INTERNATIONAL Iso STANDARD 6498 Second edition 1998-17-01 Animal feeding stuffs — Preparation of test samples Aliments des animaux — Préparation des échantilons pour essai Reference number 180 6498:1998(E}1SO 6498:1998(E) Foreword ISO (the International Organization tor Standardization) is a worldwide tederation of national standards bodies (ISO member bodies}. The work of Preparing Intemational Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented ‘on that committee. International organizations, governmental and non- governmental, in liaison with ISO, also take part in the work, ISO collaborates closely with the Intemational Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. international Standards are drafted in accordance with the rules given in the ISOMEC Directives, Part 3. Draft International Standards adopted by the technical committees are Circulated to the member bodies for voting. Publication as an Intemational ‘Standard requires approval by at least 75 % of the member bodies casting avole. International Standard [SO 6498 was prepared by Technical Committee ISO/TC 34, Agricutural food products, Subcommittee SC 10, Animal feeding stuffs, This second edition cancels and replaces the first edition (ISO 6498:1983), ‘which has been technically revised. ‘Annex A of this International Standard is for information only. © 1807998 A rights rasorved. Unless ofnersise spectted, no part of tis pubicaton may be reproduced Cr utlized in any form or by any means, electronic or mecharical,incluting photocopying anc ‘mierofim, without perrission in wing from tha publisher. Intemational Organization for Standardization ‘Gasp postale 66 = CH-1211 Geneve 20 » Suitzorand Internet is0@iso.ch Printod in SwitzertandINTERNATIONAL STANDARD sO 150 6498:1998(E) Animal feeding stuffs — Preparation of test samples 1 Scope This International Standard specifies methods for the preparation of test samples from laboratory samples of animal feeding stuts including pet foods. 2 Normative references ‘The foliowing normative documents contain provisions which, through reference in this text, constitute provisions of this Intemational Standard. For dated references, subsequent amendments to, or revisions of, any of these publications do not apply. However, parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO and 1EC maintain registers of currently valid International Standards. 180 6492, Animal feeding stuffs — Determination of fat content. ISO 6496, Animal feeding stutts — Determination of moisture content. 3 Terms and definitions For the purposes of this Intetnational Standard, the following terms and definitions apoly. 34 laboratory sample sample representative of the quality and condition of the lot, obtained by reduction of the bulk sample and intended for analysis or other examination 32 test sampie representative portion of the laboratory sample, obtained by dividing by means of a sample divider or by hand, if necessary after reduction of the particle size 3.3 test portion representative portion of the test sample or laboratory sample 4 Principle For solids, the laboratory sample is thoroughly mixed and divided successively using a specified procedure until a test sample of a suitable size is obtained. A process of crushing, grinding, mincing or homogenizing is used, where appropriate, 10 ensure thal the test sample, from which the test portion(s) will be taken, truly represents the laboratory sample. In the case of a fluid feeding stuff, the laboratory sample is mixed mechanically and a ‘representative test sample is obtained while the fluid is agitatedISO 6498:1998(E) e180 5 Apparatus 5.1. Mechanical mill, easy to clean and capable of grinding feeding stuffs without generation of excessive heat {and without causing appreciable change in moisture, until the sample passes completely through a sieve ot appropriate aperture size (5.5). A few feeding stutts are likely to lose or gain moisture. In these cases, it is necessary to apply a correction factor to the results (see 7.2 and clause 8). NOTE The screen size in the mils not necessary the same as the sieve size for checking the extent of grinding. 5.2. Mechanical stirrer or homogenizer 5.3. Mincer, fitted with a 4 mm plate. 5.4 Crushing apparatus, for example, a pestle and mortar. 