欧盟生物柴油标准EN

EUROPEANSTANDARDNORMEEUROPÉENNEEUROPÄISCHENORMEN14214November2008ICS75.160.20SupersedesEN14214:2003EnglishVersionAutomotivefuels-Fattyacidmethylesters(FAME)fordieselengines-RequirementsandtestmethodsCarburantspourautomobiles-Estersméthyliquesd'acidesgras(EMAG)pourmoteursdiesel-Exigencesetméthodesd'essaisKraftstoffefürKraftfahrzeuge-Fettsäure-Methylester(FAME)fürDieselmotoren-AnforderungenundPrüfverfahrenThisEuropeanStandardwasapprovedbyCENon25October2008.CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEuropeanStandardthestatusofanationalstandardwithoutanyalteration.Up-to-datelistsandbibliographicalreferencesconcerningsuchnationalstandardsmaybeobtainedonapplicationtotheCENManagementCentreortoanyCENmember.ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).AversioninanyotherlanguagemadebytranslationundertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheCENManagementCentrehasthesamestatusastheofficialversions.CENmembersarethenationalstandardsbodiesofAustria,Belgium,Bulgaria,Cyprus,CzechRepublic,Denmark,Estonia,Finland,France,Germany,Greece,Hungary,Iceland,Ireland,Italy,Latvia,Lithuania,Luxembourg,Malta,Netherlands,Norway,Poland,Portugal,Romania,Slovakia,Slovenia,Spain,Sweden,SwitzerlandandUnitedKingdom.EUROPEANCOMMITTEEFORSTANDARDIZATIONCOMITÉEUROPÉENDENORMALISATIONEUROPÄISCHESKOMITEEFÜRNORMUNGManagementCentre:ruedeStassart,36B-1050Brussels©2008CENAllrightsofexploitationinanyformandbyanymeansreservedworldwideforCENnationalMembers.Ref.No.EN14214:2008:EEN14214:2008(E)2ContentsPageForeword.............................................................................................................................................................3Introduction........................................................................................................................................................41Scope......................................................................................................................................................52Normativereferences...........................................................................................................................53Sampling................................................................................................................................................64Pumpmarking.......................................................................................................................................75Requirementsandtestmethods.........................................................................................................75.1Dyesandmarkers.................................................................................................................................75.2Additives................................................................................................................................................75.3Stabilizingagents..................................................................................................................................75.4Generallyapplicablerequirementsandrelatedtestmethods.........................................................75.5Climatedependentrequirementsandrelatedtestmethods............................................................95.6Precisionanddispute...........................................................................................................................9AnnexA(normative)Detailsofinterlaboratorytestprogramme................................................................11AnnexB(normative)CalculationofIodineValue..........................................................................................12AnnexC(normative)CorrectionfactorforcalculationofdensityofFAME..............................................14Bibliography.....................................................................................................................................................15EN14214:2008(E)3ForewordThisdocument(EN14214:2008)hasbeenpreparedbyTechnicalCommitteeCEN/TC19“Gaseousandliquidfuels,lubricantsandrelatedproductsofpetroleum,syntheticandbiologicalorigin”,thesecretariatofwhichisheldbyNEN.ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationofanidenticaltextorbyendorsement,atthelatestbyMay2009,andconflictingnationalstandardsshallbewithdrawnatthelatestbyMay2009.Attentionisdrawntothepossibilitythatsomeoftheelementsofthisdocumentmaybethesubjectofpatentrights.CEN[and/orCENELEC]shallnotbeheldresponsibleforidentifyinganyorallsuchpatentrights.ThisdocumentsupersedesEN14214:2003.ThisEuropeanStandardexistsinparallelwithEN590.SignificanttechnicalchangesbetweenthisEuropeanStandardandthepreviouseditionare:suitablelimitsandtestmethodsontheesters,glyceridesandstabilitycharacteristicsofFAMEresultingfromEU-fundedresearchprogrammes‘BIOSTAB’and'BIOScopes'havebeenincorporated,althoughapossiblereplacementforiodinevalueisstillunderdiscussioninCEN/TC19;thephosphoruslimithasbeenloweredfrom10ppmto4ppm,asafirstreasonablesteptowardsmeetingtheneedsofthelatesttechnologyengines,beingameasurableamountandachievablewithnottoolargeinvestmentsbytheFAMEproducers;allowanceoftheautomaticPensky-Martenstestmethodasanalternativeforflashpointdeterminationandacorrespondingchangeofthelimitfrom120°Cto101°C;additionofaworkmanshipsubclause(5.4.5);inclusionofanotereferringtogoodhousekeepingviaCEN/TR15367-1;anotetoclarifythatcoldflowrequirementsoffattyacidmethylesters(FAME)whenusedasanextenderfordieselaccordingtoEN590(assetoutinTable2)donotapply;ageneralupdateoftherevisedtestmethods,someofthemalreadyhavingbeenincludedintheTechnicalCorrigendumtothepreviousversion.AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowingcountriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,Bulgaria,Cyprus,CzechRepublic,Denmark,Estonia,Finland,France,Germany,Greece,Hungary,Iceland,Ireland,Italy,Latvia,Lithuania,Luxembourg,Malta,Netherlands,Norway,Poland,Portugal,Romania,Slovakia,Slovenia,Spain,Sweden,SwitzerlandandtheUnitedKingdom.EN14214:2008(E)4IntroductionThisEuropeanStandardgivesallrelevantcharacteristics,requirementsandtestmethodsforfattyacidmethylesters(FAME),whichareknownatthistimetobenecessarytodefinetheproducttobeusedasautomotivedieselfuel.ManyofthetestmethodsincludedinthisEuropeanStandardwerethesubjectofinterlaboratorytestingtodeterminetheirapplicabilityandtheirprecisioninrelationtodifferentsourcesofFAME.TheseFAMEwereproducedfromvegetableoilsavailableinthemarketatthattime,i.e.rapeseed,palm,soyandsunfloweroil.Concerningtotalcontamination,aninterlaboratorystudywithfieldsamples,followingastudywithartificialsamples,ispendingandthereforetherepeatabilityandreproducibilityofEN12662havenotyetbeenfullyestablished.TheprecisionforvolumepercentagelevelsofFAMEof7,10and100willbeinvestigated.EN14214:2008(E)51ScopeThisEuropeanStandardspecifiesrequirementsandtestmethodsformarketedanddeliveredfattyacidmethylesters(hereafterknownasFAME)tobeusedeitherasautomotivefuelfordieselenginesat100%concentration,orasanextenderforautomotivefuelfordieselenginesinaccordancewiththerequirementsofEN590.At100%concentrationitisapplicabletofuelforuseindieselenginevehiclesdesignedorsubsequentlyadaptedtorunon100%FAME.NOTEForthepurposesofthisEuropeanStandard,theterms“%(m/m)”and“%(V/V)”areusedtorepresentrespectivelythemassfractionandthevolumefraction.2NormativereferencesThefollowingreferenceddocumentsareindispensablefortheapplicationofthisdocument.Fordatedreferences,onlytheeditioncitedapplies.Forundatedreferences,thelatesteditionofthereferenceddocument(includinganyamendments)applies.EN116:1997,Dieselanddomesticheatingfuels—DeterminationofcoldfilterpluggingpointEN590,Automotivefuels—Diesel—RequirementsandtestmethodsEN12662:2008,Liquidpetroleumproducts—DeterminationofcontaminationinmiddledistillatesEN14103:2003,Fatandoilderivatives—FattyAcidMethylEsters(FAME)—DeterminationofesterandlinolenicacidmethylestercontentsEN14104:2003,Fatandoilderivatives—FattyAcidMethylEsters(FAME)—DeterminationofacidvalueEN14105:2003,Fatandoilderivatives—FattyAcidMethylEsters(FAME)—Determinationoffreeandtotalglycerolandmono-,di-andtriglyceridecontent(Referencemethod)EN14106:2003,Fatandoilderivatives—FattyAcidMethylEsters(FAME)—DeterminationoffreeglycerolcontentEN14107:2003,Fatandoilderivatives—FattyAcidMethylEsters(FAME)—Determinationofphosphoruscontentbyinductivelycoupledplasma(ICP)emissionspectrometryEN14108:2003,Fatandoilderivatives—FattyAcidMethylEsters(FAME)—DeterminationofsodiumcontentbyatomicabsorptionspectrometryEN14109:2003,Fatandoilderivatives—FattyAcidMethylEsters(FAME)—DeterminationofpotassiumcontentbyatomicabsorptionspectrometryEN14110:2003,Fatandoilderivatives—FattyAcidMethylEsters(FAME)—DeterminationofmethanolcontentEN14111:2003,Fatandoilderivatives—FattyAcidMethylEsters(FAME)—DeterminationofiodinevalueEN14112:2003,Fatandoilderivatives—FattyAcidMethylEsters(FAME)—Determinationofoxidationstability(acceleratedoxidationtest)EN14538:2006,Fatandoilderivatives—Fattyacidmethylesters(FAME)—DeterminationofCa,K,MgandNacontentbyopticalemissionspectralanalysiswithinductivelycoupledplasma(ICPOES)prEN15751:2008,Automotivefuels—Fattyacidmethylester(FAME)fuelandblendswithdieselfuel—DeterminationofoxidationstabilitybyacceleratedoxidationmethodEN14214:2008(E)6ENISO2160:1998,Petroleumproducts—Corrosivenesstocopper—Copperstriptest(ISO2160:1998)ENISO2719:2002,Determinationofflashpoint—Pensky-Martensclosedcupmethod(ISO2719:2002)ENISO3104:1996,Petroleumproducts—Transparentandopaqueliquids—Determinationofkinematicviscosityandcalculationofdynamicviscosity(ISO3104:1994)ENISO3170:2004,Petroleumliquids—Manualsampling(ISO3170:2004)ENISO3171:1999,Petroleumliquids—Automaticpipelinesampling(ISO3171:1988)ENISO3675:1998,Crudepetroleumandliquidpetroleumproducts—Laboratorydeterminationofdensityorrelativedensity—Hydrometermethod(ISO3675:1998)ENISO3679:2004,Determinationofflashpoint—Rapidequilibriumclosedcupmethod(ISO3679:2004)ENISO4259:2006,Petroleumproducts—Determinationandapplicationofprecisiondatainrelationtomethodsoftest(ISO4259:2006)ENISO5165:1998,Dieselfuels—Determinationofignitionqualityofdieselfuels—Cetaneenginemethod(ISO5165:1998)ENISO10370:1995,Petroleumproducts—Determinationofcarbonresidue(micromethod)(ISO10370:1993)ENISO12185:1996,Crudepetroleumandpetroleumproducts—Determinationofdensity—OscillatingU-tubemethod(ISO12185:1996)ENISO12937:2000,Petroleumproducts—Determinationofwater—CoulometricKarlFishertitrationmethod(ISO12937:2000)ENISO13759:1996,Petroleumproducts—Determinationofalkylnitrateindieselfuels—Spectrometricmethod(ISO13759:1996)ENISO20846:2004,Petroleumproducts—Determinationofsulfurcontentofautomotivefuels—Ultravioletfluorescencemethod(ISO20846:2004)ENISO20884:2004,Petroleumproducts—Determinationofsulfurcontentofautomotivefuels—Wavelength-dispersiveX-rayfluorescencespectroscopy(ISO20884:2004)ISO3987:1994,Petroleumproducts—Lubricatingoilsandadditives—DeterminationofsulfatedashASTMD1160-06,StandardTestMethodforDistillationofPetroleumProductsatReducedPressure3SamplingSamplesshallbetakenasdescribedinENISO3170orENISO3171and/orinaccordancewiththerequirementsofnationalstandardsorregulationsforthesamplingofautomotivedieselfuel.ThenationalrequirementsshallbesetoutinanationalannextothisEuropeanStandard,eitherindetailorbyreferenceonly.InviewofthesensitivityofsomeofthetestmethodsreferredtointhisEuropeanStandard,particularattentionshallbepaidtocompliancewithanyguidanceonsamplingcontainers,whichisincludedinthetestmethodstandard.EN14214:2008(E)74PumpmarkingInformationtobemarkedondispensingpumpsusedfordeliveringFAMEdieselfuel,andthedimensionsofthemarkshallbeinaccordancewiththerequirementsofnationalstandardsorregulationsforthemarkingofpumpsforautomotivedieselfuel.SuchrequirementsshallbesetoutindetailorshallbereferredtobyreferenceinanationalannextothisEuropeanStandard.5Requirementsandtestmethods5.1DyesandmarkersTheuseofdyesormarkersisallowed.5.2AdditivesInordertoimprovetheperformancequality,theuseofadditivesisallowed.Suitablefueladditiveswithoutknownharmfulsideeffectsarerecommendedintheappropriateamount,tohelptoavoiddeteriorationofdriveabilityandemissionscontroldurability.Othertechnicalmeanswithequivalenteffectmayalsobeused.NOTE1Depositformingtendencytestmethodssuitableforroutinecontrolpurposeshavenotyetbeenidentifiedanddeveloped.NOTE2ForfurtherinformationonpreventingcontaminationbywaterorsedimentthatmayoccurinthesupplychainitisadvisabletocheckCEN/TR15367-1[1].5.3StabilizingagentsInordertoimprovethelongtermstabilityofFAME,itisrecommendedthatstabilizingagentsshouldbeaddedtotheproductimmediatelyafteritsproduction,atleastbeforeitseventualblendingintoamixturewithpetroleumbaseddieselfuel.5.4Generallyapplicablerequirementsandrelatedtestmethods5.4.1WhentestedbythemethodsindicatedinTable1,FAMEshallbeinaccordancewiththelimitsspecifiedinTable1.ThetestmethodslistedinTable1havebeenshowntobeapplicabletoFAMEinaninterlaboratorytestprogramme.PrecisiondatafromthisprogrammearegiveninnormativeAnnexA,wherethesewerefoundtobedifferentfromtheprecisiondatagiveninthetestmethodsforpetroleumproducts.5.4.2IncaseofaneedforidentificationofFAME,arecommendedmethodbasedonseparationandcharacterisationofFAMEbyLC/GCisEN14331[2].5.4.3IncaseofaneedforacheckuponFAMEquality,iodinevalueofFAMEmaybecalculatedbythemethodpresentedinAnnexB,butthismethoddoesnotconstituteanalternativetotheiodinevaluerequirementofTable1.SeealsotheForewordandIntroduction.5.4.4ThelimitingvalueforthecarbonresiduegiveninTable1isbasedonproductpriortoadditionofignitionimprover,ifused.Ifavalueexceedingthelimitisobtainedonfinishedfuelinthemarket,ENISO13759shallbeusedasanindicatorofthepresenceofanitrate-containingcompound.Ifanignitionimproveristhusprovedpresent,thelimitvalueforthecarbonresidueoftheproductundertestcannotbeapplied.Theuseofadditivesdoesnotexemptthemanufacturerfrommeetingtherequirementofmaximum0,30%(m/m)ofcarbonresiduepriortoadditionofadditives.5.4.5FAMEfuelshallbefreefromanyadulterantorcontaminantthatmayrenderthefuelunacceptableforuseindieselenginevehicles.EN14214:2008(E)8Table1—GenerallyapplicablerequirementsandtestmethodsPropertyUnitLimitsTestmethodaminimummaximum(SeeClause2)FAMEcontenta%(m/m)96,5b–EN14103Densityat15°Cckg/m3860900ENISO3675ENISO12185Viscosityat40°Cdmm2/s3,505,00ENISO3104Flashpoint°C101–ENISO2719eENISO3679fSulfurcontentmg/kg–10,0ENISO20846ENISO20884Carbonresidue(on10%distillationresidue)g%(m/m)–0,30ENISO10370Cetanenumberh–51,0–ENISO5165Sulfatedashcontent%(m/m)–0,02ISO3987Watercontentmg/kg–500ENISO12937Totalcontaminationmg/kg–24EN12662Copperstripcorrosion(3hat50°C)ratingclass1ENISO2160Oxidationstability,110°Chours6,0–prEN15751iEN14112AcidvaluemgKOH/g–0,50EN14104Iodinevaluegiodine/100g–120EN14111Linolenicacidmethylester%(m/m)–12,0EN14103Polyunsaturated(≥4doublebonds)methylesters%(m/m)–1kMethanolcontent%(m/m)–0,20EN14110Monoglyceridecontent%(m/m)–0,80EN14105Diglyceridecontent%(m/m)–0,20EN14105Triglyceridecontenta%(m/m)–0,20EN14105Freeglycerol%(m/m)–0,02EN14105iEN14106Totalglycerol%(m/m)–0,25EN14105GroupImetals(Na+K)GroupIImetals(Ca+Mg)mg/kgmg/kg–5,05,0EN14108lEN14109EN14538EN14538Phosphoruscontentmg/kg–4,0EN14107aSee5.6.1.bTheadditionofnon-FAMEcomponentsotherthanadditivesisnotallowed,see5.2.WhenC17-methylestersnaturallyappearinFAMEthiscanresultinalowermeasuredfattyacidmethylestercontent.Inthissituationreferenceshouldbemadeforverificationtoamodifieddeterminationprocedure[4],untilamodifiedmethodisestablishedwithinCEN.cDensitymaybemeasuredbyENISO3675overarangeoftemperaturesfrom20°Cto60°C.TemperaturecorrectionshallbemadeaccordingtotheformulagiveninAnnexC.Seealso5.6.2.dIfCFPPis-20°Corlower,theviscosityshallbemeasuredat-20°C.Themeasuredvalueshallnotexceed48mm2/s.Inthiscase,ENISO3104isapplicablewithouttheprecisiondataowingtonon-Newtonianbehaviourinatwo-phasesystem.eProcedureAtobeapplied.Onlyaflashpointtestapparatusequippedwithasuitabledetectiondevice(thermalorionizationdetection)shallbeused.Seealso5.6.2.fA2mlsampleandapparatusequippedwithathermaldetectiondeviceshallbeused.gASTMD1160shallbeusedtoobtainthe10%distillationresidue.Seealso5.3.4.hSee5.6.3.iSee5.6.2.kAsuitabletestmethodisunderdevelopmentbyCEN[3].lSee5.6.2.SeeAnnexAforprecisiondataforsumofNa+K.EN14214:2008(E)95.5Climatedependentrequirementsandrelatedtestmethods5.5.1Forclimate-dependentrequirementsoptionsaregiventoallowforseasonalgradestobesetnationally.TheoptionsarefortemperateclimatessixCFPP(coldfilterpluggingpoint)gradesandforarcticclimatesfivedifferentclasses.Climate-dependentrequirementsaregiveninTable2.Table2isdividedintotwosections,onefortemperateclimates(Table2a)andoneforarcticclimates(Table2b).WhentestedbythemethodsgivenintheTables2aand2b,FAME"asfuelfordieselengines"shallbeinaccordancewiththelimitsspecifiedinthesetables.5.5.2Theclimate-dependentrequirementsinTable2donotapplyforFAMEbeingusedasablendcomponentinEN590dieselfuel.NOTEArequirementforFAMEtomeettheclimate-dependentrequirementscouldresultinincompatibilitybetweenthecoldflowadditivesusedintheFAMEandthedieselfuel.Thismaycompromisetheperformanceofthefinisheddiesel/FAMEblendinrespectofitslowtemperatureoperabilityandcausefieldfailuresasresultoffilterpluggingincoldweather.ColdflowadditivesshouldbespecificallymatchedtothebasedieselfuelandFAMEqualitytoensurecorrectperformanceconsistentwiththerequirementssetoutinEN590.Thechoiceofcoldflowadditivetechnologyshouldbeacontractualmatterbetweenthefuelblenderandthebiodieselsuppliertakingintoaccounttheclimatic-dependentrequirementsofthefinisheddieselfuel.5.5.3InanationalannextothisEuropeanStandardeachcountryshalldetailrequirementsforasummerandawintergradeandmayinclude(an)intermediateand/orregionalgrade(s)whichshallbejustifiedbynationalmeteorologicaldata.Table2—Climate-relatedrequirementsandtestmethodsTable2a—TemperateclimatesLimitsPropertyUnitGradeAGradeBGradeCGradeDGradeEGradeFTestmethodaCFPP°C,max.+50-5-10-15-20EN116aSeealso5.6.1.Table2b—ArcticclimatesLimitsPropertyUnitsclass0class1class2class3class4TestmethodaCFPP°C,max.-20-26-32-38-44EN116aSeealso5.6.1.5.6Precisionanddispute5.6.1AlltestmethodsreferredtointhisEuropeanStandardincludeaprecisionstatementaccordingtoENISO4259.Incasesofdispute,theproceduresdescribedinENISO4259shallbeusedforresolvingthedispute,andinterpretationoftheresultsbasedonthetestmethodprecisionshallbeused.However,themethodscurrentlyavailableforFAMEcontentandtriglyceridecontent,donotmeetthe2RrequirementofENISO4259atthelimitinTable1.AtthemomentrevisedmethodsareunderdevelopmentinajointeffortbyCEN/TC19andCEN/TC307.EN14214:2008(E)105.6.2Incasesofdisputeconcerningdensity,ENISO3675shallbeusedwiththedeterminationcarriedoutat15°C.Incasesofdisputeconcerningflashpoint,ENISO3679shallbeused.Incasesofdisputeconcerningoxidationstability,prEN15751shallbeused.Incasesofdisputeconcerningfreeglycerol,EN14105shallbeused.Incasesofdisputeconcerningmetalcontent,EN14538shallbeused,asEN14108andEN14109donotmeetthe2RrequirementsofENISO4259atthelimitinTable1.5.6.3Forthedeterminationofcetanenumberalternativemethodsmayalsobeusedincasesofdispute,providedthatthesemethodsoriginatefromarecognizedmethodseries,andhaveavalidprecisionstatement,derivedinaccordancewithENISO4259,whichdemonstratesprecisionatleastequaltothatofthereferencedmethod.Thetestresult,whenusinganalternativemethod,shallalsohaveademonstrablerelationshiptotheresultobtainedwhenusingthereferencemet