1、BRITISH STANDARD BS 5766-23:2001 BS EN ISO 6865:2001 Methods for analysis of animal feeding stuffs Part 23: Determination of crude fibre content Method with intermediate filtration The European Standard EN ISO 6865:2000 has the status of a British Standard ICS 65.120 NO COPYING WITHOUT BSI PERMISSIO
2、N EXCEPT AS PERMITTED BY COPYRIGHT LAWBS 5766-23:2001 This British Standard, having been prepared under the direction of the Consumer Products and Services Sector Committee, was published under the authority of the Standards Committee and comes into effect on 15 May 2001 BSI 05-2001 ISBN 0 580 37285
3、 5 National foreword This British Standard is the official English language version of EN ISO 6865:2000. It is identical with ISO 6865:2000. The UK participation in its preparation was entrusted to Technical Committee AW/10, Animal feeding stuffs, which has the responsibility to: A list of organizat
4、ions represented on this committee can be obtained on request to its secretary. Cross-references Attention is drawn to the fact that CEN and CENELEC Standards normally include an annex which lists normative references to international publications with their corresponding European publications. The
5、British Standards which implement these international or European publications may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not
6、 purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible int
7、ernational/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the EN
8、 ISO title page, the EN ISO foreword page, the ISO title page, pages ii and iii, a blank page, pages 1 to 10, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date Commen
9、tsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM ENISO6865 October2000 ICS06.012 Englishversion AnimalfeedingstuffsDeterminationofcrudefibrecontent Methodwithintermediatefiltration(ISO6865:2000) AlimentsdesanimauxDterminationdelateneuren cellulosebruteMthodeavecfiltrationintermdiaire(ISO 6865:2000)
10、FuttermittelBestimmungdesRohfasergehaltes VerfahrenmitZwischenfiltration(ISO6865:2000) ThisEuropeanStandardwasapprovedbyCENon4October2000. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyal
11、teration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmember
12、intoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingd
13、om. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2000CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.ENISO6865:2000EForeword ThetextoftheInternationalStandar
14、dISO6865:2000hasbeenpreparedbyTechnical CommitteeISO/TC34“Agriculturalfoodproducts“incollaborationwithTechnicalCommittee CEN/TC327“AnimalfeedingstuffsMethodsofsamplingandanalysis“,thesecretariatof whichisheldbyNEN. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublication ofan
15、identicaltextorbyendorsement,atthelatestbyApril2001,andconflictingnational standardsshallbewithdrawnatthelatestbyApril2001. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsof thefollowingcountriesareboundtoimplementthisEuropeanStandard:Austria,Belgium, CzechRepublic,Den
16、mark,Finland,France,Germany,Greece,Iceland,Ireland,Italy, Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandtheUnited Kingdom. NOTEFROMCEN/CS:Theforewordissusceptibletobeamendedonreceptionofthe Germanlanguageversion.Theconfirmedoramendedforeword,andwhenappropriate,the normativeannexZ
17、Aforthereferencestointernationalpublicationswiththeirrelevant EuropeanpublicationswillbecirculatedwiththeGermanversion. Endorsementnotice ThetextoftheInternationalStandardISO6865:2000wasapprovedbyCENasaEuropean Standardwithoutanymodification. ENISO6865:2000 Reference number ISO 6865:2000(E) INTERNAT
18、IONAL STANDARD ISO 6865 First edition 2000-10-15 Animal feeding stuffs Determination of crude fibre content Method with intermediate filtration Aliments des animaux Dtermination de la teneur en cellulose brute Mthode avec filtration intermdiaire ENISO6865:2000 ii ENISO6865:2000 ISO 5686:(0002)Eiii F
19、oreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a te
20、chnical 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 International Electrotechnical Commission (IEC) on all matters
21、of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard re
22、quires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this International Standard may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Sta
23、ndard ISO 6865 was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 10, Animal feeding stuffs. Annex A of this International Standard is for information only. ENISO6865:2000 ENISO6865:2000 INTENRATIONAL TSANDADR ISO 5686:(0002)E1 Animal feeding stuffs Determination of crude
24、fibre content Method with intermediate filtration 1 Scope This International Standard specifies a method with intermediate filtration for the determination of the crude fibre content. A manual procedure and a semi-automatic procedure are described. The method is applicable to animal feeding stuffs w
25、ith a crude fibre content greater than 10 g/kg. NOTE For animal feeding stuffs with a crude fibre content equal to or less than 10 g/kg, the method described in ISO 6541 7 may be used. This International Standard is also applicable to cereals and pulses. 2 Normative references The following normativ
26、e documents contain provisions which, through reference in this text, constitute provisions of this International 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
27、 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 documents referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards.
