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 BS EN ISO 9831:2003 This British Standard, having been prepared under the direction of the Consumer Products and Services Sector Board, was published under the authority of the Standards Board and comes into effect on 15 October 1998 BSI 12 March 2004 ISBN
3、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 was entrusted to Technical Committee AW/10, Animal feeding stuffs, which has the responsibility to: A list o
4、f organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards
5、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 provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does
6、 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, or proposals for change, and keep the UK interests informed; monitor related international and European develo
7、pments 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 ii and iii, a blank page, pages 1 to 18, the Annex ZA page and a back cover. This BSI copyright notice displ
8、ayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date Comments 14856 12 March 2004 Implementation of the European StandardEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM ENISO9831 November2003 ICS65.120 Englishversion Animalfeedingstuffs,
9、animalproducts,andfaecesorurine DeterminationofgrosscalorificvalueBombcalorimeter method(ISO9831:1998) Alimentsdesanimaux,produitsdorigineanimaleet excrmentsouurinesDterminationdelavaleur calorifiquebruteMthodelabombecalorimtrique(ISO 9831:1998) Futtermittel,tierischeProdukteundKotoderUrin Bestimmun
10、gdeseffektivenBrennwertsVerfahrenmitder kalorimetrischenBombe(ISO9831:1998) ThisEuropeanStandardwasapprovedbyCENon13November2003. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.
11、Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsow
12、nlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Slovakia,Spain,Sweden,Switzerland
13、andUn ited Kingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2003CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.ENISO9831:2003EINESO89:1302(30E) 2 Forew
14、ord ThetextofISO9831:1998hasbeenpreparedbyTechnicalCommitteeISO/TC34“Agricultural foodproducts”oftheInternationalOrganizationforStandardization(ISO)andhasbeentaken overasENISO9831:2003byTechnicalCommitteeCEN/TC327“Animalfeedingstuffs Methodsofsamplingandanalysis“,thesecretariatofwhichisheldbyNEN. Th
15、isEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationof anidenticaltextorbyendorsement,atthelatestbyMay2004,andconflictingnationalstandards shallbewithdrawnatthelatestbyMay2004. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsof thefollowingcoun
16、triesareboundtoimplementthisEuropeanStandard:Austria,Belgium,Czech Republic,Denmark,Finland,France,Germany,Greece,Hungary,Iceland,Ireland,Italy, Luxembourg,Malta,Netherlands,Norway,Portugal,Slovakia,Spain,Sweden,Switzerlandand theUnitedKingdom. Endorsementnotice ThetextofISO9831:1998hasbeenapprovedb
17、yCENasENISO9831:2003withoutany modifications. NOTENormativereferencestoInternationalStandardsarelistedinannexZA(normative). ENISO9831:2003EN ISO 9831:2003 21 ISB March 4002 iii oFerword SIO (the IntenratoinaO lrganiazoitn for atSndadrtazinoi) si a owdlrwdie edefarito nof tanianol tsdnaadrob sidse (I
18、OS emebmr obid)se. Thow efo kr prepnirag nItenratoinal tSnadadrs si nomradeirrac 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 ,snon
19、revtnemal an-non devogtnemnral, in liaison with ISO, also take part in thow 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 t
20、he emebmr obdies fov rotinguP .btaciloin sa na nIetnrtanoial Standadr qeruseri 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
21、 Ad nAnex era B na inetgral patr fo thnI sitenrtaoinaS ltandadr. C xennA tF xennA o are foi rnamroftiolno ny.EN ISO 9831:2003 ii Contents Page Foreword iii 1S c o p e 1 2 Normative references 1 3 Definitions 1 4 Principle 1 5 Reagents and materials 1 6 Apparatus 2 7 Sampling 4 8 Preparation of test
22、sample and test portion 4 9 Procedure 4 10 Corrections 6 11 Expression of results 8 12 Precision 8 13 Test report 9 Annex A (normative) Determination of the effective heat capacity of the calorimeter 10 Annex B (normative) Special procedures for preparation of the test sample 11 Annex C (informative
23、) Method of checking that the average deviation of the rate of change of temperature is within the specified limit 12 Annex D (informative) Examples of calculating the results of calorific determinations 13 Annex E (informative) Results of interlaboratory tests 17 Annex F (informative) Bibliography
24、18 Table 1 Repeatability limit (r) and reproducibility limit (R)9 Table C.1 Acceptable difference sequences 12 Table C.2 Example 13 Table D.1 Observed temperature readings 15 Table E.1 Statistical results of the interlaboratory tests 17EN ISO 9831:2003 BSI 12 March 2004 iii Foreword ISO (the Interna
25、tional 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 technical committee has be
26、en 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 of electrotechnical stan
27、dardization. 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 75 % of the member bodies casting a vote. International Standard ISO 9831 was prepared by Technical Co
28、mmittee 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 information only.blankEN ISO 9831:2003 BSI 12 March 2004 1 1 Scope This International Standard specifies a met
29、hod 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 at constant volume,
30、 the water of the combustion products being condensed to liquid at the calorimeter temperature. NOTE The international reference temperature for thermochemistry of 25 C is used as the reference temperature for calorific value, although the temperature dependence of the calorific value of the materia
31、ls to which this International Standard applies is small (about 1 J g p1 K p1 ). 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 indicated were vali
32、d. 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 International Sta
33、ndards. 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 calorific va
34、lue 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 Preparation
35、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 from the tem
36、perature 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 Reagents an
37、d 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 1 Oxygen manufactured by an electrolytic process may contain up
38、to 4 % of hydrogen and is therefore unsuitable. N O T E 2 1 M P a=1M N / m 2 . 1) To be published. (Revision of ISO 6496:1983) 2) To be published. (Revision of ISO 6498:1983)EN ISO 9831:2003 2 BSI 12 March 2004 5.3 Fuse, comprising the following. 5.3.1 Firing wire, nickel/chromium wire (0,16 mm to 0
39、,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 bags, of dimensions 68 mm by 110 mm. 5.5 Polyethylene bags, of dimensions 50 mm by 55 mm, and mass approxima
40、tely 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, =1g/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
41、 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 calorific value at constant volume of the benzoic acid, listed in the certificate for the conditions of use, s
42、hall 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 withstanding safely the pressure developed during combustion. The design shall permit complete recovery of all l
43、iquid 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 attention to the condition of the threads of the main closure. 6.2 Calorimeter vessel, made of metal, highly polished
44、 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 centre the bomb in the vessel and to obtain water circulation below the bomb. 6.3 Stirrer, driven at a const
45、ant 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 stati
46、c bomb calorimeters, the rate of stirring shall ensure that the length of the main period (see 9.6) in determinations of effective heat capacity using benzoic acid (see Annex A) does not exceed 10 min. 6.4 Water jacket, which may be an adiabatic, isothermal or static type, enclosing the calorimeter
47、vessel with an air-gap of approximately 10 mm separating the vessel and water jacket. The adiabatic water jacket shall have either electrode or immersion heaters capable of supplying energy at a rate sufficient to maintain the temperature of the water in the jacket to within 0,1 C of that of the cal
48、orimeter vessel after the charge has been fired. When in equilibrium at 25 C, the temperature drift of the calorimeter vessel shall not exceed 0,000 5 C/min. NOTE 1 Special precautions are needed at high environmental temperatures. The isothermal water jacket shall be provided with a means of maintaining it at a constant temperature to the nearest 0,1 C
