METHODS OF SAMPLING
ANNEX ISupplementary provisions
ANNEX I METHODS OF SAMPLING 1. PURPOSE AND SCOPE Samples intended for the official control of feed shall be taken according to the methods described below. Samples thus obtained shall be considered as representative of the sampled portions. 2. SAMPLING PERSONNEL The samples shall be taken by persons authorised for that purpose by the Member States. 3. DEFINITIONS Sampled portion: A quantity of product constituting a unit, and having characteristics presumed to be uniform. Incremental sample: A quantity taken from one point in the sampled portion. Aggregate sample: An aggregate of incremental samples taken from the same sampled portion. Reduced sample: A representative part of the aggregate sample, obtained from the latter by a process of reduction. Final sample: A part of the reduced sample or of the homogenised aggregate sample. 4. APPARATUS 4.1. The sampling apparatus must be made of materials which cannot contaminate the products to be sampled. Such apparatus may be officially approved by the Member States. 4.2. Apparatus recommended for the sampling of solid feed. 4.2.1. Manual sampling 4.2.1.1. Flat-bottomed shovel with vertical sides. 4.2.1.2. Sampling spear with a long split or compartments. The dimensions of the sampling spear must be appropriate to the characteristics of the sampled portion (depth of container, dimensions of sack, etc.) and to the particle size of the feed. 4.2.2. Mechanical sampling Approved mechanical apparatus may be used for the sampling of moving feed. 4.2.3. Divider Apparatus designed to divide the sample into approximately equal parts may be used for taking incremental samples and for the preparation of reduced and final samples. 5. QUANTITATIVE REQUIREMENTS 5.A. In relation to the control of substances or products uniformly distributed throughout the feed 5.A.1. Sampled portion The size of the sampled portion must be such that each of its constituent parts can be sampled 5.A.2. Incremental samples 5.A.2.1. Loose feed: Minimum number of incremental samples: 5.A.2.1.1. sampled portions not exceeding 2,5 metric tons seven 5.A.2.1.2. sampled portions exceeding 2,5 metric tons √ 20 times the number of metric tons making up the sampled portion ( *1 ) , up to a maximum of 40 incremental samples 5.A.2.2. Packaged feed: Minimum number of packages to be sampled ( *2 ) : 5.A.2.2.1. Packages of more than 1 kg: 5.A.2.2.1.1. sampled portions of one to four packages all packages 5.A.2.2.1.2. sampled portions of 5 to 16 packages four 5.A.2.2.1.3. sampled portions of more than 16 packages √ number of packages making up the sampled portion ( *1 ) , up to maximum of 20 packages 5.A.2.2.2. Packages not exceeding 1 kg four 5.A.2.3. Liquid or semi-liquid feed: Minimum number of containers to be sampled ( *2 ) : 5.A.2.3.1. Containers of more than one litre: 5.A.2.3.1.1. sampled portions of one to four containers all containers 5.A.2.3.1.2. sampled portions of 5 to 16 containers four 5.A.2.3.1.3. sampled portions of more than 16 containers √ number of containers making up the sampled portion ( *1 ) , up to a maximum of 20 containers 5.A.2.3.2. Containers not exceeding one litre four 5.A.2.4. Feed blocks and mineral licks Minimum number of blocks or licks to be sampled ( *2 ) : one block or lick per sampled portion of 25 units, up to a maximum of four blocks or licks 5.A.3. Aggregate sample A single aggregate sample per sampled portion is required. The total amount in the incremental samples making up the aggregate sample shall be not less than the following: 5.A.3.1. Loose feed 4 kg 5.A.3.2. Packaged feed: 5.A.3.2.1. packages of more than 1 kg 4 kg 5.A.3.2.2. packages not exceeding 1 kg weight of the contents of four original packages 5.A.3.3. Liquid or semi-liquid feed: 5.A.3.3.1. containers of more than one litre four litres 5.A.3.3.2. containers not exceeding one litre volume of the contents of four original containers 5.A.3.4. Feed blocks or mineral licks: 5.A.3.4.1. each weighing more than 1 kg 4 kg 5.A.3.4.2. each weighing not more than 1 kg weight of four original blocks or licks 5.A.4. Final samples The aggregate sample gives the final samples on reduction when necessary. Analysis of at least one final sample is required. The amount in the final sample for analysis shall be not less than the following: Solid feed 500 g Liquid or semi-liquid feed 500 ml 5.B. In relation to the control of undesirable substances or products likely to be distributed non-uniformly throughout the feed, such as aflatoxins, rye ergot, castor-oil plant and crotalaria in feed materials ( *3 ) 5.B.1. Sampled portion: see 5.A.1. 5.B.2. Incremental samples 5.B.2.1. Loose feed: see 5.A.2.1. 5.B.2.2. Packaged feed: Minimum number of packages to be sampled: 5.B.2.2.1. sampled portions consisting of one to four packages all packages 5.B.2.2.2. sampled portions consisting of 5 to 16 packages four 5.B.2.2.3. sampled portions consisting of more than 16 packages √ number of packages making up the sampled portion ( *1 ) , up to a maximum of 40 packages 5.B.3. Aggregate samples The number of aggregate samples will vary with the size of the sampled portion. The minimum number of aggregate samples per sampled portion is given below. The total weight of the incremental samples making up each aggregate sample shall be not less than 4 kg 5.B.3.1. Loose feed Weight of the sampled portion in metric tons: Minimum number of aggregate samples per sampled portion: up to 1 1 more than 1 and up to 10 2 more than 10 and up to 40 3 more than 40 4 5.B.3.2. Packaged feed Size of the sampled portion in number of packages: Minimum number of aggregate samples per sampled portion: 1 to 16 1 17 to 200 2 201 to 800 3 more than 800 4 5.B.4. Final samples Each aggregate sample gives the final samples on reduction. Analysis of at least one final sample per aggregate sample is required. The weight of the final sample for analysis may not be less than 500 g 6. INSTRUCTIONS FOR TAKING, PREPARING AND PACKAGING THE SAMPLES 6.1. General The samples must be taken and prepared as quickly as possible bearing in mind the precautions necessary to ensure that the product is neither changed nor contaminated. Instruments and also surfaces and containers intended to receive samples must be clean and dry. 6.2. Incremental samples 6.2.A. In relation to the control of substances or products uniformly distributed throughout the feed Incremental samples must be taken at random throughout the whole sampled portion and they must be of approximately equal sizes. 