Decree of the Ministry of Agriculture No. 124 / 2001 Coll.
Decree of the Ministry of Agriculture laying down the sampling requirements and principles of methods of analysis of feed, additives and premixtures and the method of storage of samples
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124
DECLARATION
Ministry of Agriculture
of 23 March 2001
laying down the sampling requirements and principles for methods of analysis of feed, feed additives and premixtures and the method of storage of samples
According to Article 17 (8) of Act No. 91 / 1996 Coll., on Feed, as amended by Act No. 244 / 2000 Coll., ("the Act '), the Ministry of Agriculture provides for the implementation of Article 4 (12):
Sampling of feed, feed additives and premixtures
(1) This decree (1) implements the relevant provisions of the European Community (1a) and regulates the requirements for sampling, the principles of methods of analysis of feed, additives and premixtures and the method of storage of samples.
(2) When sampling feed, additives and premixtures carried out in the framework of professional supervision and testing (Sections 16 to 19 of the Act), the procedures set out in this Decree shall apply.
(3) The sampling of feed, feed additives and premixtures includes the taking of incremental samples for the purposes of compiling the aggregate and final samples, the taking of incremental samples for the purpose of determining the working accuracy of the mixing device and the assessment of the homogeneity of the additives and amino acids in premixtures and feedingstuffs using premixtures (hereinafter referred to as "homogeneity") and the method of marking and storage of final and, where appropriate, incremental samples, including the drawing up of a report on their collection. This provision shall not apply to sampling for the determination of the presence of micro-organisms and pesticide residues, which shall be carried out in accordance with a specific legislation.2)
(1) When a partial sample is taken which is considered to be the mass part of a single lot obtained by a single lot, the aids and equipment listed in Annex 1 to this Decree shall be used.
(2) The minimum number of incremental samples per type of feed, feed additive and premixture and following the weight or number of packages of the sampled lot is given in column 2 of Annex 2 to this Decree.
(3) For feed, additives and premixtures packed in packages of less than 1 kg or of a volume of less than 1 litre, the contents of each package, such as one box, bag or block of feed, shall be considered as a partial sample.
(4) The partial sampling procedure provided for in paragraphs 2 and 3 does not apply to the taking of incremental samples for the assessment of homogeneity (3) of the additive in the premixture batch or feed produced using a premixture or for the assessment of the working accuracy of the mixing devices.
(5) When sampling to assess the homogeneity of the additive in a premixture or feed batch using a premixture, partial samples shall be taken from at least five packages.
(6) The quantity of feed, feed additive or premixture showing consistency with its external arrangements, labelling and local storage shall be considered as the sampled lot. Where the size, storage and accessibility of a lot of feed, feed additive or premixture does not allow sampling at all lot sites, sampling and marking shall be carried out as a sampled lot the part or weight from which the incremental samples have been taken.
(7) When taking incremental samples to assess the working accuracy of the mixing device, 10 incremental samples shall be taken from the content of the mixing device considered as set out in Annex 16.
(1) The total weight of all incremental samples taken from one lot of feed, feed additive or premixture constitutes the aggregate sample; its minimum weight is set out in column 2 of Annex 3. The reduced sample is a representative part of the aggregate sample from which it is obtained by division. The final sample is a part of the reduced sample or a homogenised aggregate sample.
(2) The provisions of paragraph 1 shall not apply to incremental samples taken to assess the homogeneity of the additive in a premixture or feed batch using a premixture or to assess the working accuracy of the mixing devices and to determine the presence or content of undesirable substances and prohibited substances and products in feedingstuffs.
(3) When sampling for the assessment of the homogeneity of the additive in a premixture or feed batch using the premixture, the incremental samples from one package shall each form one aggregate sample.
(4) When sampling to assess the working accuracy of the agitators, the incremental sample taken from the agitators shall always constitute one aggregate sample which is considered to be the final sample at the same time.
