paints

Wet scrub resistance	Indoor limit (g/m2)
Class 1	40
Class 2	36

For all other paints, including limed paints, silicate paints, primers, anti-rust paints and facade paints, the white pigment content (white inorganic pigments with a refractive index higher than 1,8) shall not exceed 36 g/m2 for indoor products and 38 g/m2 for outdoor products. In the case of paints for both indoor and outdoor use the more stringent limit shall apply.

In case the above mentioned products fall under the exemption indicated in part (b) then the white pigment content (white inorganic pigments with a refractive index higher than 1,8) shall not exceed 25 g/m2 of dry film, with 98 % opacity.

1(b)   Minimum requirement for Wet Scrub Resistance (for indoor paints only)

All indoor wall and ceiling paints (finishes) shall achieve class 1 or class 2 in wet scrub resistance (WSR) according to EN 13300 and EN ISO 11998. This requirement only applies to tinting bases (base paints).

Exempted from this requirement are indoor wall and ceiling paints with a white pigment content (white inorganic pigments with a refractive index higher than 1,8) that is equal or lower to 25 g/m2of dry film, with 98 % opacity.

Only WSR class 1 and 2 ecolabelled paints may claim wet scrub resistance on the label or other marketing documentation.

Assessment and verification: the requirements of both 1(a) and 1(b) shall be fulfilled. the applicant shall provide documentation showing that the content of white pigments is compliant with this criterion.

The applicant shall provide a test report according to EN 13300 using the method EN ISO 11998 (Test for cleanability and scrub resistance). For ceiling paints and indoor wall paints the labelling for the packaging, including the accompanying text, shall be provided as evidence regarding claims of wet scrub resistance.

Criterion 2. Titanium Dioxide pigment

If the product contains more than 3,0 % w/w of titanium dioxide, the emissions and discharges of wastes from the production of any titanium dioxide pigment used shall not exceed the following (2):

For the sulphate process:

—	SOx calculated as SO2 : 7,0 kg/tonne TiO2 pigment

—	Sulphate waste: 500 kg/tonne TiO2 pigment

For the chloride process:

—	If natural rutile ore is used, 103 kg chloride waste/tonne TiO2 pigment

—	If synthetic rutile ore is used: 179 kg chloride waste/tonne TiO2 pigment

—	If slag ore is used: 329 kg chloride waste/tonne TiO2 pigment

If more than one type of ore is used, the values will apply in proportion to the quantity of the individual ore types used.

Note:

SOx emissions only apply to the sulphate process.

The Waste Framework Directive 2008/98/EC of the European Parliament and of the Council (3), Article 3 shall be used for the definition of waste. If the TiO2 producer can satisfy Article 5 (by-product production) of the Waste Framework Directive for its solid wastes then, the wastes shall be exempted.

Assessment and verification: the applicant shall submit supporting documentation showing compliance by the titanium dioxide producer manufacturing the raw material for the paint product either in the form of a declaration of non-use or a declaration supported by data indicating that the respective levels of process emissions and waste discharges of wastes are met.

Criterion 3. Efficiency in use

In order to demonstrate the efficiency in use of paints and varnishes the following tests per type of paint and/or varnish, as indicated in Table 2, shall be undertaken:

Table 2

Performance requirements for different kind of paints and varnishes

Criteria	Paints and Varnishes (with their subcategories identified according to the Directive 2004/42/EC)
	Indoor paint (a, b)	Outdoor paint (c)	Trim and cladding (d)	Thick decorative coating indoor and outdoor (l)	Varnish and woodstain (e, f)	One pack performance and floor covering paint (i)	Primer (g)	Undercoat and primer (h)
3(a) Spreading rate (only for white and light coloured paints, including the white base paints used in tinting systems)) — ISO 6504/1	8 m2/L	4 m2/L (elastomeric paint) 6 m2/L (masonry paint)	Outdoor products 6 m2/L Indoor products 8 m2/L	1 m2/L	—	Outdoor products 6 m2/L Indoor products 8 m2/L	6 m2/L (without opacity) 8 m2/L (with opacity)	6 m2/L (without opacity) 8 m2/L (with opacity)
3(b) Resistance to water — ISO 2812-3	—	—	—	—	Resistant to water	Resistant to water	—	—
3(c) Adhesion — EN 24624		—	—	—	—	Score 2	1,5 MPa (masonry paint)	1,5 MPa (masonry paint)
3(d) Abrasion — EN ISO 7784-2	—	—	—	—	—	70 mg weight loss	—	—
3(e) Weathering — EN 11507/EN 927-6	—	1 000 h	1 000 h (outdoor)	1 000 h (outdoor)	1 000 h (outdoor)	1 000 h (outdoor)	—	—
3(f) Water vapour permeability (4) — EN ISO 7783	—	Class II or better	—	Class II or better (outdoor)	—	—	—	—
3(g) Liquid water permeability (4)	—	Where claims are made Class III	—	Class II or better (outdoor)	—	—	—	—
— EN 1062-3		All other products Class II or better
3(h) Fungal resistance (4) — EN 15457	—	Class 1 or lower (masonry or wood paints)	Class 0 (outdoor wood products)	Class 1 or lower (outdoor)	—	—	—	—
3(h) Algal resistance — EN 15458 (4)	—	Class 1 or lower (masonry or wood paints)	Class 0 (outdoor wood products)	Class 1 or lower (outdoor)	—	—	—	—
3(i) Crack bridging (4) — EN 1062-7	—	A1 (elastomeric paint only)	—	—	—	—	—	—
3(j) Alkali resistance — ISO 2812-4	—	Masonry paint	—	—	—	—	Outdoor for masonry	Outdoor for masonry
3(k) Corrosion resistance (4)	—	Anti-rust paint	Anti-rust paint	—	—	Anti-rust paint	Anti-rust paint	Anti-rust paint
EN ISO 12944-2 and 12944-6, ISO 9227, ISO 4628-2 and 4628-3		Blistering: ≥ size 3/density 3 Rusting: ≥ Ri2	Blistering: ≥ size 3/density 3 Rusting: ≥ Ri2			Blistering: ≥ size 3/density 3 Rusting: ≥ Ri2	Blistering: ≥ size 3/density 3 Rusting: ≥ Ri2	Blistering: ≥ size 3/density 3 Rusting: ≥ Ri2

3(a)   Spreading rate

Spreading rate requirement shall apply to white and light coloured paint products. For paints that are available in more colours the spreading rate shall apply to the lightest colour.

White paints and light-coloured paints (including finishes and intermediates) shall have a spreading rate (at a hiding power of 98 %) of at least 8 m2 per litre of product for indoor paints and 6 m2 for outdoor paints. Products marketed for both — indoor and outdoor shall have a spreading rate (at a hiding power of 98 %) of at least 8 m2 per litre.

For tinting systems, this criterion applies only to the white base (the base containing the most TiO2). In cases where the white base is unable to achieve this requirement, the criterion shall be met after tinting the white base to produce the standard colour RAL 9010.

For paints that are a part of a tinting system, the applicant must advise the end-user on the product packaging and POS which shade or primer/undercoat (if possible bearing the Community Eco-label) should be used as a basecoat before applying the darker shade.

Transparent and semi-transparent primers and undercoats shall have a spreading rate of at least 6 m2 and those with opacity at least 8 m2. Opaque primers with specific blocking/sealing, penetrating/binding properties and primers with special adhesion properties shall have a spreading rate of at least 6 m2 per litre of product.

Thick decorative coatings (paints that are specially designed to give a three-dimensional decorative effect and are therefore characterised by a very thick coat) shall alternatively have a spreading rate of 1 m2 per kg of product.

Opaque elastomeric paints shall have a spreading rate of at least 4 m2 per litre of product.

This requirement does not apply to varnishes, lasures, transparent adhesion primers or any other transparent coatings.

