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1、BRITISH STANDARD BS EN ISO 9831:2003 Incorporating Amendment No. 1 to BS ISO 9831:1998 (renumbers the BS ISO as BS EN ISO 9831:2003) Animal feeding stuffs, animal products, and faeces or urine Determination of gross calorific value Bomb calorimeter method The European Standard EN ISO 9831:2003 has t
2、he status of a British Standard ICS 65.120 ? Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 13:52:19 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 9831:2003 This British Standard, having been prepared under the direction of the Consumer Products and Services Sector Board, was publishe
3、d under the authority of the Standards Board and comes into effect on 15 October 1998 BSI 12 March 2004 ISBN 0 580 30383 7 National foreword This British Standard is the official English language version of EN ISO 9831:2003. It is identical with ISO 9831:1998. The UK participation in its preparation
4、 was entrusted to Technical Committee AW/10, Animal feeding stuffs, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referr
5、ed to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the necessary provisi
6、ons of a contract. Users are responsible for its 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 international/European committee any enquiries on the interpretation, o
7、r 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 ISO title page, the EN ISO foreword page, the ISO title page, pages
8、 ii and iii, a blank page, pages 1 to 18, the Annex ZA page and a back cover. This BSI copyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No.DateComments 1485612 March 2004Implementation of the European Standard Licensed
9、Copy: sheffieldun sheffieldun, na, Sun Nov 19 13:52:19 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 9831 November 2003 ICS 65.120 English version Animal feeding stuffs, animal products, and faeces or urine - Determination of gross calorific valu
10、e - Bomb calorimeter method (ISO 9831:1998) Aliments des animaux, produits dorigine animale et excrments ou urines - Dtermination de la valeur calorifique brute - Mthode la bombe calorimtrique (ISO 9831:1998) Futtermittel, tierische Produkte und Kot oder Urin - Bestimmung des effektiven Brennwerts -
11、 Verfahren mit der kalorimetrischen Bombe (ISO 9831:1998) This European Standard was approved by CEN on 13 November 2003. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard witho
12、ut any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the 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
13、 by translation under the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Hungary, Ic
14、eland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2003 CENAll ri
15、ghts of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 9831:2003 E Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 13:52:19 GMT+00:00 2006, Uncontrolled Copy, (c) BSI I NESO 89:1302( 30E) 2 Foreword The text of ISO 9831:1998 has been pre
16、pared by Technical Committee ISO/TC 34 “Agricultural food products” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 9831:2003 by Technical Committee CEN/TC 327 “Animal feeding stuffs - Methods of sampling and analysis“, the secretariat of which is held b
17、y 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 May 2004, and conflicting national standards shall be withdrawn at the latest by May 2004. According to the CEN/CENELEC Internal Regulations,
18、 the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Sw
19、itzerland and the United Kingdom. Endorsement notice The text of ISO 9831:1998 has been approved by CEN as EN ISO 9831:2003 without any modifications. NOTE Normative references to International Standards are listed in annex ZA (normative). EN ISO 9831:2003 Licensed Copy: sheffieldun sheffieldun, na,
20、 Sun Nov 19 13:52:19 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 9831:2003 21 ISB March 4002 iii oFerword SIO (the IntenratoinaO lrganiazoitn for atSndadrtazinoi) si a owdlrwdie edefarito nof tanianol tsdnaadrob sidse (IOS emebmr obid)se. Thow efo kr prepnirag nItenratoinal tSnadadrs si nomrad
21、eirrac yll tuo thguorSI ht Oelacinhc timmocteeaE .sem hcbmer doby tnietsered ni s aujbtce fow rhhci a ethcnilac immocttee has ebse neatblisah deht shir ethg ot eb erserptneeo dn ahtt immocttee. tnIenratioanl oraginaztiog ,snonrevtnemal an-non devogtnemnral, in liaison with ISO, also take part in tho
22、w ekrSI .alloc Otarobes olcstiw yleh the nItenrtaoinalE ltcertohceniacoC lsimmsoin (I)CE on lla ttamsre of letcertoinhceacl stanadidrzation. tfarD tnIenratlanoi Stsdradna adtpoet yb dht eeacinhctimmoc ltees era icucrlaetd ot the emebmr obdies fov rotinguP .btaciloin sa na nIetnrtanoial Standadr qeru
23、seri approvla yb ta elsat 75 % of hte emebmr obdies tsacnig a vote. nItenrtaoinaS ltnadadr SIO 389w 1as prpeerad yb TehcniacoC ltimmtee SIO/CT ,43 ucirgAof larutldorp dotcus, uSbcmomiette CS ,01 laminA gnideef tsfu.sf nAnex na Ad nAnex era B na inetgral patr fo thnI sitenrtaoinaS ltandadr. C xennA t
24、F xennA o are foi rnamroftiolno ny. Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 13:52:19 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 9831:2003 ii Contents Page Forewordiii 1Scope1 2Normative references1 3Definitions1 4Principle1 5Reagents and materials1 6Apparatus2 7Sampling4 8Prepa
25、ration of test sample and test portion4 9Procedure4 10Corrections6 11Expression of results8 12Precision8 13Test report9 Annex A (normative) Determination of the effective heat capacity of the calorimeter10 Annex B (normative) Special procedures for preparation of the test sample11 Annex C (informati
26、ve) Method of checking that the average deviation of the rate of change of temperature is within the specified limit12 Annex D (informative) Examples of calculating the results of calorific determinations13 Annex E (informative) Results of interlaboratory tests17 Annex F (informative) Bibliography18