6.2.A.1. Loose feed An imaginary division shall be made of the sampled portion into a number of approximately equal parts. A number of parts corresponding to the number of incremental samples required in accordance with 5.A.2 shall be selected at random and at least one sample taken from each of these parts. Where appropriate, sampling may be carried out when the sampled portion is being moved (loading or unloading). 6.2.A.2. Packaged feed Having selected the required number of packages for sampling as indicated in 5.A.2, part of the contents of each package shall be removed using a spear or shovel. Where necessary, the samples shall be taken after emptying the packages separately. Any lumps shall be broken up, if necessary, by separating them out and returning into the sample, in each aggregate sample separately. 6.2.A.3. Homogeneous or homogenisable liquid or semi-liquid feed Having selected the required number of containers for sampling as indicated in 5.A.2, the contents shall be homogenised if necessary and an amount taken from each container. The incremental samples may be taken when the contents are being discharged. 6.2.A.4. Non-homogenisable, liquid or semi-liquid feed Having selected the required number of containers for sampling as indicated in 5.A.2, samples shall be taken from different levels. Samples may also be taken when the contents are being discharged but the first fractions shall be discarded. In either case the total volume taken must not be less than 10 litres. 6.2.A.5. Feed blocks and mineral licks Having selected the required number of blocks or licks for sampling as indicated in 5.A.2, a part of each block or lick shall be taken. 6.2.B. In relation to the control of undesirable substances or products likely to be distributed non-uniformly throughout the feed, such as aflatoxins, rye ergot, castor-oil plant and crotalaria in feed materials An imaginary division shall be made of the sampled portion into a number of approximately equal parts, corresponding to the number of aggregate samples provided for in 5.B.3. 1f this number is greater than one, the total number of incremental samples provided for in 5.B.2 shall be distributed approximately equally over the different parts. Then take samples of approximately equal sizes ( 1 ) and such that the total amount in the samples from each part is not less than the minimum 4 kg quantity required for each aggregate sample. Incremental samples taken from different parts shall not be aggregated. 6.3. Preparation of aggregate samples 6.3.A. In relation to the control of substances or products distributed uniformly throughout the feed The incremental samples shall be mixed to form a single aggregate sample. 6.3.B. In relation to the control of undesirable substances or products likely to be distributed non-uniformly throughout the feed, such as aflatoxins, rye ergot, castor-oil plant and crotalaria in feed materials The incremental samples from each part of the sampled portion shall be mixed and the number of aggregate samples provided for in 5.B.3, made up taking care to note the origin of each aggregate sample. 6.4. Preparation of final samples The material in each aggregate sample shall be carefully mixed to obtain an homogenised sample ( 2 ) . If necessary the aggregate sample shall first be reduced to at least 2 kg or two litres (reduced sample) either by using a mechanical or automatic divider or by the quartering method. At least three final samples shall then be prepared, of approximately the same amount and conforming to the quantitative requirements of 5.A.4 or 5.B.4. Each sample shall be put into an appropriate container. All necessary precautions shall be taken to avoid any change of composition of the sample, contamination or adulteration which might arise during transportation or storage. 6.5. Packaging of final samples The containers or packages shall be sealed and labelled (the total label must be incorporated in the seal) in such a manner that they cannot be opened without damaging the seal. 7. SAMPLING RECORD A record must be kept of each sampling, permitting each sampled portion to be identified unambiguously. 8. DESTINATION OF SAMPLES For each aggregate sample, at least one final sample shall be sent as quickly as possible to the authorised analytical laboratory, together with the information necessary for the analyst. ( *1 ) Where the number obtained is a fraction, it shall be rounded up to the next whole number. ( *2 ) For packages or containers whose contents do not exceed 1 kg or one litre and for blocks or licks weighing not more than 1 kg each, an incremental sample shall be the contents of one original package or container, one block or one lick. ( *3 ) The methods provided for in 5.A are for use in the control of aflatoxins, rye ergot, castor-oil plant and crotalaria in complete and complementary feed. ( 1 ) For packaged feed, a part of the contents of the packages to be sampled shall be removed, using a spear or shovel, after having, if necessary, emptied the packages separately. ( 2 ) Any lumps shall be broken up (if necessary by separating them out and returning them to the sample) in each aggregate sample separately.