Assessment and verification: the applicant shall provide a test report using the method ISO 6504/1 (Paints and varnishes — determination of hiding power — Part 1: Kubelka-Munk method for white and light-coloured paints) or 6504/3 (Part 3: determination of contrast ratio (opacity) of light-coloured paints at a fixed spreading rate), or for paints specially designed to give a three-dimensional decorative effect and characterised by a very thick coat the method NF T 30 073. For bases used to produce tinted products not evaluated according to the abovementioned requirements, the applicant shall produce evidence of how the end-user will be advised to use a primer and/or grey (or other relevant shade) of undercoat before application of the product.

3(b)   Resistance to water

All varnishes, floor coatings and floor paints shall have resistance to water, as determined by ISO 2812-3 such that after 24 hours' exposure and 16 hours' recovery no change of gloss or of colour occurs.

Assessment and verification: the applicant shall provide a test report using the method ISO 2812-3.

3(c)   Adhesion

Pigmented masonry primers for exterior uses shall score a pass in the EN 24624 (ISO 4624) pull-off test where the cohesive strength of the substrate is less than the adhesive strength of the paint, otherwise the adhesion of the paint must be in excess of a pass value of 1,5 MPa.

Floor coatings, floor paints, floor undercoats, interior masonry primers, metal and wood undercoats shall score 2 or less in the EN 2409 test for adhesion.

Transparent primers are not included in this requirement.

The applicant shall evaluate the primer and/or finish alone or both applied together. When testing the finish alone this shall be considered the worst case scenario concerning adhesion.

Assessment and verification: the applicant shall provide a test report using the method EN ISO 2409 or EN 24624 (ISO 4624) as applicable.

3(d)   Abrasion

Floor coatings and floor paints shall have an abrasion resistance not exceeding 70 mg weight loss after 1000 test cycles with a 1000 g load and a CS10 wheel according to EN ISO 7784-2.

Assessment and verification: the applicant shall provide a test report showing compliance with this criterion using the method EN ISO 7784-2.

3(e)   Weathering (for outdoor paints and varnishes)

Masonry finish paints and wood and metal finishes including varnishes shall be exposed to artificial weathering in apparatus including fluorescent UV lamps and condensation or water spray according to ISO 11507. They shall be exposed to test conditions for 1000 hours. Test conditions are: UVA 4 h/60 °C + humidity 4 h/50 °C.

Alternatively, outdoor wood finishes and wood varnishes shall be exposed to weathering for 1000 hours in the QUV accelerated weathering apparatus with cyclic exposure with UV(A) radiation and spraying according to EN 927-6.

According to ISO 7724 3, the colour change of samples exposed to weathering shall not be greater than ΔΕ * = 4. It is not applicable to varnishes and bases.

Decrease of gloss for gloss paints and varnishes exposed to weathering shall not be greater than 30 % of its initial value and shall be measured using ISO 2813. This requirement is not applicable to mid sheen and matt-finishes (5)which have an initial gloss value less than 60 % at 60o angle of incidence.

Chalking shall be tested using method EN ISO 4628-6 on masonry finish coats and wood and metal finishes (where applicable) after the samples have been exposed to weathering. Coatings shall achieve a score of 1,5 or better (0,5 or 1,0) in this test. In the standard there are illustrated references.

The following parameters shall also be evaluated on masonry finish coats and wood and metal finishes after the samples have been exposed to weathering:

Flaking according to ISO 4628-5; flake density 2 or less, flake size 2 or less

Cracking according to ISO 4628-4; crack quantity 2 or less, crack size 3 or less

Blistering according to ISO 4628-2; blister density 3 or less, blister size 3 or less.

Tests should be performed on the tinting base.

Assessment and verification: the applicant shall provide test reports using either ISO 11507 according to the specified parameters or EN 927-6, or both. The applicant shall provide test reports using EN ISO 4628-2, 4, 5, 6 and a test report in conformance ISO 7724-3 where applicable.

3(f)   Water vapour permeability

Where claims are made that exterior masonry and concrete paints are breathable the paint shall be classified according to EN1062-1 as class II (medium vapour permeability) or better according to the test method EN ISO 7783.

