BS EN ISO 9832-2003 Animal and vegetable fats and oils - Determination of residual technical hexane content《动植物脂肪和油 工业己烷残留量的测定》.pdf

1、BRITISH STANDARD BS EN ISO 9832:2003 Animal and vegetable fats and oils Determination of residual technical hexane content The European Standard EN ISO 9832:2003 has the status of a British Standard ICS 67.200.10 BS EN ISO 9832:2003 This British Standard was published under the authority of the Stan

2、dards Policy and Strategy Committee on 6 August 2003 BSI 6 August 2003 ISBN 0 580 42396 4 National foreword This British Standard is the official English language version of EN ISO 9832:2003. It is identical with ISO 9832:2002. It supersedes BS EN ISO 9832:2000 which is withdrawn. The UK participati

3、on in its preparation was entrusted to Technical Committee AW/307, Oil seeds, animal and vegetable fats and oils, 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

4、 international or European publications referred 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 no

5、t purport to include all the necessary provisions 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 co

6、mmittee 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 ISO title page, the E

7、N ISO foreword page, the ISO title page, pages ii and iii, a blank page, pages 1 to 10, the Annex ZA page and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORM

8、EEUROPENNE EUROPISCHENORM ENISO9832 July2003 ICS67.200.10 SupersedesENISO9832:2000 Englishversion AnimalandvegetablefatsandoilsDeterminationofresidual technicalhexanecontent(ISO9832:2002) CorpsgrasdoriginesanimaleetvgtaleDosagede lhexanetechniquersiduel(ISO9832:2002) TierischeundpflanzlicheFetteundl

9、eBestimmungdes GehaltesantechnischemResthexan(ISO9832:2002) ThisEuropeanStandardwasapprovedbyCENon10July2003. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibl

10、iographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotified

11、totheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Slovakia,Spain,Sweden,SwitzerlandandUn ited Kingdom.

12、EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2003CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.ENISO9832:2003EForeword ThetextofISO9832:2002hasbeenprepared

13、byTechnicalCommitteeISO/TC34“Agricultural foodproducts”oftheInternationalOrganizationforStandardization(ISO)andhasbeentaken overasENISO9832:2003byTechnicalCommitteeCEN/TC307“Oilseeds,vegetableand animalfatsandoilsandtheirbyproductsMethodsofsamplingandanalysis“,thesecretariatof whichisheldbyAFNOR. Th

14、isEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationof anidenticaltextorbyendorsement,atthelatestbyJanuary2004,andconflictingnational standardsshallbewithdrawnatthelatestbyJanuary2004. ThisdocumentsupersedesENISO9832:2000. AccordingtotheCEN/CENELECInternalRegulations,thenat

15、ionalstandardsorganizationsof thefollowingcountriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,Czech Republic,Denmark,Finland,France,Germany,Greece,Hungary,Iceland,Ireland,Italy, Luxembourg,Malta,Netherlands,Norway,Portugal,Slovakia,Spain,Sweden,Switzerlandand theUnitedKingdom. Endorseme

16、ntnotice ThetextofISO9832:2002hasbeenapprovedbyCENasENISO9832:2003withoutany modifications. NOTENormativereferencestoInternationalStandardsarelistedinannexZA(normative). ENISO9832:2003 Reference number ISO 9832:2002(E)INTERNATIONAL STANDARD ISO 9832 Second edition 2002-02-15 Animal and vegetable fat

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22、Web ww.wiso.ch Prnietdi nS wztierland ii ENISO9832:2003 iiiForeword 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 committ

23、ees. 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 Int

24、ernational Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3. The main task of technical committees is to prepare International Standards. Draft International

25、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. Attention is drawn to the possibility that some of the elements of this International Standar

26、d may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 9832 was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 11, Animal and vegetable fats and oils. This second edition cancels and replaces the first ed

27、ition (ISO 9832:1992), of which it constitutes a minor revision to incorporate Amendment 1:1998. Annex A of this International Standard is for information only. ENISO9832:2003INTENRATIONAL TSANDADR IS:2389 O2002(E)1Animal and vegetable fats and oils Determination of residual technical hexane content

28、 1 Scope This International Standard specifies a method for the determination of the residual technical hexane content of animal and vegetable fats and oils (referred to as fats hereinafter). The method is suitable for the determination of hexane contents between 10 mg and 1 500 mg per kilogram of f

29、at. The method is not applicable to marine oils 2 Normative reference The following normative document contains 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 public

30、ations do not apply. However, parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent edition of the normative document indicated below. For undated references, the latest edition of the normative document referred to appli

31、es. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 661:1989, Animal and vegetable fats and oils Preparation of test sample 3 Term and definition For the purposes of this International Standard, the following term and definition applies. 3.1 residual technic