(5) When sampling for the presence or content of undesirable substances and prohibited substances and products in feedingstuffs, with the exception of the determination of the levels of dioxins and dioxin-like polychlorinated biphenyls, the minimum number of aggregate samples as set out in column 2 of Annex 4 to this Decree shall be determined; the minimum mass of these samples shall not be less than four kilograms or, for liquid forms, the volume shall not be less than four litres.
(6) A aggregate sample shall be considered to represent the sampled lot or sublot.
(7) The determination of the levels of dioxins as well as the levels of dioxins similar to polychlorinated biphenyls is carried out in a laboratory sample.
(1) At least three final samples shall be taken from the aggregate or reduced sample, which shall constitute the quantity of the aggregate sample intended for testing; the minimum weight of the final sample is given in column 2 of Annex 5.
(2) The provisions of paragraph 1 shall not apply to aggregate samples when sampling for the assessment of the homogeneity of the additive in the premixture or feed batch using the premixture and for the assessment of the working accuracy of the mixing device for which the aggregate sample forms the final sample at the same time.
(3) The procedure for sampling feed, feed additives and premixtures is set out in Annex 6 to this Regulation.
(4) Samples intended for laboratory testing shall be delivered without delay together with the sampling protocol to the laboratory concerned.
(1) When sampling feed, additives and premixtures, final samples shall be kept in clean, dry, moisture-free, airtight sealed packages. The packaging with final samples shall be closed and the seal shall be sealed or sealed so as to avoid opening the packaging without damaging the seal or seal. The seal or seal shall be such that it is not applicable after opening the container.
(2) The final samples shall be marked with at least the following particulars when taken:
(a) the name of the sampled feed, additive or premixture,
(b) the commercial name and registered office of the legal person which has ensured the final sampling when sampling on request;
(c) by the name and surname (hereinafter referred to as "the name") of the natural person who carried out the procurement.
(3) The marking of the sample shall be such that it is firmly linked to the sample, its seal or seal.
(4) The provisions of paragraphs 1, 2 and 3 shall not apply to incremental samples taken to assess the homogeneity and working accuracy of the mixing equipment.
(5) When taking incremental samples for the assessment of homogeneity or the working accuracy of the mixing devices, the incremental samples, which are also final samples, shall be kept in clean, dry, moisture-free, airtight sealed packages. The packaging shall be sealed and marked with the following particulars:
(a) the name of the sampled feed, additive, premixture or, for samples, for the assessment of working accuracy by the type of mixing device verified;
(b) the commercial name and registered office of the legal person or the natural person who is the manufacturer of the feed, the additive and the premixture, for samples for the assessment of the professional accuracy on the commercial name and registered office of the legal person or on behalf of the natural person who is the owner of the mixing establishment;
(c) on behalf of the natural person responsible for sampling.
(6) When sampling feed, additives and premixtures intended for the testing of photolabelled substances, final samples shall be kept in packages which prevent light access.
(1) A protocol shall be drawn up for each final sample of feed, feed additive and premixture to allow for the accurate identification of each sampled lot so as not to confuse the samples. The sampling protocol shall be attached to each final sample. For the purpose of assessing the homogeneity or working accuracy of the agitators, only one protocol shall be taken for all samples.
(2) The Protocol shall always contain the following information:
(a) the name and address of the natural person or the business name and registered office of the legal person who supplied, imported or produced the sampled feed, additive or premixtures;
(b) the name and address of the natural person or the business name and registered office of the legal person where the sampled feed, additive or premixtures have been supplied;
(c) the name of the sampled feed, additive or premixture and the weight or volume of the sampled lot;
(d) the date of sampling;
(e) the registered office of the professional supervisor, (1) which ensured the sampling;
(f) the name of the natural person who carried out the procurement;
(g) place of storage of the lot;
(h) sampling plan, specifying the sampling points, if any;
(i) the reason for sampling.
Laboratory testing of feed, additives and premixtures
(1) In the framework of professional supervision and testing, the methods of analysis laid down by the provisions of the European Communities are used. Where the method is not provided for in the rules, the control shall be carried out according to other methods of analysis, the principles of which are set out in the Annexes to this Decree.