Due to the large number of potential tinting colours, this criterion will be restricted to testing of the base paint.

Assessment and verification: the applicant shall provide a test report using methodology EN ISO 7783 and classification according EN1062-1.

3(g)   Liquid water permeability

Where claims are made that exterior masonry and concrete paints are water repellent or elastomeric, the coating shall be classified according to EN1062-1 as class III (low liquid permeability) according to method EN 1062-3.

Due to the large number of potential tinting colours, this criterion will be restricted to the testing of the base paint.

All other masonry paints shall be classified according to EN1062-1 as class II (medium liquid permeability) or better according to the test method EN 1062-3.

Assessment and verification: the applicant shall provide a test report using methodology EN 1062-3 and classification according EN1062-1.

3(h)   Fungal and algal resistance

Where claims are made that exterior masonry finish and wood paints have anti-fungal and algal properties, and in accordance with PT7 of the Biocide Regulation (EU) No 528/2012 of the European Parliament and of the Council (6), the following requirements shall be determined using EN 15457 and EN 15458.

Masonry paints shall have a score of class 1 or lower (1 or 0) for fungal resistance, (i.e. less than 10 % fungal coverage) and a score of class 1 or lower for algal resistance.

Wood paints shall have a score of 0 for fungal resistance and 0 for algal resistance.

Due to the large number of possible tinting colours, this criterion will be restricted to the testing of the base paint.

Assessment and verification: the applicant shall provide a test report using the methodology in EN 15457 and EN 15458.

3(i)   Crack bridging

Where claims are made that masonry (or concrete) paint has elastomeric properties, the paint shall be at least classified as A1 at 23 °C according to EN 1062.

Due to the large number of potential tinting colours, this criterion will be restricted to the testing of the base paint.

Assessment and verification: the applicant shall provide a test report using methodology DIN EN 1062-7.

3(j)   Alkali resistance

Masonry paints and primers shall show no noticeable damage when the coating is spotted for 24 hours with 10 % NaOH solution according to method ISO 2812-4. The evaluation is done after 24 hours drying-recovery.

Assessment and verification: the applicant shall provide a test report using methodology ISO 2812-4.

3(k)   Corrosion resistance

Simulated corrosion stresses shall be applied to a substrate for the purpose of rating according to the appropriate atmospheric corrosivity category or categories in EN ISO 12944-2 and the accompanying test procedures specified in EN ISO 12944-6. Anti-rust paints for steel substrates shall be tested after 240 h salt spray following ISO 9227. The results shall be rated using ISO 4628-2 for blistering and ISO 4628-3 for rusting. The paint shall achieve result not worse than size 3 and density 3 in blistering and not worse than Ri2 in rusting test.

Assessment and verification: the applicant shall provide testing and rating reports to confirm compliance with this criterion.

Criterion 4. Content of Volatile and Semi-volatile Organic Compounds (VOCs, SVOCs)

The maximum content of Volatile Organic Compounds (VOCs) and Semi-Volatile Organic Compounds (SVOCs) shall not exceed the limits given in Table 3.

The content of VOCs and SVOCs shall be determined for the ready to use product and shall include any recommended additions prior to application such as colourants and/or thinners.

Products with a VOC content that is in accordance with the limits in Table 3 may display the text ‘reduced VOC content’ and the VOC content in g/l next to the Ecolabel.

Table 3

VOC and SVOC content limits

Product description (with subcategory denotation according to Directive 2004/42/EC)	VOC limits (g/l including water)	SVOC limits (g/l including water)
a. Interior matt walls and ceilings (Gloss < 25@60°)	10	30 (7)/40 (8)
b. Interior glossy walls and ceilings (Gloss > 25@60°)	40	30 (7)/40 (8)
c. Exterior walls of mineral substrate	25	40
d. Interior/Exterior trim and cladding paints for wood and metal	80	50 (7)/60 (8)
e. Interior trim varnishes and woodstains, including opaque woodstains	65	30
e. Exterior trim varnishes and woodstains, including opaque woodstains	75	60
f. Interior and Exterior minimal build woodstains	50	30 (7)/40 (8)
g. Primers	15	30 (7)/40 (8)
h. Binding primers	15	30 (7)/40 (8)
i. One-pack performance coatings	80	50 (7)/60 (8)
j. Two-pack reactive performance coatings for specific end use such as floors	80	50 (7)/60 (8)
l. Decorative effect coatings	80	50 (7)/60 (8)
Anti-rust paints	80	60