32、al hexane content content of volatile hydrocarbons such as those remaining in fats following processing involving the use of hydrocarbon solvents, when determined by the method specified in this International Standard NOTE The content is expressed as milligrams of hexane per kilogram of sample. 4 Pr

33、inciple Desorption of volatile hydrocarbons by heating at 80 C in a closed vessel after addition of an internal standard. Determination of the particular volatile hydrocarbons content of the headspace by gas chromatography using packed or capillary columns. 5 Reagents Use only reagents of recognized

34、 analytical grade, unless otherwise stated, and distilled or demineralized water or water of equivalent purity. ENISO9832:20032 5.1 Technical hexane, with a composition similar to that of hexane used in industrial processing or, if this is not available, n-hexane. It is recommended that technical he

35、xane be used for the calibration. This reagent usually has an n-hexane content of 50 % (by mass) and consists mainly of C 6isomers but may include C 5and C 7hydrocarbons. 5.2 Internal standard, n-heptane. If this is not available, cyclohexane may be used, provided that the solvent (5.1) used for the

36、 extraction or calibration has a negligible content of cyclohexane and/or n-heptane or components with similar retention times. 5.3 Carrier gas, e.g. hydrogen, nitrogen or helium, etc., thoroughly dried and with an oxygen content of less than 10 mg/kg. 5.4 Auxiliary gases, hydrogen (99,9 % pure, fre

37、e from organic impurities) and air (free from organic impurities). 5.5 Calibration fat, freshly refined and deodorized vegetable fat, the technical hexane content of which is negligible. This material should be free from peroxides or other components likely to decompose with the formation of volatil

38、e material which could be confused with hydrocarbons during the test. 6 Apparatus Usual laboratory equipment and, in particular, the following. 6.1 Septum vials, of 20 ml capacity. 6.2 Septa, inert to fats and solvents, made of a material such as butyl rubber or red rubber free from hydrocarbon solv

39、ent residues and of a suitable quality that they will not swell under the conditions of use, aluminium caps suitable for use with the vials (6.1) and crimping pliers. 6.3 Tongs, suitable for holding the vials (6.1). 6.4 Syringes, of 10 l capacity, used only for the analysis of residual technical hex

40、ane. They shall not be cleaned with hydrocarbon solvent. 6.5 Syringes, of 1 l capacity, used only for the analysis of residual technical hexane. They shall not be cleaned with hydrocarbon solvent. 6.6 Syringes, of 1 000 l capacity, gas-tight, used only for the analysis of residual technical hexane.

41、They shall not be cleaned with hydrocarbon solvent. 6.7 Gas chromatograph, with a flame ionization detector and an integrator and/or recorder, equipped with either a) a packed glass column, 2 m to 4 m long and of internal diameter 3,2 mm approximately, packed with an acid- washed and silanized diato

42、maceous earth support of particle size 150 m to 180 m (Chromosorb P NAW 60-80 mesh 1)is suitable), and coated with 10 % squalane or any other phase permitting the chromatographic separation required, or b) a glass capillary column, approximately 30 m long and of 0,3 mm internal diameter, coated with

43、 methylpolysiloxane of film thickness 0,2 m. 1) Chromosorb P NAW 60-80 is an 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 by ISO of this product. ENISO9832:2003 3The

44、injector and detector temperature shall be set at 100 C and the oven temperature at 50 C. If a capillary column see b) is used, the apparatus shall have a 1/100 split injection system. NOTE For analyses in series, a headspace gas chromatograph with automatic sample injection and tempering bath has b

45、een shown to be satisfactory. In this case, manual injection is not necessary. 6.8 Heating bath, equipped with clamps for holding septum vials, regulated thermostatically at 80 C 2 C. NOTE For continuous operation, glycerol is recommended as the heating medium. 6.9 Shaking machine 7 Sampling It is i

46、mportant that the laboratory receive a sample which is truly representative and has not been damaged or changed during transport and storage. Sampling is not part of the method specified in this International Standard. A recommended sampling method is given in ISO 5555. It is essential that the samp

47、le be protected from gain or loss of solvent residues. 8 Preparation of test sample Prepare the test sample in accordance with ISO 661, taking care to prevent gain or loss of solvent. 9 Procedure 9.1 Calibration 9.1.1 Weigh, to the nearest 0,01 g, 5 g of calibration fat (5.5) into each of seven vial

48、s (6.1). Close each vial with a septum and a cap (6.2). To six of the seven vials (6.1) add, using a syringe (6.4 or 6.5), the quantity of solvent (5.1) specified in Table 1 to obtain the concentrations indicated. Do not add solvent to the seventh vial. Shake vigorously, in the shaking machine (6.9) for 1 h at room temperature, the six vials to which solvent w