欢迎来到麦多课文档分享! | 帮助中心 海量文档,免费浏览,给你所需,享你所想!
麦多课文档分享
全部分类
  • 标准规范>
  • 教学课件>
  • 考试资料>
  • 办公文档>
  • 学术论文>
  • 行业资料>
  • 易语言源码>
  • ImageVerifierCode 换一换
    首页 麦多课文档分享 > 资源分类 > PDF文档下载
    分享到微信 分享到微博 分享到QQ空间

    BS EN 14110-2003 Fat and oil derivatives - Fatty acid methyl esters (FAME) - Determination of methanol content《脂肪和油的衍生物 脂肪酸甲基酯(FAME) 测定甲醇含量》.pdf

    • 资源ID:572170       资源大小:219.18KB        全文页数:14页
    • 资源格式: PDF        下载积分:10000积分
    快捷下载 游客一键下载
    账号登录下载
    微信登录下载
    二维码
    微信扫一扫登录
    下载资源需要10000积分(如需开发票,请勿充值!)
    邮箱/手机:
    温馨提示:
    如需开发票,请勿充值!快捷下载时,用户名和密码都是您填写的邮箱或者手机号,方便查询和重复下载(系统自动生成)。
    如需开发票,请勿充值!如填写123,账号就是123,密码也是123。
    支付方式: 支付宝扫码支付    微信扫码支付   
    验证码:   换一换

    加入VIP,交流精品资源
     
    账号:
    密码:
    验证码:   换一换
      忘记密码?
        
    友情提示
    2、PDF文件下载后,可能会被浏览器默认打开,此种情况可以点击浏览器菜单,保存网页到桌面,就可以正常下载了。
    3、本站不支持迅雷下载,请使用电脑自带的IE浏览器,或者360浏览器、谷歌浏览器下载即可。
    4、本站资源下载后的文档和图纸-无水印,预览文档经过压缩,下载后原文更清晰。
    5、试题试卷类文档,如果标题没有明确说明有答案则都视为没有答案,请知晓。

    BS EN 14110-2003 Fat and oil derivatives - Fatty acid methyl esters (FAME) - Determination of methanol content《脂肪和油的衍生物 脂肪酸甲基酯(FAME) 测定甲醇含量》.pdf

    1、BRITISH STANDARD BS EN 14110:2003 Fat and oil derivatives Fatty Acid Methyl Esters (FAME) Determination of methanol content The European Standard EN 14110:2003 has the status of a British Standard ICS 67.200.10 BS EN 14110:2003 This British Standard was published under the authority of the Standards

    2、 Policy and Strategy Committee on 15 May 2003 BSI 15 May 2003 ISBN 0 580 41842 1 National foreword This British Standard is the official English language version of EN 14110:2003. The UK participation in its preparation was entrusted to Technical Committee AW/307, Oilseed animal present to the respo

    3、nsible international/European committee 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 cov

    4、er, the EN title page, pages 2 to 10, an inside back cover 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 NORMEEUROPENNE EUROPISCHENORM EN14110 April2003 ICS

    5、67.200.10 Englishversion FatandoilderivativesFattyAcidMethylEsters(FAME) Determinationofmethanolcontent ProduitsdrivsdescorpsgrasEstersmthyliques dacidesgras(EMAG)Dterminationdelateneuren mthanol ErzeugnisseauspflanzlichenundtierischenFettenund lenFettsureMethylester(FAME)Bestimmungdes Methanolgehal

    6、tes ThisEuropeanStandardwasapprovedbyCENon2January2003. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standards

    7、maybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official ve

    8、rsions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Slovakia,Spain,Sweden,SwitzerlandandUn ited Kingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORM

    9、ALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2003CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN14110:2003EEN14110:2003(E) 2 Foreword Thisdocument(EN14110:2003)hasbeenpreparedbyTechnicalCommitteeCEN/TC307“Oil

    10、seeds,vegetable andanimalfatsandoilsandtheirbyproductsMethodsofsamplingandanalysis“,thesecretariatofwhichisheld byAFNOR. This EuropeanStandard shallbegiventhestatusofanationalstandard,eitherbypublicationofanidenticaltextor byendorsement,atthelatestbyOctober2003,andconflictingnationalstandardsshallbe