The VOC content shall be determined either by calculation based on the ingredients and raw materials or by using the methods given in ISO 11890-2 or, alternatively for products with a VOC content of less than 1.0 g/l, the methods given in ISO 17895. The SVOC content shall be determined using the method given in ISO 11890-2. The markers given in Table 4 shall be used as the basis for delimiting the Gas Chromatography results for SVOC's. In the case of products used both indoors and outdoors the strictest SVOC limit value for indoor paints shall prevail.

Table 4

Marker compounds to be used in the determination of SVOC content

	Polar systems (water-borne coating products)	Non-polar systems (solvent-borne coating products)
SVOC	Diethyl adipate (C10H18O4) to methylpalmitate (C17H34O2)	n-Tetradecane (C14H30) to n-Docosan (C22H46)

Assessment and verification: the applicant shall provide for the VOC content of the ready to use product either a test report using the methods given in ISO 11890-2 or ISO 17895 that demonstrates compliance or a declaration of compliance supported by calculations based on the paint ingredients and raw materials.

The applicant shall provide for the SVOC content of the ready to use product either a test report using the method given in ISO 11890-2 or a declaration of compliance supported by calculations based on the paint ingredients and raw materials. The test should be carried out with reference to the markers specified in Table 4 and the Criteria User Manual. At the request of a Competent Body applicants may be required to validate calculations using the specified test method.

Criterion 5. Restriction of hazardous substances and mixtures

The final product shall not contain hazardous substances and mixtures in accordance with the rules set out in the following sub-criteria which apply to:

—	Hazard classifications and risk phrases

—	Substances of Very High Concern

—	Specific other listed substances

Applicants are required to evidence that the final product formulation complies with the overall assessment and verification requirements together with any additional requirements contained within the Appendix.

5(a)   Overall restrictions to hazard classifications and risk phrases

The final product formulation, including all intentionally added ingredients present at a concentration of greater than 0,010 %, shall not, unless expressly derogated in the Appendix, contain substances or mixtures classified as toxic, hazardous to the environment, respiratory or skin sensitisers, or carcinogenic, mutagenic or toxic for reproduction in accordance with Regulation (EC) No 1272/2008 or Council Directive 67/548/EC (9) and as interpreted according to the hazard statements and risk phrases listed in Table 5 of this criteria.

Table 5

Restricted hazard classifications and their categorisation

Acute toxicity
Category 1 and 2	Category 3
H300 Fatal if swallowed (R28)	H301 Toxic if swallowed (R25)
H310 Fatal in contact with skin (R27)	H311 Toxic in contact with skin (R24)
H330 Fatal if inhaled (R23/26)	H331 Toxic if inhaled (R23)
H304 May be fatal if swallowed and enters airways (R65)	EUH070 Toxic by eye contact (R39/41)
Specific target organ toxicity
Category 1	Category 2
H370 Causes damage to organs (R39/23, R39/24, R39/25, R39/26, R39/27, R39/28)	H371 May cause damage to organs (R68/20, R68/21, R68/22)
H372 Causes damage to organs (R48/25, R48/24, R48/23)	H373 May cause damage to organs (R48/20, R48/21, R48/22)
Respiratory and skin sensitisation
Category 1A	Category 1B
H317: May cause allergic skin reaction (R43)	H317: May cause allergic skin reaction (R43)
H334: May cause allergy or asthma symptoms or breathing difficulties if inhaled (R42)	H334: May cause allergy or asthma symptoms or breathing difficulties if inhaled (R42)
Carcinogenic, mutagenic or toxic for reproduction
Category 1A and 1B	Category 2
H340 May cause genetic defects (R46)	H341 Suspected of causing genetic defects (R68)
H350 May cause cancer (R45)	H351 Suspected of causing cancer (R40)
H350i May cause cancer by inhalation (R49)
H360F May damage fertility (R60)	H361f Suspected of damaging fertility (R62)
H360D May damage the unborn child (R61)	H361d Suspected of damaging the unborn child (R63)
H360FD May damage fertility. May damage the unborn child (R60, R60/61)	H361fd Suspected of damaging fertility. Suspected of damaging the unborn child (R62/63)
H360Fd May damage fertility. Suspected of damaging the unborn child (R60/63)	H362 May cause harm to breast fed children (R64)
H360Df May damage the unborn child. Suspected of damaging fertility (R61/62)
Hazardous to the aquatic environment
Category 1 and 2	Category 3 and 4
H400 Very toxic to aquatic life (R50)	H412 Harmful to aquatic life with long-lasting effects (R52/53)
H410 Very toxic to aquatic life with long-lasting effects (R50/53)	H413 May cause long-lasting effects to aquatic life (R53)
H411 Toxic to aquatic life with long-lasting effects (R51/53)
Hazardous to the ozone layer
EUH059 Hazardous to the ozone layer (R59)