28、 ISO 3696:1987, Water for analytical laboratory use Specification and test methods. ISO 6498:1998, Animal feeding stuffs Preparation of test samples. 3 Term and definition For the purposes of this International Standard, the following term and definition apply. 3.1 crude fibre content loss in mass r
29、esulting from ashing of the dried residue obtained after acid and alkaline digestion of the sample by the procedure described in this International Standard, divided by the mass of the test portion NOTE The crude fibre content is expressed in grams per kilogram. It may also be expressed as a mass fr
30、action in percent. 4P r i n c i p l e The test portion is treated with boiling dilute sulfuric acid. The residue is separated by filtration, washed and then treated with boiling potassium hydroxide solution. The residue is separated by filtration, washed, dried, weighed and then ashed. The loss in m
31、ass resulting from ashing corresponds to the mass of crude fibre in the test portion. ENISO6865:2000 ISO 5686:(0002)E 2 5 Reagents and materials Use only reagents of recognized analytical grade. 5.1 Water, complying with at least grade 3 in accordance with ISO 3696. 5.2 Hydrochloric acid, c(HCl) = 0
32、,5 mol/l. 5.3 Sulfuric acid, c(H 2 SO 4 )=(0 ,1 3 0,005) mol/l. 5.4 Potassium hydroxide solution, c(KOH) = (0,23 0,005) mol/l. 5.5 Acetone. 5.6 Filter aid: sea sand , or Celite 1) 545, or material of an equivalent quality. Before use, treat sea sand with boiling hydrochloric acid c(HCl) = 4 mol/l, w
33、ash with water until free from acid and heat at a temperature of (500 25) C for at least 1 h. Before use, heat other filter aids at a temperature of (500 25) C for at least 4 h. 5.7 Antifoam agent, for instance n-octanol. 5.8 Light petroleum, boiling range 40 Cto60C. 6 Apparatus Usual laboratory app
34、aratus and, in particular, the following. 6.1 Grinding device, capable of grinding the sample so that it passes completely through a sieve with 1 mm apertures. 6.2 Analytical balance, with accuracy of at least 0,1 mg. 6.3 Filter crucibles, of quartz, porcelain or hard glass, with fused sintered filt
35、er plate with a pore size of 40 m to 100 m (porosity grade P 100 according to ISO 4793:1980 1). Before using for the first time, carefully and gradually heat a new filter crucible to a temperature not exceeding 525 C and leave for a few minutes at (500 25) C. Stainless-steel crucibles with stainless
36、-steel sieve plates with an aperture size of 90 m of identical performance characteristics may be used as an alternative. 6.4 Porcelain sieve plates. 6.5 Incineration dishes. 6.6 Beakers or conical flasks, of 500 ml capacity, provided with a suitable cooling device, for example a condensor or a dish
37、. 1) Celite is the tradename of a commercially available product. This information is given for the convenience of users of this International Standard and does not constitute an endorsement by ISO of this product. Equivalent products may be used if they can be shown to lead to th esa mer e su lt s.
38、 ENISO6865:2000 ISO 5686:(0002)E3 6.7 Drying oven, electrically heated and ventilated, capable of being maintained at a temperature of (130 2) C. 6.8 Desiccator, containing blue silicagel as desiccant, provided with a perforated plate, preferably of aluminium or stainless steel, of thickness 2 mm to
39、 3 mm. 6.9 Muffle furnace, electrically heated, provided with air circulation and temperature control capable of maintaining the temperature around the crucibles to the nearest 25 C at temperatures of 475 C to 525 C. The reading of the pyrometer of the muffle furnace cannot always be trusted: deviat
40、ions may occur. Therefore, the temperature in the muffle furnace should be checked regularly. Depending on the size and type of the muffle furnace, temperatures in the furnace may differ from one place to another place. When the oven door is closed, adequate air supply should be guaranteed. The volu
41、me flow rate of air should not be so great that material is carried away from the crucibles. 6.10 Cold-extraction device, provided with a support for the filter crucible (6.3); a discharge pipe with a tap to the vacuum and liquid outlet; and connecting rings for connecting the filter crucible (6.3).
42、 6.11 Heating device (for manual method), provided with a suitable cooling device capable of maintaining the volume constant during boiling. 6.12 Heating device (for the semi-automatic method) for acid and alkaline digestion, provided with a support for the filter crucible (6.3); a discharge pipe wi
43、th a tap to the vacuum and liquid outlet; a boiling cylinder of at least 270 ml capacity, with a reflux condenser; connecting rings for connecting the heating device to the filter crucible (6.3) and the boiling cylinder; and optionally, provision for compressed air. Before use, preheat the apparatus
44、 with boiling water for 5 min. 7 Sampling Sampling is not part of the method specified in this International Standard. A recommended sampling method is given in ISO 6497 6. It is important that the laboratory receive a sample which is truly representative and has not been damaged or changed during t
45、ransport or storage. 8 Preparation of test sample Prepare the test sample in accordance with ISO 6498. Using the grinding device (6.1), grind the air-dry laboratory sample so that it passes completely through a sieve with 1 mm apertures. Mix thoroughly. ENISO6865:2000 ISO 5686:(0002)E 4 For the manu
46、al method, proceed in accordance with clause 9. For the semi-automatic method, proceed in accordance with clause 10. 9 Procedure for manual method 9.1 Test portion Weigh about 1 g of the prepared test sample (clause 8) to the nearest 0,1 mg (m 1 ). If the fat content of the sample exceeds 100 g/kg,
47、or if the sample contains fats which cannot be extracted directly with light petroleum (5.8), transfer the sample to a crucible (6.3) and proceed in accordance with 9.2. If the fat content of the sample does not exceed 100 g/kg, transfer the sample to a beaker (6.6) and proceed in accordance with 9.
48、3 if the carbonate content, expressed as calcium carbonate, exceeds 50 g/kg. If this is not the case, proceed in accordance with 9.4. 9.2 Preliminary defatting In the cold-extraction device (6.10), defat the sample three times under vacuum with 30 ml of light petroleum (5.8) each time. Dry the residue by suction after each washing. Transfer the residue to a beaker (6.6). If the carbonate cont
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