(2) The list and principles of methods of analysis of feed, feed additives and premixtures are set out in Annexes 9 to 14. The full procedures of the methods set out in Annexes 9 to 12 and the sampling aids referred to in Annex 1 shall be published in the Bulletin of the Central Audit and Examination Institute of the Agricultural Institute (5).
(3) Where the principle of the method for testing the character is not set out in Annexes 9 to 14, the method set out in the Bulletin of the Central Control and Examination Institute of the Agricultural Institute (hereinafter referred to as "Bulletin ') shall be used, and, if not, another appropriate method shall be used which corresponds to the level of scientific and technical knowledge achieved. The general characteristics to be met by the test methods are defined by the directly applicable regulation of the European Communities. 6)
(1) For laboratory testing of feed, additives and premixtures, except physical, sensory and special testing, the final sample shall be adjusted to the test sample. The test sample is a representative part of the final sample, adjusted in the manner set out in Annex 7 to this Decree.
(2) The sample is adjusted to avoid contamination or change its composition. Grinding, mixing and sifting shall be carried out as quickly as possible to minimise exposure to air and light. No mills or other apparatus which could cause the sample to heat above 40 ° C may be used for the treatment of the sample. The specially sensitive sample shall be crushed manually. In addition, it is necessary to ensure that the devices themselves are not the source of contamination with trace elements.
(3) If the sample cannot be adjusted without substantially changing its moisture content, the moisture content shall be determined before and after treatment in accordance with the method set out in Annex 7.
(1) Test samples of feed, feed additives and premixtures shall be kept after the completion of the tests by the methods set out in Annex 8 to this Regulation.
(2) The samples of feed, feed additives and perishable premixtures shall be adjusted within a maximum period of 24 hours to allow them to be used for testing in their original state or to be dried; The divided part of the wet sample shall be stored in an airtight container at 0 to + 5 ° C at least until the test of the sample has been completed.
Chemical testing of feed, additives and premixtures
(1) For the chemical testing of feedingstuffs, feed additives and premixtures, only chemicals are used, analytical pure or chemically pure, unless otherwise provided in Annexes 7 to 14 to this Regulation. When determining trace elements, the purity of test chemicals shall be verified by a separate experiment (blank test).
(2) Distilled or demineralised water or solvent or diluent listed in Annexes 7 to 14 to this Decree shall be used for the preparation of solutions, for dilution, rinsing or washing.
(3) The concentration of the solutions shall be expressed either by weight or volume percent, or expressed as a concentration of the substance (mol / l) or by weight (mg / l, mg / ml).
(1) The chemical test of feed, feed additive or premixture results in an average value obtained from at least two analyses carried out on two samples taken, provided that the analytical result does not deviate by more than the limit of repeatability / r / (hereinafter referred to as "repeatability") set out in Annexes 9 and 10 to this Decree. In order to express the analytical result, measurement uncertainty shall be reported as the parameter associated to the measurement result.
(2) Repeatability is a value that can be assumed to be less than or equal to the absolute value of the difference between the two test results obtained under repeatability conditions with 95% probability. Repeatability conditions are conditions where independent test results are obtained by the same method, on identical material, in the same laboratory, by the same worker, using the same equipment, within a short period of time.
(3) If the repeatability value is not stated, it shall be calculated in accordance with the procedure set out in point 8 of Annex No 15 to this Decree.
(4) The chemical test result shall be expressed in the units listed in Annexes 9 to 14 to this Decree. In determining the original moisture content of feed, feed additive or premixture, the results shall be converted into the original dry matter.