The most recent classification rules adopted by the Union shall take precedence over the listed hazard classifications and risk phrases. In accordance with Article 15 of Regulation (EC) No 1272/2008 applicants shall therefore ensure that classifications are based on the most recent rules on the classification, labelling and packaging of substances and mixtures.

Applicants are required to calculate the hazard classification of the final paint product in order to demonstrate compliance. This shall be in accordance with the methodologies for the classification of mixtures contained in Regulation (EC) No 1272/2008 and all amending legislation. Equivalence between mixture classifications according to the Dangerous Substances Directive 67/548/EEC (referred to as DSD) and those made according to Regulation (EC) No 1272/2008 (the CLP Regulation) can be found in Table 6.

The final product shall not be classified and labelled as being acutely toxic, a specific target organ toxicant, a respiratory or skin sensitiser, or carcinogenic, mutagenic or toxic for reproduction hazardous to the environment, in accordance with Regulation (EC) No 1272/2008 or Directive 67/548/EEC.

Table 6

Final product classification: CLP versus DSD equivalence

CLP Mixture classification	DSD equivalent
Acutely toxic	T or T+
Specific target organ toxicant	T, T+ or Xn
A respiratory or skin sensitiser	—
A carcinogen, mutagen or reproductive toxicant	Carcinogen, Mutagen or Reproductive toxicant categories 1-3
Hazardous to the environment	N (excluding R53 and R52/53)

5(a)(i)   Derogations applying to substance groups

For the purpose of this product group, derogations have been granted for defined groups of substances that may be contained within the final product. These derogations stipulate the hazard classifications that are derogated for each specific substance group and the associated derogation conditions and concentration limits that apply. The derogations are set out in the Appendix and apply to the following substance groups:

1.	Preservatives added to colourants, binders and the final product (a) In-can preservatives (b) Tinting machine preservatives (c) Dry film preservatives (d) Preservative stabilisers

2.	Drying and anti-skinning agents (a) Drying agents (b) Anti-skinning agents

3.	Corrosion inhibitors (a) Corrosion inhibitors (b) Verdigris prevention

4.	Surfactants (a) General purpose surfactants (b) Alkylphenolethoxylates (APEOs) (c) Perfluorinated surfactants

5.	Miscellaneous functional substances with general application (a) Silicon resin emulsion in white paints, colourant and tinting bases (b) Metals and their compounds (c) Mineral raw materials including fillers (d) Neutralising agents (e) Optical brighteners (f) Pigments

6.	Miscellaneous functional substances with specialist applications (a) UV protectors and stabilisers (b) Plasticisers

7.	Residual substances that may be present in the final product (a) Formaldehyde (b) Solvents (c) Unreacted monomers (d) Volatile Aromatic Compounds and halogenated compounds

