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    EN 14111-2003 en Fat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of iodine value《脂肪和油的衍生物 脂肪酸甲基酯(FAME) 碘值的测定》.pdf

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    EN 14111-2003 en Fat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of iodine value《脂肪和油的衍生物 脂肪酸甲基酯(FAME) 碘值的测定》.pdf

    1、BRITISH STANDARD BS EN 14111:2003 Fat and oil derivatives Fatty Acid Methyl Esters (FAME) Determination of iodine value The European Standard EN 14111:2003 has the status of a British Standard ICS 67.200.10 BS EN 14111:2003 This British Standard was published under the authority of the Standards Pol

    2、icy and Strategy Committee on 14 May 2003 BSI 14 May 2003 ISBN 0 580 41483 X National foreword This British Standard is the official English language version of EN 14111:2003. The UK participation in its preparation was entrusted to Technical Committee AW/307, Oilseeds animal and vegetable fats and

    3、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 international or European publications referred to in this document may be found in the BSI Catalogue under

    4、 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 provisions of a contract. Users are responsible for its correct appli

    5、cation. 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, or proposals for change, and keep the UK interests informed; mo

    6、nitor 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 title page, pages 2 to 9 and a back cover. The BSI copyright notice displayed in this document indicates when the document was la

    7、st issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN14111 April2003 ICS67.200.10 Englishversion FatandoilderivativesFattyAcidMethylEsters(FAME) Determinationofiodinevalue ProduitsdrivsdescorpsgrasEstersmthyliques dacidesgras(EMAG)Dter

    8、minationdelindicediode ErzeugnisseauspflanzlichenundtierischenFettenund lenFettsureMethylester(FAME)Bestimmungder lodzahl ThisEuropeanStandardwasapprovedbyCENon2January2003. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthest

    9、atusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation

    10、 undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norwa

    11、y,Portugal,Slovakia,Spain,Sweden,SwitzerlandandUn ited Kingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2003CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref

    12、.No.EN14111:2003EEN14111:2003(E) 2 Foreword Thisdocument(EN14111:2003)hasbeenpreparedbyTechnicalCommitteeCEN/TC307,“Oilseeds,vegetable andanimalfatsandoilsandtheirbyproductsMethodsofsamplingandanalysis“,thesecretariatofwhichisheld byAFNOR. This EuropeanStandard shallbegiventhestatusofanationalstanda

    13、rd,eitherbypublicationofanidenticaltextor byendorsement,atthelatestbyOctober2003,andconflictingnationalstandardsshallbewithdrawnatthelatest byOctober2003. ThisdocumenthasbeenpreparedunderMandateM/245onFattyAcidMethylester(FAME)giventoCENbythe EuropeanCommissionandtheEuropeanFreeTradeAssociation. Ann

    14、exAisinformative. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portu

    15、gal, Slovakia,Spain,Sweden,SwitzerlandandtheUnitedKingdom.EN14111:2003(E) 3 Introduction ThisEuropeanStandardisbasedontheENISO39611whichwasspecificallyadaptedforthedeterminationof iodinevalueoffattyacidmethylesters(FAME).EN14111:2003(E) 4 1Scope ThisEuropeanStandardspecifiesatitrimetricmethodforthed

    16、eterminationofiodinevalueinFattyAcidMethyl Esters,hereinafterreferredasFAME. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedorundatedreference,provisionsfromotherpublications.These normativereferencesarecitedattheappropriateplacesinthetext,andthepublicationsarelistedhereafter.For dated

    17、references,subsequentamendmentstoorrevisionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthelatesteditionofthe publicationreferredtoapplies(includingamendments). ENISO661:1995, AnimalandvegetablefatsandoilsPreparationoftestsamp

    18、le(ISO661:1989). ENISO3696, WaterforanalyticallaboratoryuseSpecificationandtestmethods(ISO3696:1987). 3 Termsanddefinitions ForthepurposesofthisEuropeanStandard,thefollowingtermanddefinitionapply. 3.1 iodinevalue massofhalogen,expressedasiodine,absorbedbythetestportionwhendeterminedinaccordancewitht

    19、he procedurespecifiedinthisEuropeanStandard,dividedbythemassofthetestportion Iodinevalueisreportedasgramsofiodineper100gofFAME. 4Principle AtestportionisdissolvedinamixedsolventandthenWijsreagentisadded.Afteraspecifiedtime,potassium iodideandwaterareaddedtothesampleandtheliberatediodineistitratedusi

