1、BS EN ISO13906:2008ICS 65.120NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDAnimal feeding stuffs Determinationof acid detergentfibre (ADF) and aciddetergent lignin(ADL) contents (ISO13906:2008)Incorporating Corrigendum March 2009This British Standardwas publis
2、hed underthe authority of theStandards Policy andStrategy Committee on 3ember 2008 BSI 2009ISBN 978 0 580 Amendments/corrigenda issued since publicationDate CommentsBS EN ISO 13906:2008National forewordThis British Standard is the UK implementation of EN ISO 13906:2008 The UK participation in its pr
3、eparation was entrusted to TechnicalCommittee AW/10, Animal feeding stuffs.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are responsible for its correct ap
4、plication.Compliance with a British Standard cannot confer immunityfrom legal obligations.1Dec67112 831 March 2009 Replacement to ISO text EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 13906July 2008ICS 65.120English VersionAnimal feeding stuffs - Determination of acid detergent fibre(ADF) a
5、nd acid detergent lignin (ADL) contents (ISO13906:2008)Aliments des animaux - Dtermination des teneurs enfibres au dtergent acide (ADF) et en lignine sulfurique(ADL) (ISO 13906:2008)Futtermittel - Bestimmung des Gehalts an Sure-Detergens-Faser (ADF) und Sure-Detergens-Lignin (ADL)(ISO 13906:2008)Thi
6、s European Standard was approved by CEN on 11 July 2008.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
7、concerning such nationalstandards may be obtained on application to the CEN Management Centre or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its
8、own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuan
9、ia, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2008 CEN Al
10、l rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 13906:2008: EEN ISO 13906:2008 (E) 3 Foreword This document (EN ISO 13906:2008) has been prepared by Technical Committee ISO/TC 34 “Agricultural food products“ in collaboration with Techn
11、ical Committee CEN/TC 327 “Animal feeding stuffs - Methods of sampling and analysis” the secretariat of which is held by NEN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by January 2009, and conf
12、licting national standards shall be withdrawn at the latest by January 2009. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. According
13、 to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, L
14、ithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 13906:2008 has been approved by CEN as a EN ISO 13906:2008 without any modification. BS EN ISO 13906:2008ISO 13906:20
15、08(E) ISO 2008 All rights reserved iiiContents Page Foreword iv 1 Scope 1 2 Normative references 1 3 Terms and definitions .1 4 Principle2 5 Reagents.2 6 Apparatus .3 7 Sampling.4 8 Preparation of test sample4 9 Procedure .4 10 Calculation and expression of results.6 11 Precision.7 12 Test report 9
16、Annex A (informative) Results of interlaboratory test.10 Annex B (informative) Results of interlaboratory test.14 Bibliography 17 BS EN ISO 13906:2008ISO 13906:2008(E) iv ISO 2008 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of nation
17、al 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 technical committee has been established has the right to be represented on that committee. Internatio
18、nal 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 of electrotechnical standardization. International Standards are drafted in accordance with the rule
19、s given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at l
20、east 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 13906 was prepared by Technical Committee ISO/TC 3
21、4, Food products, Subcommittee SC 10, Animal feeding stuffs. BS EN ISO 13906:2008INTERNATIONAL STANDARD ISO 13906:2008(E) ISO 2008 All rights reserved 1Animal feeding stuffs Determination of acid detergent fibre (ADF) and acid detergent lignin (ADL) contents WARNING The use of this International Sta
22、ndard may involve hazardous materials, operations and equipment. This International Standard does not purport to address any safety risks associated with its use. It is the responsibility of the user of this International Standard to establish appropriate safety and health practices and determine th