(5) Unless otherwise stated for the method, the results shall be expressed after rounding as follows:
| pro vyjádření obsahu v jednotkách mg/kg: | |
| pro obsah do 9,99 mg/kg | s přesností na 0,01 mg/kg |
| pro obsah od 10,0 do 99,9 mg/kg | s přesností na 0,1 mg/kg |
| pro obsah od 100 do 999 mg/kg | s přesností na 1 mg/kg |
| pro obsah od 1000 do 9999 mg/kg | s přesností na 10 mg/kg |
| pro obsah od 10000 do 99999 mg/kg | s přesností na 100 mg/kg |
| pro obsah nad 100 000 mg/kg | s přesnostína 1000 mg/kg |
| pro vyjádření obsahu v %: | |
| pro obsah do 0,999 % | s přesností na 0,001 % |
| pro obsah od 1,0 do 9,99 % | s přesností na 0,01 % |
| pro obsah nad 10,0 % | s přesností na 0,1 % |
| Pro vyjádření obsahu vitaminu A v m.j./kg | |
| do 999 m.j./kg | s přesností na 1 m.j./kg |
| od 1 000 do 9 999 m.j./kg | s přesností na 10 m.j./kg |
| od 10 000 do 99 999 m.j./kg | s přesností na 100 m.j./kg |
| od 100 000 do 999 999 m.j./kg | s přesností na 1 000 m.j./kg |
| nad 1 00 0000 m.j./kg | s přesností na 10 000 m.j./kg |
(6) The limit of reproducibility / R / (hereinafter referred to as "reproducibility") is a value that can be assumed to be less than or equal to the absolute value of the difference between the two test results obtained under reproducibility conditions. Reproducibility conditions are conditions where independent test results are obtained by the same method, on identical material in different laboratories, different workers using different equipment. Reproducibility does not include a sampling error.
(7) The reproducibility values for each test method are set out in Annexes 9 and 10 to this Decree. If the reproducibility value is not determined, it shall be calculated in accordance with the procedure set out in point 8 of Annex No 15 to this Decree.
(8) The limit of determination is the value of the smallest quantity of the determined substance that can be reliably quantified.
(1) Measurement uncertainty is a parameter associated to the measurement result that characterises the dispersion of values that can reasonably be attributed to the measured value. For test results, the expanded measurement uncertainty calculated using an extension coefficient equal to 2 shall be reported, corresponding to a confidence level of at least 95%.
(2) Recovery is the efficiency of separation of the determined substance from a complex matrix. The determination of recovery may be carried out either by analysis of a certified reference material with a known content of the specified substance or by a known addition of the specified substance to the matrix blank sample and by re-determination of its content.
(3) As regards undesirable substances, including dioxins and dioxin-like PCBs, the product intended for animal feeding shall be considered as not complying with the maximum specified content if, taking into account the expanded measurement uncertainty and recovery correction, the analytical result exceeds the maximum content. For the assessment of compliance, the analysed recovery corrected concentration and the subtracted expanded measurement uncertainty shall be used. This procedure cannot be used for microscopic analysis. The analytical result, if the analytical method used makes it possible to estimate measurement uncertainty and recovery ratio, shall be reported.
(a) as corrected or uncorrected for recovery, the method of detection and its value must be indicated;
(b) in the form of "x ± U," where x is the result of the analysis and U is the expanded measurement uncertainty, using a coverage factor of 2 which corresponds to a confidence level of at least 95%.
The test of homogeneity (3) of additives and amino acids in a premixture or feed batch using premixtures shall be carried out by means of a feed additive or an added amino acid. When assessing the working accuracy of the agitator (3), an additive shall be used which shows the lowest repeatability and reproducibility for the content verified in the laboratory.
They shall be deleted:
1. Decree No 222 / 1996 Coll., laying down the methods of sampling, the methods of analysis for the testing of feedingstuffs, additives and premixtures and the method of storage of perishable samples.
2. Decree No. 16 / 2000 Coll., amending Decree of the Ministry of Agriculture No. 222 / 1996 Coll., laying down the methods of sampling, the methods of analysis of feed, additives and premixtures and the method of storage of samples subject to destruction.
This Decree shall take effect on 1 May 2001.
Minister:
Ing. Fencl v. r.