    11、withdrawnatthelatest byOctober2003. ThisdocumenthasbeenpreparedunderMandateM/245onFattyAcidMethylester(FAME)giventoCENbythe EuropeanCommissionandtheEuropeanFreeTradeAssociation,andsupportsessentialrequirementsofEU Directive(s). AnnexesAandBareinformative. AccordingtotheCEN/CENELECInternalRegulations

    12、,thenationalstandardsorganizationsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal, Slovakia,Spain,Sweden,SwitzerlandandtheUnitedKingdom.EN14

    13、110:2003(E) 3 1Scope ThisEuropeanStandardspecifiesamethodforthedeterminationofmethanolcontentinfattyacidmethylesters (FAME)foruseasdieselfuelanddomesticheatingfuel.Themethodisapplicableforaconcentrationrangefrom 0,01%( m/m)to0,5%( m/m)methanol.ThemethodisnotapplicabletomixturesofFAMEwhichcontainothe

    14、rlow boilingcomponents. 2Principle Thesampleisheatedat80Cinahermeticallysealedvialtoallowdesorptionofcontainedmethanolintothegas phase.Whenequilibriumisreached,adefinedpartofthegasphaseisinjectedintoagaschromatograph,where methanolisdetectedwithaflameionisationdetector.Normallymethanolistheonlypeaki

    15、nthechromatogram. Theamountofmethanoliscalculatedbyreferencetoanexternalcalibration.Methanolcanalsobedetermined afteradditionofaninternalstandardtothesamplebeforeheating,followedbycalculationwiththeuseofan internalcalibrationfactor. NOTE Ifonlymanualequipmentisavailablethenonlyinternalstandardcalibr

    16、ationshouldbeused. 3Reagents Useonlyreagentsofrecognizedanalyticalgrade,unlessotherwisespecified. 3.1 Methanol,ofknownpuritygreaterthan99,5%. 3.2 2propanol ,ofknownpurity,greaterthan99,5%(forprocedureA,internalcalibration). 3.3 ReferenceFAME ,withamethanolcontentlessthan0,001%( m/m). NOTE ReferenceF

    17、AMEcaneitherbeobtainedfromcommercialsourcesorbywashingbythreeorfivetimeswithdistilled waterinaseparatorfunnel.FAMEshouldbethendriedbyheatingat90Cunderstirringandreducedpressure. 3.4 Carriergas ,nitrogen,heliumorhydrogen,ofknowpuritygreaterthan99%. 4Apparatus 4.1 Septumvials ,20mlcapacity. 4.2 Inerts

    18、epta (e.g.TFEorViton 1) ) andmetalliccaps . 4.3 Syringe,10l,accurateto0,1l. 4.4 Gassyringe 500l,fittedwithavalve(formanualprocedure). 4.5 Crimpingpliers. 4.6 Pipettes,of1ml,2ml,5mlcapacity. 4.7 Volumetricflask ,capacity10mland25ml. 1) ThisinformationisgivenfortheconvenienceofusersofthisEuropeanStand

    19、ardanddoesnotconstituteanendorsement byCENoftheseproducts.Equivalentproductsmaybeusediftheycanbeshowntoleadtothesameresults.EN14110:2003(E) 4 4.8 Gaschromatograph ,equippedwithacapillarycolumn,suitableinjector(automaticheadspacesystemora split/splitlessinjector)andflameionisationdetector,integrator.

    20、 4.9 Capillarycolumn,thecolumnshalleluatemethanolasasymmetricalpeak.Stationaryphaseslike methylpolysiloxane(e.g.DB1 2) ,SE30 2) )orpolyethylenglycol(e.g.DBWAX 2) ,CARBOWAX 2) )canbeused successfullyandafilmthicknessofminimum0,5misrecommended. NOTE Theuseofapackedcolumnequippedbyoneoftheabovementione

    21、dstationaryphasesorofChromosorb101 2) is alsoallowed. 4.10 Automaticheadspaceequipment Theautomaticheadspaceequipmentusedshallhavearepeatabilityof1%orbetterconcerningexperimental conditionslikeequilibriumtemperature,heatingtimes,andheadspacesamplingvolume.Thiscanbechecked,if necessary,byrepeatedanal