23、e applicability of local regulatory limitations prior to use. 1 Scope This International Standard specifies a method for the determination of acid detergent fibre (ADF) insoluble residue and acid detergent lignin (ADL) in all types of animal feeding stuffs. The limit of determination is 1 % mass fra
24、ction for ADF and 1,5 % mass fraction for ADL. A gravimetric routine and reference method is used. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the lates
25、t edition of the referenced document (including any amendments) applies. ISO 6498, Animal feeding stuffs Preparation of test samples 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 acid detergent fibre content ADF content mass fraction of fib
26、rous residue obtained after treatment with cationic detergent in 0,5 mol/l sulfuric acid, primarily consisting of cellulose, lignin and insoluble protein complexes NOTE The ADF mass fraction is expressed as a percentage. 3.2 acid detergent lignin content ADL content mass fraction of residue remainin
27、g after cellulose and other organic matter is solubilized by 72 % mass fraction (12,00 mol/l) sulfuric acid NOTE The ADL mass fraction is expressed as a percentage. BS EN ISO 13906:2008ISO 13906:2008(E) 2 ISO 2008 All rights reserved4 Principle ADF is determined in the first stage of the method. Cat
28、ionic detergent solution is used to remove acid-labile carbohydrates, protein that is not complexed into Maillard products (heat damaged), and fats. The remaining fibrous residue is primarily cellulose and lignin (plant products) or insoluble protein complexes (animal products and heat-damaged feeds
29、). The residue is weighed for the determination of ADF. In the second stage, the remaining residue is solubilized by 72 % mass fraction (12,00 mol/l) sulfuric acid, leaving the lignin (ADL) which is determined gravimetrically. 5 Reagents Use only reagents of recognized analytical grade, unless other
30、wise specified, and only distilled or deionized water or water of at least equivalent purity. 5.1 Acid detergent solution. Add 20 g cetyl(trimethyl)ammonium bromide (technical grade) to 1 l of 0,5 mol/l sulfuric acid, previously standardized. Agitate to aid dissolution. 5.2 Sulfuric acid, 72 % mass
31、fraction (12,00 mol/l). Standardize sulfuric acid (H2SO4) to a relative density of 1,634 at 20 C or 12,00 mol/l as follows. Calculate the mass, in grams, of acid, m(H2SO4), and the mass, in grams, of water, m(H2O), needed to prepare 1 000 ml of solution using Equations (1) and (2): 2424100 98,08 12(
32、H SO )(H SO )mw= (1) where w(H2SO4) is the assay mass fraction of sulfuric acid, expressed as a percentage. ( )224(H O) 1000 1,634 (H SO )mm= (2) where 1,634 is the relative density of 72 % mass fraction sulfuric acid. Weigh water into a 1 000 ml volumetric flask and add the calculated amount of sul
33、furic acid slowly with occasional swirling. Cool the flask in a water bath while adding the required mass of acid. Cool to 20 C and verify the volume. The meniscus should be within 0,5 cm of the calibration mark at 20 C. If volume is too large, remove 5 ml water and add 4,55 ml sulfuric acid. If vol
34、ume is too small, remove 1,5 ml and add 2,5 ml water. Repeat if necessary. 5.3 Filtration aid, diatomaceous earth1). 5.4 Acetone, technical grade. 5.5 n-Octanol, antifoaming agent. 1) Celite, acid washed, and Celite 545 AW are examples of suitable products available commercially. This information is
35、 given for the convenience of users of this International Standard, and does not constitute an endorsement of these products by ISO. Alternative products may be used if they can be demonstrated to give comparable results. BS EN ISO 13906:2008ISO 13906:2008(E) ISO 2008 All rights reserved 36 Apparatu
36、s Usual laboratory apparatus and, in particular, the following. 6.1 Analytical balance. 6.1.1 Analytical balance, capable of weighing to the nearest 1 mg, with readability to 0,1 mg. 6.1.2 Analytical balance, with a measuring range up to 2 500 g, with readability to 1 g, for weighing sulfuric acid (