Příloha č. 1
Annex No 1 to Decree No. 124 / 2001 Coll.
Auxiliary plant for the sampling of feed, feed additives and premixtures
1. For incremental sampling shall be used:
(a) vertical two-shell samples, whether or not cut or split, with an effective height corresponding to the height of the sampled lot;
(b) single-shell samples for horizontal sampling;
(c) blades of suitable dimensions with a straight bottom and edges raised to a right angle;
(d) sample boxes of suitable dimensions,
(e) mechanical devices which are set in motion by the operator or move separately;
(f) a filling or pump with a continuous sampling cap for liquid or semi-liquid feed.
2. Other means and equipment other than those referred to in point 1 may be used to sample manure.
3. Sample dividers may be used to reduce aggregate and final samples.
4. Samples shall be taken and assembled in such a way that there are no undesirable changes compared to the sampled lot and that they are not contaminated by other materials. The equipment used and the working areas where the samples are processed, as well as the packaging, must be clean and dry.
Příloha č. 2
Annex No 2 to Decree No. 124 / 2001 Coll.
Minimum number of incremental samples *)
| Druh a rozsah partie | Minimální počet dílčích vzorků |
|---|---|
| 1 | 2 |
| 1. Pevné materiály volně ložené nebo v obalech nad 100 kg: | |
| - zelená píce konzervovaná silážováním | 20 |
| - pastevní porost | 50 |
| - jiná | |
| do 2,5 t | 7 |
| nad 2,5 t | druhá odmocnina z 20ti násobku hmotnosti |
| 2. Pevné materiály balené do obalů: | |
| - balení do hmotnosti 1 kg | 4 obaly |
| - balení o hmotnosti nad 1 kg | |
| do 4 balení | všechny obaly |
| 5 až 16 balení | 4 obaly |
| více než 16 balení | druhá odmocnina z počtu balení (obalů), zaokrouhleno na celá čísla, nejvýše však 20 obalů; při odběru vzorků na stanovení nežádoucích nebo zakázaných látek nejvýše 40 obalů |
| 3. Tekuté a polotekuté materiály: | |
| balení o obsahu do 1 litru | 4 obaly |
| balení o obsahu nad 1 litr | |
| do 4 balení | všechny obaly |
| 5 až 16 balení | 4 obaly |
| více než 16 balení | druhá odmocnina z počtu obalů, zaokrouhleno na celá čísla, nejvýše však 20 obalů |
| 4. | 1 blok (liz) z každé |
Materials are feed, feed additives and premixtures.
*) Not applicable to the sampled lot if the number of packages or the weight or volume is lower than that shown in the table.
Příloha č. 3
Annex No. 3 to Decree No. 124 / 2001 Coll.
Minimum weight of aggregate sample *)
| Druh a rozsah partie | Minimální hmotnost souhrnného vzorku nebo počet (balení, kusy a jiné) |
|---|---|
| 1 | 2 |
| 1. Pevná | |
| - seno, sláma | 1 kg |
| - ostatní | 4 kg |
| 2. | |
| - do 1 kg | obsah 4 balení |
| - nad 1 kg | 4 kg |
| 3. Tekutá nebo polotekutá | |
| - nádoby do obsahu 1 litr | obsah 4 nádob |
| - nádoby s obsahem nad 1 litr | 4 litry |
| 4. | |
| - do 1 kg 4 kusy (bloky) | |
| - nad 1 kg | 4 kg |
| 5. | |
| - pevná forma | 0,2 kg |
| - tekutá forma | 0,2 litru |
| 6. Premixy: | |
| - pevná forma | 1 kg |
| - tekutá forma | 1 litr |
*) Not applicable to the sampled lot if the number of packages or the weight or volume is lower than that shown in the table.
Příloha č. 4
Annex No. 4 to Decree No. 124 / 2001 Coll.