5.5 Sieves, of aperture sizes 1,00 mn, 2,80 mm and 4,00 mm, made from woven metal wire cloth, 8.6 Dividing or quartering apparatus, such as a conical divider (see Figure A.1), muttiple-siot divider with a sorting system (see Figure A.2), or other dividing apparatus that will ensure uniform distribution of the components of the laboratory sample in the test sample, 5.7. Sample container, suitabie for protecting the test sample from change in composttion, and from the effect of light, and of such a size that it will be almost completely filed by the test sample, It is essential that the container can be securely closed. 6 Sampling ‘Sampling is not part of the method specified in this International Standard. A recommended sampling method is, Given in 1SO 6497 [1]. Itis important that the laboratory receive a sample which is truly representative and has no! been damaged or ‘changed during transport or storage. ‘Store the sample in such a way that deterioration and change in composition are minimized. 7 Procedure WARNING: It is emphasized that care is to be taken to ensure that the apparatus is not a source of contamination. 7A Grinding TAA General Grinding of some samples may lead to a loss or gain of moisture and, if appropriate, allowance for this should be made (see 7.2 and clause 6). Grinding shouid be as rapid as possible and exposure to the atmosphere should be minimized. itnecessary, first break or crush the pieces to a suitable size for grinding. It is essential that the sample be thoroughly mixed betore each stage of the procedure. 7.1.2 Fine samples 1 the laboratory sample passos the 1,00mm sieve (5.5) completely. mix it thoroughly. Divide the mixture successively using the dividing or quartering apparatus (5.6) until a test sample of suitable size is obtained (00 7.9).etso 180 6498:1998(E) 7.1.3 Coarse samples 7.1.3.1 Hf the laboratory sample does not pass the 1,00 mm sieve (5.6) completely, but passes the 2,80 mm sieve completely, mix it thoroughly and prepare a sample of suitable size (see 7.9) by successive divisions as in 7.4.2. 7.1.3.2 Carelully grind this sample in the well-cleaned mill (6.1) as in 7.1.1, until t passes through the 1,00 mm sieve completely. 7.1.4 Coarser samples 7.1.4.1 Ifthe laboratory sample does not pass completely through the 2.80 mm sieve (5.5), carefully grind it in the welk-cleaned mill (5.1) until it passes the 2,80 mm sieve completely. Mix t thoroughly, 7.1.42 Divide the ground laboratory sample successively by means of the dividing apparatus (5.6) until a test sample of suitable size (see 7.9) for all the determinations required is obtained. Grind this sample in the well- cleaned mill (5.1) until i passes the 1,00 mm sieve (5.5) completely. 7.2. Samples likely to lose or gain moisture If grinding operations are likely to result in loss or gain of moisture, determine the moisture content by the method described in ISO 6496. Apply the method to the well-mixed laboratory sample as received and to the prepared test sample, so that the results of analyses may be corrected to relate to the sample in its original condition as regards. moisture content (see clause 8) 7.3. Samples difficutt to grind It the condition of a laboratory sample not passing through the 4,00 mm sieve (5.5) makes grinding difficult, take a portion immediately atter the preliminary mixing described in 7.1.3.1, or after the preliminary grinding procedure desoribed in 7.1.4.1. Determine the moisture content by the method described in ISO 6496. Dry the sample unti, after crushing with the pestle and mortar (5.4) or by other means, it passes the 1,00 mm sieve completely. Again determine the moisture content of the prepared test sample so that the results of analyses may be corrected to relate to the sample in its original condition as regards moisture content (see clause 8), 7.4 Moist feeding stuffs such as canned or chilled pet foods Homogenize the laboratory sample (which may be the entire contents of a can or other package) using the mechanical stirrer or homogenizer (5.2). Thoroughly mix the homogenized sample. Fill a clean, dry sample container (6.7) and close tightly. Take test portions as scon as possible, preferably immediately. Otherwise store the test sample at between 0 °C and 4°C. 7.5 Frozen feeding stuffs Cut oF break the laboratory sample into small pieces with a suitable implement. Immediately pass the pieces through the mincer (5.3). Mix the minced sample until any quid that has separated out is thoroughly re-dispersed ‘throughout the sample. Filla clean, dry sample container (5.7) and close tightly. Take test portions as soon as possible, preferably immediately, storing the test sample at between 0 °C and 4 °C. 7.8 Feeding stuffs of intermediate moisture