27、 Table 1 Repeatability limit (r) and reproducibility limit (R)9 Table C.1 Acceptable difference sequences12 Table C.2 Example13 Table D.1 Observed temperature readings15 Table E.1 Statistical results of the interlaboratory tests17 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 13:52:19 GMT+0
28、0:00 2006, Uncontrolled Copy, (c) BSI EN ISO 9831:2003 BSI 12 March 2004 iii Foreword 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
29、 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 cl
30、osely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. 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 least
31、75 % of the member bodies casting a vote. International Standard ISO 9831 was prepared by Technical Committee ISO/TC 34, Agricultural food products, Subcommittee SC 10, Animal feeding stuffs. Annex A and Annex B are an integral part of this International Standard. Annex C to Annex F are for informat
32、ion only. Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 13:52:19 GMT+00:00 2006, Uncontrolled Copy, (c) BSI blank Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 13:52:19 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 9831:2003 BSI 12 March 2004 1 1 Scope This International Standa
33、rd specifies a method for the determination of the gross calorific value of animal feeding stuffs, animal products and faeces or urine at constant volume in an adiabatic, an isothermal, or a static bomb calorimeter. The result obtained by this method is the gross calorific value of the test sample a
34、t constant volume, the water of the combustion products being condensed to liquid at the calorimeter temperature. NOTEThe international reference temperature for thermochemistry of 25 C is used as the reference temperature for calorific value, although the temperature dependence of the calorific val
35、ue of the materials to which this International Standard applies is small (about 1 Jgp1Kp1). 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the editions indicat
36、ed were valid. All standards are subject to revision, and parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO maintain registers of currently valid Inter
37、national Standards. ISO 651:1975, Solid-stem calorimeter thermometers. ISO 652:1975, Enclosed-scale calorimeter thermometers. ISO 1770:1981, Solid-stem general purpose thermometers. ISO 1771:1981, Enclosed-scale general purpose thermometers. ISO 1928:1995, Solid mineral fuels Determination of gross
38、calorific value by the bomb calorimeter method, and calculation of net calorific value. ISO 3696:1987, Water for analytical laboratory use Specification and test methods. ISO 6496: 1), Animal feeding stuffs Determination of moisture and volatile matter content. ISO 6498: 2), Animal feeding stuffs Pr
39、eparation of test samples. 3 Definitions For the purposes of this International Standard, the definitions given in ISO 1928 apply. 4 Principle Combustion of a weighed portion of the test sample in oxygen in a bomb calorimeter under standardized conditions. Calculation of the gross calorific value fr
40、om the temperature rise of the water in the calorimeter vessel and the mean effective heat capacity of the calorimeter. Allowances are made for the heat released by the ignition fuse, for thermochemical corrections and, where appropriate, for heat losses from the calorimeter to the water jacket. 5 R
41、eagents 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 Oxygen, at a pressure capable of filling the bomb to 3 MPa and free from combustible matter. NOTE 1Oxygen manufactured by an electrolytic process may co
42、ntain up to 4 % of hydrogen and is therefore unsuitable. NOTE 21 MPa = 1 MN/m2. 1)To be published. (Revision of ISO 6496:1983) 2)To be published. (Revision of ISO 6498:1983) Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 13:52:19 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 9831:2003 2
43、BSI 12 March 2004 5.3 Fuse, comprising the following. 5.3.1 Firing wire, nickel/chromium wire (0,16 mm to 0,20 mm in diameter), or platinum wire (0,06 mm to 0,10 mm in diameter). 5.3.2 Cotton thread, white cellulose. 5.3.3 Polyethylene strip, thin film of dimensions 30 mm by 5 mm. 5.4 Polyethylene b
44、ags, of dimensions 68 mm by 110 mm. 5.5 Polyethylene bags, of dimensions 50 mm by 55 mm, and mass approximately 170 mg. 5.6 Silica gel, Chromatographic-grade powder. 5.7 Sodium hydroxide solution, standard volumetric solution, c(NaOH) = 0,1 mol/l. 5.8 Screened methyl orange indicator solution, = 1 g
45、/l. Dissolve 0,25 g of methyl orange and 0,15 g of xylene cyanol FF in 50 ml of 95 % (V/V) ethanol and dilute to 250 ml with water. 5.9 Benzoic acid, thermochemical standard, certified by a national testing authority. Drying or any treatment other than pelleting shall not be carried out. The gross c
46、alorific value at constant volume of the benzoic acid, listed in the certificate for the conditions of use, shall be adopted in calculating the effective heat capacity of the calorimeter (see Annex A). 6 Apparatus Usual laboratory apparatus and, in particular, the following. 6.1 Bomb, capable of wit
47、hstanding safely the pressure developed during combustion. The design shall permit complete recovery of all liquid products. The construction materials shall resist corrosion by the acids produced by the combustion. CAUTION Inspect bomb parts regularly for wear and corrosion. Pay particular attentio
48、n to the condition of the threads of the main closure. 6.2 Calorimeter vessel, made of metal, highly polished on the outside and capable of holding sufficient water to cover completely the flat upper surface of the bomb while the water is being stirred. The vessel shall be provided with a console to
49、 centre the bomb in the vessel and to obtain water circulation below the bomb. 6.3 Stirrer, driven at a constant rotational speed. The stirrer shaft shall contain a non-conducting section below the cover of the water jacket to minimize the transmission of heat to or from the system. If a cover is used for the calorimeter vessel, the non-conducting section shall be above this cover. For isothermal and static bomb calorimeters, the rate of stirring shall ensure that t