Minimum number of aggregate samples for the determination of undesirable and prohibited substances and products
| Druh a rozsah partie | Minimální počet souhrnných vzorků z každé partie |
|---|---|
| 1 | 2 |
| 1. Pevná | |
| - do 1 tuny | 1 |
| -od 1,0 do 10 tun | 2 |
| -od 10,0 do 40 tun | 3 |
| - nad 40,0 tun | 4 |
| 2. | |
| -do 16 obalů | 1 |
| -od 17 do 200 obalů | 2 |
| - od 201 do 800 obalů | 3 |
| - nad 800 obalů | 4 |
Příloha č. 5
Annex No 5 to Decree No. 124 / 2001 Coll.
Minimum weight of final sample *)
| Druh a rozsah partie | Minimální hmotnost konečného vzorku |
|---|---|
| 1 | 2 |
| 1. Pevná | 0,5 kg |
| 2. Tekutá a polotekutá | 0,5 l |
| 3. | 0,05 kg |
| 4. Premixy | 0,25 kg. |
*) Not applicable to the sampled lot if the number of packages or the weight or volume is lower than that shown in the table.
Příloha č. 6
Annex No 6 to Decree No. 124 / 2001 Coll.
Procedure for sampling feed, feed additives and premixtures
1. Partial samples, with the exception of incremental samples for the determination of the presence and content of undesirable substances, prohibited substances and products, as well as incremental samples for the determination of homogeneity and assessment of the working accuracy of the agitators shall be taken at random to cover the whole sampled lot. The mass or volume of each incremental sample taken is approximately the same. In addition, the following shall be observed during the sampling:
(a) For feedingstuffs in packages of more than 100 kg, each packaging shall be hypothetically divided into approximately the same parts as the number of incremental samples to be taken according to Annex 2, column 2. Similarly, sampling shall be carried out where the lot is sampled from feed flow in a dynamic manner or in bulk feed.
(b) for feed, additives and premixtures in packages, at least one incremental sample shall be taken from each packaging intended for sampling; the contents of the package are emptied separately and a partial sample is then taken.
(c) In the case of liquid or semi-liquid feedingstuffs, partial samples shall be taken after uniform mixing of the contents of the packaging for the taking of the incremental samples. At least one incremental sample shall be taken from each package. Similarly, partial sampling shall be carried out where the lot is sampled from feed flow in a dynamic manner.
(d) In the case of liquid or semi-liquid feedingstuffs which cannot be mixed evenly, partial samples shall be taken from the various depths of the packaging. The provisions shall not apply to the collection of liquid and semi-liquid feed in the case of sampling from feed flow in a dynamic manner, in which such feed is generally not sampled in the initial phase of feed flow. However, in such cases the volume of the aggregate sample shall be at least 10 litres.
(e) In the case of feed in blocks or lizas, one part of each block or of the lick intended for sampling shall be taken.
(f) In the case of grazing crops, one full handful shall be considered as a partial sample.
(2) Parts of feedingstuffs, additives and premixtures for which the presence or content of undesirable and prohibited substances and products is to be determined shall be divided into approximately the same parts corresponding to the expected number of aggregate samples referred to in Annex 3, column 2. The total number of incremental samples determined in accordance with Annex 2, column 2, shall be evenly divided into all parts of the sampled lot. Partial samples from individual parts cannot be mixed.
3. The incremental samples from each individual part of the sampled lot taken in accordance with point 2 shall be taken into an aggregate sample which shall be adjusted separately and shall be marked according to the sampling plan with the appropriate number of the part of the lot from which they originated.
4. The aggregate samples shall be treated by mixing until they are even. Where lumps are present in the aggregate sample, they shall be crushed separately and then mixed with the remainder of the aggregate sample. The weight or volume of the aggregate sample shall be reduced by a mechanical divider or a quarter to a mass of two kilograms or a volume of two litres.
5. Partial samples for the assessment of the homogeneity of the lot shall be taken from randomly selected packaging or, in the case of bulk feed, from randomly selected sites which are evenly distributed across the sampled lot. The number of incremental samples taken from the lot is given in Annex 14.
