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    BS EN 14106-2003 Fat and oil derivatives Fatty acid methyl esters (FAME) Determination of free glycerol content《脂肪和油的衍生物 脂肪酸甲基酯(FAME) 游离甘油含量的测定》.pdf

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    BS EN 14106-2003 Fat and oil derivatives Fatty acid methyl esters (FAME) Determination of free glycerol content《脂肪和油的衍生物 脂肪酸甲基酯(FAME) 游离甘油含量的测定》.pdf

    1、BRITISH STANDARD BS EN 14106:2003 Fat and oil derivatives Fatty Acid Methyl Esters (FAME) Determination of free glycerol content The European Standard EN 14106:2003 has the status of a British Standard ICS 67.200.10 BS EN 14106:2003 This British Standard was published under the authority of the Stan

    2、dards Policy and Strategy Committee on 14 May 2003 BSI 14 May 2003 ISBN 0 580 41839 1 National foreword This British Standard is the official English language version of EN 14106:2003. The UK participation in its preparation was entrusted to Technical Committee AW/307, Oil seeds animal and vegetable

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

    4、ogue 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 provisions of a contract. Users are responsible for its cor

    5、rect 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, or proposals for change, and keep the UK interests in

    6、formed; 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 title page, pages 2 to 10, an inside back cover and a back cover. The BSI copyright notice displayed in this document i

    7、ndicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN14106 April2003 ICS67.200.10 Englishversion FatandoilderivativesFattyAcidMethylEsters(FAME) Determinationoffreeglycerolcontent Produitsdrivsdescorpsg

    8、rasEstersmthyliques dacidesgras(EMAG)Dterminationdelateneuren glycrollibre ErzeugnisseauspflanzlichenundtierischenFettenund lenFettsureMethylester(FAME)Bestimmungdes GehaltesanfreiemGlycerin ThisEuropeanStandardwasapprovedbyCENon2January2003. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegul

    9、ationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversion

    10、s(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Gre

    11、ece, Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Slovakia,Spain,Sweden,SwitzerlandandUn ited Kingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2003CEN Allrightsofexploitat

    12、ioninanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN14106:2003EEN14106:2003(E) 2 Foreword Thisdocument(EN14106:2003)hasbeenpreparedbyTechnicalCommitteeCEN/TC307“Oilseeds,vegetable andanimalfatsandoilsandtheirbyproductsMethodsofsamplingandanalysis“,thesecretariatofwhichisheld b

    13、yAFNOR. This EuropeanStandard shallbegiventhestatusofanationalstandard,eitherbypublicationofanidenticaltext orbyendorsement,atthelatestbyOctober2003andconflictingnationalstandardsshallbewithdrawnatthelatest byOctober2003. ThisdocumenthasbeenpreparedunderMandateM/245onFattyAcidMethylester(FAME)givent

    14、oCENbythe EuropeanCommissionandtheEuropeanFreeTradeAssociation. AnnexAisinformative. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Hung

    15、ary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal, Slovakia,Spain,Sweden,SwitzerlandandtheUnitedKingdom.EN14106:2003(E) 3 1Scope ThisEuropeanStandardspecifiesagaschromatographicmethodforthedeterminationoffreeglycerolcontentin FattyAcidMethylEsters(FAME)intherangeof0,005%to0,070%

    16、,hereinafterreferredasFAME. ThismethodaimstoevaluatetheFAMEquality,intermsoftransesterificationbyproductscontentsuchas glycerol,whoseconcentrationmayaffectthefuelbehaviour. WARNINGTheuseofthismethodmayinvolvehazardousequipment,materialsandoperations.This methoddoesnotpurporttoaddresstoallofthesafety

    17、problemsassociatedwithitsuse,butitisthe responsibilityoftheusertosearchandestablishappropriatesafetyandhealthpracticesanddetermine theapplicabilityofregulatorylimitationspriortouse. NOTE Inthecontextofthismethod( m/m)and( v/v)canbeused. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedor

    18、undatedreference,provisionsfromotherpublications.These normativereferencesarecitedattheappropriateplacesinthetext,andthepublicationsarelistedhereafter.For datedreferences,subsequentamendmentstoorrevisionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevisio

    19、n.Forundatedreferencesthelatesteditionofthe publicationreferredtoapplies(includingamendments). ENISO661, AnimalandvegetablefatsandoilsPreparationoftestsample(ISO661:1989). 3 Termsanddefinitions ForthepurposesofthisEuropeanStandard,thefollowingtermanddefinitionapply. 3.1 freeglycerolcontent istheresi