5(a)(ii)   Derogation conditions applying to production sites

Additional conditions relating to production of paints and varnishes shall apply in the case of derogations for acute toxins or specific target organ toxins. In this case applicants shall submit evidence that they have met the following requirements:

—	Substances to which an acute toxic or specific target organ toxins classification applies shall demonstrate compliance with relevant European indicative Occupational Exposure Limit Values (OELV's) or Member State OELV's for the substance(s), with the strictest applying;

—	Where there is no reference OELV then the applicant shall demonstrate how health and safety procedures for the handling of the ingoing substance(s) at production sites for the final ecolabelled paint product minimise exposure;

—	Substances to which a classification applies as an aerosol or vapour shall demonstrate that workers are not exposed in this form;

—	Substances to which the classification applies to in their dry form shall demonstrate that workers cannot come into contact with the substance in this form during manufacturing.

Assessment and verification: the applicant shall demonstrate compliance with this criterion by providing a declaration of the classification and/or non-classification for:

—	The final paint or varnish product based on the methodologies for the classification of mixtures contained in Regulation (EC) No 1272/2008 and all amending legislation

—	Paint or varnish formula ingredients that fall within the groups of substances listed in 5(a)(i) and that are present at concentrations of more than 0,010 %

This declaration shall be based on information collected according to the requirements in the Appendix.

Active ingredients to which specific concentration limits may apply under Regulation (EC) No 1272/2008 and which may fall below the cut-off value of 0,010 % shall also be identified.

The following technical information shall be provided to support the declaration of the classification or non-classification of ingredients:

(i)	For substances that have not been registered under the REACH Regulation or which do not yet have a harmonised CLP classification: Information meeting the requirements listed in Annex VII to the REACH Regulation;

(ii)	For substances that have been registered under the REACH Regulation and which do not meet the requirements for CLP classification: Information based on the REACH registration dossier confirming the non-classified status of the substance;

(iii)

For substances that have a harmonised classification or are self-classified: safety data sheets where available. If these are not available or the substance is self-classified then information shall be provided relevant to the substances hazard classification according to Annex II to the REACH Regulation;

(iv)

In the case of mixtures: Safety data sheets where available. If these are not available then calculation of the mixture classification shall be provided according to the rules under Regulation (EC) No 1272/2008 together with information relevant to the mixtures hazard classification according to Annex II to the REACH Regulation;

Substances and mixtures shall be characterised in accordance with sections 10, 11 and 12 of Annex II to the REACH Regulation (Requirements for the Compilation of Safety Data Sheets). This shall include information on the physical form and state of the ingredients and shall include identification of manufactured nanomaterial ingredients for which 50 % or more of the particles in the number size distribution have one or more external dimensions in the size range 1 nm-100 nm.

The applicant shall also identify substances and mixtures used in the paint formulation which fall under the specific requirements for derogation as set out in the Appendix. For each derogated substance or mixture supporting information shall be provided showing how the derogation requirements have been met.

5(b)   Restrictions that apply to Substances of Very High Concern

In accordance with Article 6(7) of Regulation (EC) No 66/2010 the final product and any ingredients or raw materials, shall not, unless specifically derogated, contain substances that:

—	Meet the criteria in Article 57 of the REACH Regulation;

—	Have been identified according to the procedure described in Article 59(1) of the REACH Regulation which establishes the Candidate List for Substances of Very High Concern.

No derogation shall be given concerning substances that meet one or both of these conditions, and which are present in a paint or varnish product at concentrations higher than 0.10 % (weight by weight).

Assessment and verification: the applicant shall provide a declaration of compliance with this criterion, supported by declarations of compliance signed by their suppliers. Applicants shall demonstrate that they have carried out a screening of ingoing substances against the current Candidate List for Substances of Very High Concern and the criteria in Article 57 of the REACH Regulation.

