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
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