Commission Regulation (EU) No 589/2014 (repealed)Dangos y teitl llawn

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).

• 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).

(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.