    20、ngasodiumthiosulfate standardizedsolution. 5Reagents Useonlyreagentsofrecognisedanalyticalgradeandwaterofgrade3inaccordancewithENISO3696. 5.1 Potassiumiodide(KI) ,100g/laqueoussolutionfreefromiodateandiodine. 5.2 Starchsolution Mix5gofsolublestarchin30mlofwaterandaddto1000mlofboilingwater.Boilfor3mi

    21、nandletstandtocool. 5.3 Sodiumthiosulfate, standardvolumetricsolutioninwater, c(Na 2 S 2 O 3 5H 2 O)=0,1mol/lstandardizednot morethansevendaysbeforeuse. 5.4 Solvent, preparedbymixingequalvolumesofcyclohexaneandglacialaceticacid. 5.5 Wijsreagent ,containingiodinemonochlorideinaceticacid. TheI/Clratio

    22、ofWijsreagentshallbewithinthelimits1,10 0,1. NOTE CommerciallyavailableWijsreagentcanbeused.EN14111:2003(E) 5 6Apparatus Usuallaboratoryequipmentand,inparticular: 6.1 Glassweighingscoops ,suitableforthetestportionandforinsertingintotheflask(6.2). 6.2 Conicalflasks ,500mlcapacity,fittedwithgroundglas

    23、sstoppersandcompletelydried. 6.3 Analyticalbalance ,capableofweighingwithanaccuracyof 0,001gorless. 7Sampling SamplingisnotpartofthemethodspecifiedinthisEuropeanStandard.Arecommendedsamplingmethodisgiven inENISO55552. Itisimportantthatlaboratoryreceivesasamplewhichistrulyrepresentativeandhasnotbeend

    24、amagedor changedduringtransportationandstorage. 8 Preparationoftestsample PreparethetestsampleinaccordancewithENISO661.Thetestsampleshallnotbeheatedand/orfiltered. 9Procedure 9.1Testportion Takeapproximately0,13gto0,15gofthetestsample,weighedtothenearest0,001ginaglassweighingscoop (6.1). NOTE Inthec

    25、aseofaniodinevaluebelow100,themassofthetestportionshouldbeadjustedaccordingtoclause9of ENISO39611. 9.2Determination 9.2.1 Placetheglassweighingscoopcontainingthetestportionina500mlflask(6.2)anddissolveusing20ml ofsolvent(5.4).Add25mlofWijsreagentusingaprecisionpipette.Insertthestopper,swirlcarefully

    26、andplacethe flaskinthedark. CAUTIONDonotuseamouthpipettefortheWijsreagent. 9.2.2 Prepareablankwithsolventandreagentasin9.2.1butomittingthetestportion. 9.2.3 Leavetheflaskinthedarkfor1h. 9.2.4 Attheendofthereactiontimeadd20mlofpotassiumiodidesolution(5.1)and150mlofwater. Titratewithstandardsodiumthio

    27、sulfatesolution(5.3)untiltheyellowcolourduetoiodinehasalmostdisappeared. Addfewdropsofthestarchsolution(5.2)andcontinuethetitrationuntilthebluecolourjustdisappearsaftervery vigorousshaking.Potentiometricdeterminationofendpointisalsopermissible. 9.2.5 Carryoutablanktestusingtheblanksolution(9.2.2)con

    28、currently.EN14111:2003(E) 6 10 CalculationIodinevalue Theiodinevaluereportedingofiodine/100gofFAME,isgivenbythefollowingequation: () m V V c 2 1 69 , 12 - where c istheexactconcentration,inmolesperlitre,ofthestandardvolumetricsodiumthiosulfatesolutionused; V 1 isthevolume,inmillilitres,ofstandardvol

    29、umetricsodiumthiosulfatesolution(5.3)usedforblanktest; V 2 isthevolume,inmillilitres,ofstandardvolumetricsodiumthiosulfatesolution(5.3)usedforsample titration; m isthemass,ingrams,ofthetestportion. Resultsshallbeexpressedtothenearest1gofiodine/100g. 11Precision 11.1 Interlaboratorytest Detailsofinte

    30、rlaboratorytestsaregiveninannexA.Thevaluesderivedfromthesetestsmaynotbeapplicableto concentrationrangesandmatricesotherthanthosegiven. 11.2Repeatability Theabsolutedifferencebetweentwoindependentsingletestresults,obtainedusingthesamemethodonidentical testmaterialinthesamelaboratorybythesameoperatoru

    31、singthesameequipmentwithinashortintervaloftime, shallnotbegreaterthan3gofiodine( I 2 )/100gmorethanonceoutof20determinations. 11.3Reproducibility Theabsolutedifferencebetweentwosingletestresults,obtainedusingthesamemethodonidenticaltestmaterial indifferentlaboratorieswithdifferentoperatorsusingdiffe