    20、dualglycerolremaininginFAMEafterthevegetableoiltransesterificationreactionandtheseparationof soobtainedglycerol 4 Principleofmethod Ethylalcohol,waterandhexaneandaknownamountofinternalstandardareaddedtoaknownquantityof sample.Theadditionofthesesolventscausestheformationoftwophasesandfreeglycerolisqu

    21、antitatively transferredintothelowerone. Thegaschromatographicanalysisoflowerphaseallowstoquantifytheconcentrationoffreeglycerol. 5Reagents Useonlyreagentsofrecognizedanalyticalgrade,unlessotherwisespecified. 5.1 Hexane. 5.2 1,4Butanediol, 99%minimum. 5.3 Ethylalcohol ,95%minimum. 5.4 Formicacid, 99

    22、%minimum. 5.5 Glycerol,99%minimum.EN14106:2003(E) 4 5.6 Carriergas :helium,GLCgrade. 5.7 Auxiliarygases : hydrogen,purity99%minimum,freefrommoistureandorganiccompounds; air,freefromorganiccompounds. 5.8 InternalStandardSolution:weighapproximately80mg(accuracy 0,0001g)of1,4Butanediolina volumetricfla

    23、sk,100mlcapacity.Dissolveinsomemlofdistilledwater,add1mlofformicacidandfilluptothe markusingdistilledwater.Thesopreparedsolutionisstablefor24hifstoredatambienttemperature. 6Apparatus 6.1 Gaschromatograph equippedbythefollowingdevices: 6.1.1 Thermostaticovenforcolumn,abletomaintainthesettemperaturewi

    24、thanaccuracyof 1C. 6.1.2 Thermostaticinjectionport,equippedforcapillarycolumninsplitsplitlessmodeor,alternatively,forpacked column. 6.1.3 Flameionisationdetector(FID)andconverter/amplifierdevice. 6.1.4 Recorder/integrator,capabletorunwiththeconverter/amplifierwitharesponsetimeof1smaximumand variable

    25、chartspeed. 6.1.5 Capillarycolumn,typePoraPLOTQ,length=10m,diameter0,32mm,filmthickness=10m(Note)or, alternativelypackedcolumnfilledwithCHROMOSORB101,diameter4mm,length=1m. NOTE Someproblemsanddiscrepanciesoncapillarycolumnbehaviourfromdifferentsuppliershavebeennoticed.Some Authorsreferalsothepossib

    26、ilitytousecapillarycolumnscoatedwithFFAP(FreeFattyAcidPhase)orpolyethyleneglycol phasesinsteadofthesuggestedstationaryphase.Neverthelessthechoiceofcolumnshouldbebasedonthefollowingcriteria: theseparationbetweenglycerolandinternalstandardpeaksshouldbecomplete(baselinenearlytozerobetweentwo peaks); th

    27、eanalysistimeshouldnotexceed15min; columnswithresponsefactorforglycerol,calculatedsuchas9.3,higherthan2,5arenotsuitable. 6.1.6 Flowcontrollers,forcarrierandauxiliarygases. 6.2 Microsyringe forgaschromatography ,5lor10l. 6.3 Volumetricflasks ,50mland100mlcapacity. 6.4 Twomarkprecisionpipettes ,1mlcap

    28、acity. 6.5 Volumetricpipettes ,5mlcapacity. 6.6 Analyticalbalance ,accuracy 0,0001g. 6.7 Glassconicaltesttubes ,10mlcapacity. 6.8 Centrifugalmachine ,abletorunatthespeedof2000revolutionsperminute.EN14106:2003(E) 5 7Sampling SamplingisnotpartofthemethodspecifiedinthisEuropeanStandard.Arecommendedsamp

    29、lingmethodisgiven inENISO55551. SamplingproceduresshalltakeintoaccountthatfreeglycerolcontainedinFAMEhasastrongaffinityforglass. Thereforesamplesshallbecollectedandstoredavoidingtheuseofglass. 8 Preparationoftestsample PreparethetestsampleinaccordancewithENISO661.Thetestsampleshallnotbeheatedand/orf

    30、iltered. 9Procedure 9.1 Gaschromatographicconditions Thefollowinggeneraloperatingconditionshavebeenshowntobesatisfactory. Oventemperature:210C; injectortemperature:230C; detectortemperature:250C; splitratio:approximately50:1; carriergasflow:1ml/minto2ml/min. Conditionsforpackedcolumn: oventemperatur

    31、e:200C; injectortemperature:230C; detectortemperature:250C; carriergasflow:20ml/minto30ml/min. 9.2Peaksidentification Theidentificationofpeaksbelongingtointernalstandardandglycerolcanbeachievedbyretentiontime comparisonofsuitablestandardsanalysedunderthesameanalyticalconditions.Anillustrativechromat