6. The incremental samples to assess the working accuracy of the mixing device shall be taken so that their collection is evenly distributed over the entire area of the mixing device space or, when sampled outside the mixing compartment, evenly distributed according to the number of packaging or weight sampled.
7. The methods of sampling for the professional supervision and testing of the levels of dioxins (PCDD / Fs) and the determination of dioxin-like PCBs in certain feedingstuffs are set out in Annex No 18, Part 1.
Příloha č. 7
Annex No 7 to Decree No. 124 / 2001 Coll.
Modification of final samples of feed, feed additives and premixtures for laboratory testing
1. General sampling adjustment procedures
1.1. Feed, feed additives and premixtures shall be adjusted as required for testing. The treatment of the samples shall be based on their consistency, structure, moisture and fat content.
1.2. Mix the final sample thoroughly on a dry, smooth and clean mat. Then the quartz after spreading into a low layer and gradually removing two opposite parts of the split sample or using a mechanical divider is divided into two equal parts. Depending on the weight of the final sample, the division into two equal parts shall be repeated until one part corresponds to the mass required for the test sample. A rotary divider may also be used to divide the final sample. The mass of the test sample shall represent at least 100 g of dry matter of the final sample. If the weight of the final sample does not exceed 500 g of the dry matter of the sample, the whole final sample shall be considered as the part from which the test sample is prepared and its weight need not be reduced. In the case of a final sample which cannot be mixed perfectly without prior particle size adjustment, the whole sample shall first be adjusted appropriately so that the particle size is homogeneous. Adjustments may relate to drying, defatting, cutting, etc. This provision shall not apply to final samples to assess the content of undesirable substances, homogeneity and working accuracy of the mixing device.
1.3. The final sample outside the parts that have been assigned as a test sample shall be stored in a suitable, clean, dry, airtight closed container. It shall be left unmodified and shall be used for sensory or physical tests, or microscopic examination, etc.
1.4. The test sample shall be prepared by milling so that the batches required for each test are homogeneous and represent the final sample. The test sample after treatment shall contain particles which pass through a wire sieve with a mesh size of 1 mm, unless otherwise specified.
1.5 If the original moisture content of the final sample is determined, the part for this determination must be separated immediately after the sample packaging has been opened, if it has not already been separated during sampling, and the necessary adjustment must be made.
1.6. The final samples for the assessment of the content of undesirable substances shall be assessed in advance in a sensory manner, any physical and special tests carried out, and the final sample shall be adjusted as a whole so that the particles fall through a wire sieve with a mesh size of 1 mm, and then mix perfectly so that the lashes required for each test are homogeneous and represent the final sample. For each test, the retractions shall be prepared from the sample thus modified.
1.7. The final samples for the assessment of homogeneity and for the assessment of the working accuracy of the mixing device shall first be adjusted as a whole so that the particles fall through a wire sieve with a mesh size of 1 mm, and then mix perfectly so that the batches for each test are homogeneous and represent the final sample. For each test, the retractions shall be prepared from the samples thus prepared.
2. Modification of the final sample by drying
If the preparation of the sample cannot be carried out without significant changes in the moisture content of the sample, the moisture content must be determined before and after the preparation of the sample according to the following test method.
Working procedure:
The final sample shall be spilled on a clean drying bowl and spread evenly across the entire surface so that the layer height is not more than 20 mm. A quantity shall be taken from the final sample to obtain about 200 g of pre-dried sample by pre-drying. The sample bowls shall be dried at a temperature (55 ± 5) ° C until a solid, crush-proof consistency is obtained and the sample is mixed periodically. After pre-drying, the sample should be allowed to cool off on the bowl and be conditioned for about 12 hours to a steady-state laboratory humidity. During drying and conditioning, no dissolution or undesirable contamination of the sample shall occur. The test sample as described in paragraph 1.4 of this annex shall be adjusted from the final sample so modified.