    22、ysisofthesamesample. NOTE Automaticheadspaceequipmentisrecommendedbecauseapart,fromitsbetterrepeatability,itallowsfor automatedandfastanalysisusingexternalcalibration.Manualequipmentcanalsobeused,however,extremecareshouldbe exercisedwhengasvolumesaretakenmanuallyfromthevialsandwheninjectingthemintot

    23、hegaschromatograph. 4.11 Analyticalbalance witharesolutionof0,0001g. 4.12 Thermostaticallycontrolledbathoroven ,80C. 4.13 Thermostaticallycontrolledoven ,60C. 5Procedure 5.1Analytical conditions TheGCworkingconditionsshallbechosentakingintoaccountthecharacteristicsofthecolumnandthetypeof carriergast

    24、oreachthedesiredresolutionwhichisfixedatminimum1,5forthemethanoland2propanolpeaks. NOTE1 Thefollowingparametersaregivenasanexample: columnDB1(length=30m,internaldiameter=0,32mm,filmthickness=3m); splitinjector(flowrate:50ml/min); injectoranddetectortemperature : 150C; ovenandcolumntemperature : 50C;

    25、 carriergas(hydrogen)pressure : 40kPa; volume injected : 500 l. NOTE2 Thefollowingheadspacesamplingconditionsaregivenasanexample: equilibrium temperature : 80 C; equilibrium time : 45 min; samplingvolume : 500l. 2) ThisinformationisgivenfortheconvenienceofusersofthisEuropeanStandardanddoesnotconstit

    26、uteanendorsement byCENoftheseproducts.Equivalentproductsmaybeusediftheycanbeshowntoleadtothesameresults.EN14110:2003(E) 5 5.2Operation Thegaschromatographshallbesetupandoperatedaccordingtothemanufacturersinstructions. 6 Calibrationsolutions Threecalibrationsolutionswithapproximatelythefollowingmetha

    27、nolconcentrationsinFAME(3.3)shallbe preparedasdescribedbelow. NOTE Threecalibrationsolutionshaveprovensufficientindailypractiseforareliablecoverageoftheconcentrationrange giveninthescopeofthismethod.Forotherconcentrationranges,itisalsopossibletouseotherormorecalibrationsolutio ns. 6.1 Calibrationsol

    28、utionA (0,5%( m/m)methanolinFAME). Filla25mlvolumetricflaskwith25mlofFAME(3.3)andadd(112 0,1)mg(142l)methanolintotheliquid phaseusingasyringe(4.3),theadditionbeingmadeintotheliquidphase.Theexactmassesshallbedetermined byweightmeasurement.Itisnecessarytoensurethoroughmixingbyvigorousshaking. 6.2 Cali

    29、brationsolutionB (0,1%( m/m)methanolinFAME). Transfer5mlofcalibrationsolutionAintoa25mlanalyticalflaskandcarefullyfilltothemarkwithFAME(3.3). 6.3 CalibrationsolutionC (0,01%( m/m)methanolinFAME). Transfer1mlofcalibrationsolutionBintoa10mlanalyticalflaskandfilltothemarkwithFAME(3.3). 7Procedure Twoal

    30、ternativeprocedures,thefirstusinginternalcalibrationandthesecondusingexternalcalibrationare describedinclauses7.1and7.2,respectively. 7.1 ProcedureAUsinginternalcalibration Thisprocedureisgenerallypreferredwhenonlyasmallnumberofsamplesisanalyzedandwhenautomatichead spaceequipmentisnotavailable.Forma

    31、nualprocedure,seenoteinclause(4.10). 7.1.1 Internalcalibration (50,01)gfromeachcalibrationsolutionistransferredintoaheadspacevial(4.1)and5lof2propanol(3.2)is addedintotheliquidphaseusingasyringe(4.3),theadditionbeingmadeintotheliquidphase.Thevialsarethen immediatelycrimpedandshakenvigorouslytoensure