    32、rentequipment,shallnotbegreaterthan5gofiodine (I 2 )/100gmorethanonceoutof20determinations.EN14111:2003(E) 7 12 Testreport Thetestreportshallspecify: allinformationnecessaryforthecompleteidentificationofthesample; thesamplingmethodusedifknown; thetestmethodused,withreferencetothisEuropeanstandard; a

    33、lloperatingdetailsnotspecifiedinthisEuropeanStandard,orregardedasoptional,togetherwithdetailsof anyincidentswhichmayhaveinfluencedthetestresult(s); thetestresult(s)obtained,oriftherepeatabilityhasbeenchecked,thefinalquotedresultobtained.EN14111:2003(E) 8 Annex A (informative) Resultsofaninterlaborat

    34、orytrial AEuropeancollaborativetestinvolving11laboratoriesin5countrieswascarriedouton5samples: Sample1: FAMEpreparedfromsunflowerandrapeseedoils(75%sunflower); Sample2: FAMEpreparedfromrapeseedoil; Sample3: FAMEpreparedfromsunflowerandrapeseedoils(25%sunflower); Sample4: FAMEpreparedfromrapeseedoil;

    35、 Sample5: FAMEpreparedfromsunfloweroil. ThetestwasorganizedbyCENTC307/WG1in1998andtheresultsobtainedweresubjectedtostatistical analysisinaccordancewithENISO42593togivetheprecisiondatashowninTableA.1. TableA.1 S a m p l e 12345 Nofparticipatinglaboratories 11 11 11 11 11 Nofparticipatinglaboratoriesa

    36、ftereliminatingoutliers 11 11 11 10 11 Meanvalue (g I 2 /100g) 123,9 112,1 116,7 111,8 128,4 Repeatabilitystandarddeviation(g I 2 /100g) 0,7 0,9 0,7 1,0 1,0 Reproducibilitystandarddeviation(g I 2 /100g) 2,0 2,6 1,6 1,7 1,8 Repeatabilitylimit, r(g I 2 /100g) 2,2 2,8 2,3 3,1 3,2 Reproducibilitylimit,

    37、R(g I 2 /100g) 6,3 8,2 4,9 5,3 5,5EN14111:2003(E) 9 Bibliography 1 ENISO3961, AnimalandvegetablefatsandoilsDeterminationofiodinevalue(ISO3961:1996). 2 ENISO5555, AnimalandvegetablefatsandoilsSampling(ISO5555:2001). 3 ENISO4259, PetroleumproductsDeterminationanapplicationofprecisiondatainrelationtome

    38、thodsof test(ISO4259:1992/Cor1:1993) .BS EN 14111:2003 BSI 389 Chiswick High Road London W4 4AL BSI British Standards Institution BSI is the independent national body responsible for preparing British Standards. It presents the UK view on standards in Europe and at the international level. It is inc

    39、orporated by Royal Charter. Revisions British Standards are updated by amendment or revision. Users of British Standards should make sure that they possess the latest amendments or editions. It is the constant aim of BSI to improve the quality of our products and services. We would be grateful if an

    40、yone finding an inaccuracy or ambiguity while using this British Standard would inform the Secretary of the technical committee responsible, the identity of which can be found on the inside front cover. Tel: +44 (0)20 8996 9000. Fax: +44 (0)20 8996 7400. BSI offers members an individual updating ser

    41、vice called PLUS which ensures that subscribers automatically receive the latest editions of standards. Buying standards Orders for all BSI, international and foreign standards publications should be addressed to Customer Services. Tel: +44 (0)20 8996 9001. Fax: +44 (0)20 8996 7001. Email: ordersbsi

    42、-. Standards are also available from the BSI website at http:/www.bsi-. In response to orders for international standards, it is BSI policy to supply the BSI implementation of those that have been published as British Standards, unless otherwise requested. Information on standards BSI provides a wid

    43、e range of information on national, European and international standards through its Library and its Technical Help to Exporters Service. Various BSI electronic information services are also available which give details on all its products and services. Contact the Information Centre. Tel: +44 (0)20

    44、 8996 7111. Fax: +44 (0)20 8996 7048. Email: infobsi-. Subscribing members of BSI are kept up to date with standards developments and receive substantial discounts on the purchase price of standards. For details of these and other benefits contact Membership Administration. Tel: +44 (0)20 8996 7002. Fax: +44 (0)20 8996 7001. Email: membershipbsi-. Information regarding online access to British Standar


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