3. Special sample modification procedures
3.1. Adjusting the final sample by defatting
Purpose, scope and principle
For dry samples with a relatively high fat content, partial extraction must be carried out before their own preparation. The essence of this presentation is the partial defatting of the sample to reduce the fat content. The larger fat content is extracted by diethyl ether, petroether or hexane and analysed in a partially defatted sample. The contents of the ingredients, determined by analysis of the partially defatted sample, shall be converted into those of the final non-fat sample. The extraction device in the safety design (Soxhlet, etc.) is used to defat the sample.
3.2. Modification of the final sample by pre-drying with suction material
Purpose, scope and principle
The procedure is used for low consistency samples for which a high fat content does not allow direct drying. The sample shall be treated with appropriate intake material (e.g. hard wood sawdust, preferably beech), analysed in advance for the contents of all the components to be determined. The essence of this presentation is to suck the fatty ingredient of the feed into the intake material, which does not contain fat and thus reduce the proportional fat distribution in the sample. The contents of the components specified in the mixture of the sample and the intake mass shall be converted into the contents of the final sample.
3.3.Adjustment of the final sample by mixing
Purpose, scope and principle
If the feed is tested in its original state without pre-drying and has a liquid pasture structure, the sample shall be treated by mixing. It blends for so long as there are no apparent differences in particle size or material diversity.
3.4. Adjusting the final sample by crushing
Purpose, scope and principle
Where the feed has a lumpy structure or is in the form of granules or moulds which prevent pre-drying or grinding, the treatment shall be carried out by crushing.
3.5. Modification of the final sample with urea content
Purpose, scope and principle
If the feed contains more than 5 g of urea in 1 kg, the whole unreduced final sample shall be treated in accordance with the procedure referred to in paragraph 1.4 of this Annex. The test sample is obtained after mixing and subsequent quarting of the ground-treated sample.
3.6. Adjusting the final sample of animal or vegetable fat and oil
Purpose, scope and principle
The test sample shall be obtained from a homogenised final sample. If the test procedure so requires, they isolate insoluble particles by filtration and the water is removed by drying anhydrous sodium sulphate. The method is not suitable for emulsified fats.
3.7. Sample preparation procedures and requirements for analytical methods used to perform expert surveillance and analysis of the levels of dioxins (PCDD / Fs) and dioxins similar to polychlorinated biphenyls in certain feedingstuffs are set out in Annex No 18, Part 2
Příloha č. 8
Annex No 8 to Decree No. 124 / 2001 Coll.
Storage of samples of feed, feed additives and premixtures
1. The storage of final and test samples shall be ensured in such a way as to avoid changes in the characteristics observed, except those for which the change cannot be prevented, such as fat acidity number, presence of pests, microbial values, contents of specifically active substances subject to degradation, odour, etc.
Preservatives or anti-pest products may be used if they do not affect the quality characteristics observed.
1.1. Samples which are intended for laboratory testing of vitamins or light sensitive substances must be kept in packs which prevent light access.
1.2. The storage space temperature should not exceed 25 ° C and the relative humidity should not exceed 60%.
1.3. Samples of animal and vegetable fats and oils shall be kept in an inert and airtight container in a refrigerator at a maximum temperature of 10 ° C and protected from light. The part of the final sample which has not been subjected to tests affecting its composition shall be kept as a priority. Under the above conditions, samples shall be kept for 6 months from the date of arrival of the sample in the laboratory. After this period, samples shall be considered perishable.
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Regulation Information
| Citation | Decree of the Ministry of Agriculture No. 124 / 2001 Coll., laying down the requirements for sampling and the principles of methods of analysis of feedingstuffs, additives and premixtures and the method of storage of samples |
|---|---|
| Regulation Type | Order |
| Author | - |
| Collection | Code of Laws |
| Date of Promulgation | 10.04.2001 |
|---|---|
| Effective from | 01.05.2001 |
| Effective until | - |
| Status | Valid |
Legal Areas:
Administrative law
Agriculture
The regulation text is for informational purposes only.
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