37、5.2). 6.2 Mill, a cyclone mill or cutter mill or rotary mill or equivalent, giving a mean particle size of 0,22 mm to 0,26 mm. 6.3 Drying oven. 6.3.1 Air-ventilated oven, capable of operating at 103 C 2 C or 130 C 2 C. 6.3.2 Air-ventilated oven, capable of being maintained at 60 C 2 C. To speed up t
38、he drying of moist samples without creating artefact fibres, a vacuum oven, maintained at 60 C 2 C may also be used. 6.4 Refluxing apparatus, with individual heating units and cold water condensers. Any conventional apparatus suitable for crude fibre or amylase-treated neutral detergent fibre (aNDF)
39、 determinations is acceptable. Calibrate heating unit settings so that 50 ml of water boils in 4 min to 5 min when using cold water condensers. A Fibertec2)-type apparatus can be used and should boil 50 ml of water within 10 min. NOTE This setting can be expected to result in significant particle mo
40、vement during refluxing. 6.5 Fritted-disk crucibles. Coarse porosity (pore size 40 m to 60 m) crucibles, 40 ml to 50 ml capacity, or Fibertec P22)(pore size 40 m to 100 m, 26 ml to 28 ml capacity). Clean new crucibles and ash at 525 C 15 C for 1 h. Clean crucibles after each use by ashing at 525 C 1
41、5 C for 3 h, removing ash by inverting in a detergent solution and sonicating for 7 min to 10 min. Rinse crucibles in hot water, and soak in water at room temperature for at least 30 min. Occasionally test filtration rate as follows. Fill each crucible with 50 ml of distilled water (25 ml for Fibert
42、ec P22)crucibles) and record the time required to drain completely without vacuum should be 180 s 60 s for Gooch2)or 75 s 30 s for P2. If drain time is 240 s (or 105 s for P2), clean crucible with acid or alkaline cleaning solution (Reference 4). If cleaning does not improve filtration rate, discard
43、 crucible. 6.6 Vacuum filter manifold. Suitable apparatus e.g. Fibertec2)-type cold extraction unit that allows adequate soaking of fibrous residues. 6.7 Incineration furnace, 525 C 15 C. 6.8 Reflux beakers. As an alternative to a reflux apparatus (6.4), 600 ml Berzelius beakers with condensers, e.g
44、. made from 500 ml round-bottom flasks, may be used. 2) Example of a suitable product available commercially. This information is given for the convenience of users of this International Standard, and does not constitute an endorsement of this product by ISO. BS EN ISO 13906:2008ISO 13906:2008(E) 4
45、ISO 2008 All rights reserved7 Sampling A representative sample should have been sent to the laboratory. It should not have been damaged or changed during transport or storage. Sampling is not a part of the method specified in this International Standard. A recommended sampling method is given in ISO
46、 6497. 8 Preparation of test sample Prepare the test sample in accordance with ISO 6498. Reduce laboratory sample to approximately 100 g (dry weight equivalent) and place half in a moisture-tight, sealed container for total moisture determination. Dry remaining wet ( 15 % mass fraction moisture) mat
47、erials to 10 % mass fraction fat, and is recommended for test samples containing 5 % mass fraction fat. Weigh test samples into previously tared, oven-dried crucibles, place crucible on filtering manifold, extract four times with 30 ml to 40 ml of acetone, allowing the material to soak in acetone fo
48、r 3 min to 5 min each time, vacuum to remove all traces of acetone, air-dry for 10 min to 15 min, and transfer residue to a reflux beaker for fibre analysis. Use the same crucible to collect the fibre residue for each test portion after acid detergent extraction. For the Fibertec2)-type apparatus, p
49、lace the crucible in a cold extraction unit and fill the crucible with 25 ml acetone (5.4). Leave for 3 min to 5 min and filter by applying vacuum. Repeat three times. NOTE To simplify filtration, 1,00 g of filtration aid (5.3) can be added to the crucible before the sample. 9 Procedure 9.1 ADF 9.1.1 General Dry empty crucibles in an oven (6.3.1) at 103 C 2 C for 4 h 1 h if moved from the incineration furnace (6.7) and record tare mass, m1. 9.1.2 Conventional apparatus Weigh, into a Berzeliu
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