content Slowly pass the laboratory sample through the mincer (6.3). Thoroughly mix the minced sample and immediately pass it through a 4,00 mm sieve (5.5). Fil a clean, dry sample container (5.7) and close tightly. {the nature of the laboratory sample is such that it cannot be minced, mix and grind it as well as possible by hand.ISO 6498:1998(E) 9180 77 Silage and liquid samples 7.1.1 Grass or cereal silage Pass the entire laboratory sample through the mechanical mill (5.1) if possible, or otherwise chop it as finely as possible, Mix thoroughly and transfer a test sarmpie of at least 100 g to a sample container (5.7) If the laboratory sample cannot be passed through the mill or cannot be finely chopped, mix i as thoroughly as possible and determine the moistura content by the method described in ISO 6496, Dry the laboratory sample (for example, overnight at between 60 °C and 70 °C in an electrically heated oven, well ventilated) and then pass it through the mechanical mill (5.1). Mix thoroughly and transfer a test sample of at least 100g to a sample container (6.7), Determine the moisture content of the prepared test sample by the method described in ISO 6498 and apply a correction to all results (see clause 8). 7.7.2 Liquid samples including fis silage Mix the laboratory sample using a mechanical stizer or homogenizer (5.2), 30 that any separated material (ground bone, oil, etc.) is completely dispersed. During agitation, transfer 50 ml to 100 m! to a sample container (5.7) using a ladle, beaker or wide-bore pipette 7.8 Samples for which there are speci requirements NOTE 1 Some determinations may require special preparation of the lest samples, The specific procedures required are described in the relevant section of the test method. For determinations requiring special degrees of fineness, further grinding may be necessary. In such cases, prepare another test sample as described in 7.1, 7.2 or 7.3, but having the required degree of fineness. In some cases it may be necessary to avoid breaking or damaging the laboratory sample, for example, for the determination of pellet hardness. NOTE 2 If the laboratory sample is thought to be nonhomogeneous, for example for analytes such as mycotoxins medicinal additives, it may be necessary to grind the whole of the sample and then reduce the sample size 10 produce suitable test portion, Ht the sample is fatty, the test sample may be prepared by warming and mixing. In some cases preliminary extraction of fat may be necessary. This shall be carried out in accordance with ISO 6492, Ht microbiological examination is required, the sample shall be handled under sterile conditions and in such a way that the microbial condition does not change. 7.9 Size and storage of test samples Prepare a sufficient test sample (or all the determinations likely to be required and not lass than 100 g. Completely fil the chosen container (6.7) without delay and close it securely. Store the test sample under such conditions that changes are reduced to a minimum, paying particular attention to the avoidance of exposure to light and to the effect of temperature, 8 Correction factor 8.1 General It there is likely to be a loss or gain of moisture during the grinding or mixing operations, itis necessary to use @ correction factor to relate the results of analyses to the sample in its original condition as regards moisture content. A similar concept applies if a praliminary extraction of fat is carried out.e180 ISO 6498:1998(E) 8.2 Calculation Calculate the correction factor s by the equation: J is the correction factor; sp. is the mass fraction of moisture, expressed in percent, of the laboratory sample, datermined by the method described in ISO 6496; wy is the mass fraction of moisture, expressed in percent, of the prepared test sample, determined by the ‘method described in ISO 6486. 8.3 Correction of results Multiply the results of analyses by the correction factor f.ISO 6498:1998(E) Annex A (informative) Examples of dividing apparatus 1 2 3 4 5 6 Key + Hopper 6 Outer funnet 2 curett 7 Recoptacle 3. Spaces which open into outer tunnel 8 Baso of cone 4 Ducts which spout into inner funnel 9 Peak of cone 5 Inner tunnel 10 Ducts connected below base of cone Figure A.1— Conical divider180 6498:1998(E) eso Bibliography U1] 180.6497, Animal feeding siutts — Sampling.ISO 6498:1998(E) e180 aS Ics 65.120 Descriptors: agricultural prodvets, food, animal feeding products, tas specimens, specimen preparation Price basec'on 8 pages ee es EEE