5(c)   Restrictions that apply to specific hazardous substances

The final product shall not contain the hazardous substances that are specifically identified in the Appendix at or above the specified concentration limits. The restrictions on substances in the Appendix apply to the following paint and varnish ingredients and residues:

(i)	Dry film preservatives

(ii)	Tinting machine preservatives

(iii)

In-can preservatives

(iv)	Preservative stabilisers

(v)	Alkylphenolethoxylates (APEOs) surfactants

(vi)	Perfluorinated surfactants

(vii)

Metals and their compounds

(viii)

Pigments

(ix)	Plasticisers

(x)	Free formaldehyde

Assessment and verification: verification and testing requirements are as specified in the Appendix for each substance and as relevant to specific forms of paint and varnish.

Criterion 6. Consumer information

6(a)

The following texts shall appear on or be attached to the packaging: — ‘Minimise paint wastage by estimating how much paint you will need’ — ‘Recover unused paint for re-use’. — ‘Reuse of paint can effectively minimise the products' life cycle environmental impact’

6(b)

The following general information and advice shall be provided on or be attached to the packaging: — How to estimate the amount of paint needed prior to purchase in order to minimise paint wastage and a recommended amount as a guideline (e.g. for 1 m2 of wall x litres of paint is needed). — How to deal with the ‘unused paint’ together with, where available, a web-link or contact details from which the consumer can find more detailed information.

6(c)

The following advice and recommendations on how to handle the paint shall be provided on or be attached to the packaging: — Safety measures for the user. This shall include basic recommendation on personal protective equipment that should be worn. It shall also include additional measures that should be taken when using spray equipment. — The use of cleaning equipment and appropriate waste management (in order to limit water and soil pollution). For example, text advising that unused paint requires specialist handling for safe environmental disposal and therefore it should not be thrown away with household or commercial waste (e.g. ‘Do not put residual paint down the kitchen sink or toilet, or into a waste bin’). — Storage of the paint in appropriate conditions (before and after opening), including, where appropriate, safety advice.

Assessment and verification: the applicant shall declare that the product complies with the requirement and provide the competent body with the artwork or samples of the user information and/or a link to a manufacturer's website containing this information as part of the application. The recommended amount of paint given as a guideline shall be provided.

Criterion 7. Information appearing on the EU Ecolabel

The optional label with text box shall contain, where relevant, the following texts:

—	Minimised content of hazardous substances

—	Reduced content of volatile organic compounds (VOCs): x g/l

—	Good performance for indoor use (where indoor criteria have been met) or

—	Good performance for outdoor use (where outdoor criteria have been met) or

—	Good performance for both indoor and outdoor use (where both indoor and outdoor criteria have been met)

The guidelines for the use of the optional label with text box can be found in the ‘Guidelines for use of the Ecolabel logo’ on the website:

http://ec.europa.eu/environment/ecolabel/documents/logo_guidelines.pdf

Assessment and verification: the applicant shall provide a sample of the product label or an artwork of the packaging where the EU Ecolabel is placed, together with a declaration of compliance with this criterion.

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(1)  Regulation (EC) No 1907/2006 of the European Parliament and of the Council of 18 December 2006 concerning the Registration, Evaluation, Authorisation and Restriction of Chemicals (REACH), establishing a European Chemicals Agency (OJ L 396, 30.12.2006, p. 1).

(2)  As derived from the Reference Document on Best Available Technology for the Manufacture of Large Volume Inorganic Chemicals (BREF), August 2007.

(3)  Directive 2008/98/EC of the European Parliament and of the Council of 19 November 2008 on waste and repealing certain Directives (OJ L 312, 22.11.2008, p. 3).

(4)  Only required where marketing claims are made about the paints

(5)  EN ISO 2813.

(6)  Regulation (EU) No 528/2012 of the European Parliament and of the Council of 22 May 2012 concerning the making available on the market and use of biocidal products (OJ L 167, 27/06/2012, p. 1).

(7)  Indoor white paints and varnishes

(8)  Indoor tinted paints/outdoor paints and varnishes

(9)  Council Directive 67/548/EEC of 27 June 1967 on the approximation of laws, regulations and administrative provisions relating to the classification, packaging and labelling of dangerous substances (OJ 196, 16.8.1967, p. 1).