    32、ogramis reportedbelow.EN14106:2003(E) 6 GLCAnalysis Key 1 1,4Butanediol 2G l y c e r o l Figure1ChromatogramofasyntheticsolutionusedforresponsefactordeterminationDetermination offreeglycerolcontent 9.3 Determinationofresponsefactor Weighapproximately100mg 0,1mgofglyceroland100mg 0,1mgof1,4butanediol

    33、ina100mlvolumetric flask.Dissolvein50mlofethylalcohol(5.3)andfilluptothemarkwithwater.Considertheheatingandthevolume diminutionduetothewater/alcoholmixing.Injectatleastthreetimesinthechromatograph1 m lofthissolution usingtheexperimentalconditionslistedabove,inordertocalculatetheresponsefactor.Thesol

    34、utionisstablefor someweeksevenifstoredatroomtemperature.Usingtheobtainedchromatogramstheresponsefactor F r canbe calculatedasfollows: 2 2 1 1 / / ) ( factor Response M A M A F r = (1)EN14106:2003(E) 7 where A 1 isthepeakareaofinternalstandard; A 2 isthepeakareaofglycerol; M 1 isthemassof1,4butanedio

    35、linresponsefactorsolution,expressedinmg; M 2 isthemassofglycerolinresponsefactorsolution,expressedinmg. Theresponsefactor F r ,suchascalculatedaboveshallbe2,5orlower(seenotein6.1.5). 9.4 Quantitativeanalysis 9.4.1 Samplepreparation Weighapproximately3,5g 0,0001gofsample(correspondingtoabout4ml)intoa

    36、10mltesttube.Add1mlof ethylalcohol(5.3)andgentlyshaketoensuremixing.Addexactly1mlofinternalstandardsolution(5.8)and4ml ofhexane.Tightlyplugandshakevigorouslythetubeforfiveminutes.Centrifugethesamplefor15min.Usethe lowerphaseforgaschromatographicanalysis. 9.4.2 Gaschromatographyanalysis Takeapproxima

    37、tely1 m lofthelowerphaseusingtheGCmicrosyringeanddrawenoughairtoemptytheneedle (“hotneedle“technique).Carefullycleanbodyandneedleofsyringeusingapapertowel.Introducetheneedle throughthemembraneofinjectionport,waitfor5s,thenrapidlyinjectthesample.After5sdrawofftheneedle. Takenoteofinjectionmomentonchr

    38、omatogram.Continueelutionsomeminutesafterthecompletedetectionof glycerolpeak. 10Results Calculate,bymeansofintegrator,theareasofpeaksbelongingtotheunknownsample.Thepercentcontentof freeglycerolinsampleisgivenbythefollowingformula: 100 ) / ( (m/m) % glycerol, Free 1 1 2 = m m F A A r where A 1 , A 2

    39、, F r havethesamemeaningasinformula(1); m 1 isthemassofinternalstandardinsample(milligrams); m isthemassofsample(milligrams). Theresultshallbeexpressedasamassfractioninpercent,roundedtotwodigits 11Precision 11.1 Interlaboratorytest DetailsofinterlaboratorytestaregiveninannexA.Thevaluesderivedfromthe

    40、setestsmaynotbeapplicableto concentrationrangesandmatricesotherthanthosegiven.EN14106:2003(E) 8 11.2Repeatability Thedifferencebetweentworesultsobtainedbythesameoperator,withthesameapparatusunderconstant operatingconditionsonthesamesample,willbehigherthantherepeatabilitylimit( r)ascalculatedfromthe

    41、formulaeinfollowingtable,onlyinonecaseintwenty. 11.3Reproducibility Theabsolutedifferencebetweentwoindependentsingletestresults,obtainedbytwodifferentoperatorsworkingin differentlaboratoriesusingthesamemethodonidenticaltestmaterialwithinashortintervaloftimewillbehigher thanthereproducibilitylimit( R

    42、)ascalculatedfromtheformulaeinfollowingtable,onlyinonceoutof20 determinations. Table1Repeatabilityandreproducibilitylimits( rand R) FreeglycerolinFAME,in%( m/m) r=0,4664 X0,0012 R=0,7812 X+0,0032 X correspondingtofreeglycerolconcentrationvalue. 12 Testreport Thetestreportshallspecify: allinformation

    43、necessaryforthecompleteidentificationofthesample; thesamplingmethodusedifknown; thetestmethodused,withreferencetothisEuropeanstandard; alloperatingdetailsnotspecifiedinthisEuropeanStandard,orregardedasoptional,togetherwithdetailsof anyincidentswhichmayhaveinfluencedthetestresult(s); thetestresult(s)obtained,oriftherepeatabilityhasbeenchecked,thefinalquotedresultobtained.EN14106:2003(E) 9 Ann


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