    32、mixing. Every10min,introduceintothermostaticallycontrolledbathoroven(4.12)avialofthecalibrationsolutionwhich shallbekeptthereforexactly45min. Preheatthegassyringe(4.4)to60Cinanoven(4.13).Sample500lofgaseousphase(headspace)abovethe solutiontobeanalysedandcarryoutthechromatographicanalysis. Thecalibra

    33、tionfactor Fiscalculatedforeachcalibrationsolutionaccordingtoequation(1),shallbeexpressed roundedtothenearest0,01. () ) ( m i i m S C S C F = (1) where C i isthe2propanolcontentinthecalibrationsolution,expressedin%( m/m);EN14110:2003(E) 6 (If5lof2propanolareintroducedinto5,0gcalibrationsolution,then

    34、 C i =0,0785%( m/m). C m isthemethanolcontentinthecalibrationsolution,expressedin%( m/m); S i isthepeakareaof2propanol; S m isthepeakareaofmethanol. Thecalibrationfactorvaluesobtainedforthethreereferencesolutionsshallexhibitacoefficientofvariationbelow 15%.Ifthisvalueisexceeded,theexperimentalsetups

    35、hallbeinspectedforerrorsandthecalibrationprocedure shallberepeatedstartingfromclause(6).Themeanofthesecalibrationfactorvalues(intheregionof0,7)isused forthecalculationdescribedinclause7.1.2. 7.1.2 AnalysisandCalculationusinginternalcalibration Thesamplesshallbepreparedandanalysedwithexactlythesameex

    36、perimentalconditionsusedinthecalibration runs(7.1.1).Themethanolcontent C m ofasample,expressedin%( m/m),iscalculatedaccordingtoequation(2) androundedtotwodecimalplaces: i i m m S C S F C = (2) where F isthecalibrationfactorobtainedaccordingtoclause7.1.1; S m isthepeakareaofmethanol; C i is2propanol

    37、contentaddedtothesample,expressedin%( m/m); (If5lof2propanolareintroducedinto5,0gsample,then C i =0,0785%( m/m). S i isthepeakareaof2propanol. 7.2 ProcedureBUsingexternalcalibration Thisprocedureisusuallypreferredwhenautomaticheadspaceequipmentisusedandalargenumberofsampled isanalysed.Itisnotrecomme

    38、ndedtouseexternalcalibrationwhentheanalysisisexecutedmanually,i.e.without automaticheadspaceequipment. 7.2.1 Externalcalibration 2mlfromeachcalibrationsolutionistransferredintoaheadspacevial.Thevialshallbecrimpedimmediately.The vialsarethenplacedintotheheadspacesamplerandtheanalysisisstartedaccordin

    39、gtothemanufacturers instructionmanual. Thecalibrationfunctioniscalculatedusinglinearregression,usingthemethanolcontentsasdependentvariable andthepeakareasasindependentvariable.Usingtheresultingslope, d,andyintercept, e,theregressionfunction isthenconvertedusingequation(3): m m S b a C + = (3) where

    40、C m isthemethanolcontentin%( m/m); a isthecoefficientobtainedfrom( e/d );EN14110:2003(E) 7 b isthecoefficientobtainedfrom(1/ d); S m istheareaofthemethanolpeak; d istheslopeofregressionline; e isyinterceptofregressionline. NOTE Ifthecorrelationcoefficientislessthan0,95,theprocedureshouldbeinspectedf

    41、orerrorsandthecalibration procedureshouldberepeatedstartingwithclause6. 7.2.2 Analysisandcalculationusingexternalcalibration Thesamplesshallbepreparedandanalysedwithexactlythesameexperimentalconditionsusedinthecalibration runs(7.2.1). Themethanolcontent C m ofasample,expressedin%( m/m),iscalculateda

    42、ccordingtoequation(3) androundedtothenearest0,01%( m/m). 8Precision TheprecisiondataforprocedureAandprocedureBhavebothbeenobtainedfromaEuropeaninterlaboratorytrial organisedin1999.Inthisroundrobinexercise,nosignificantdifferenceswereobservedbetweenprocedureAand procedureB(withautomaticheadspacesystemorwithmanualprocedure)forthemethanolconcentrationrange of0,01%to0,20%( m/m). 8.1Repeatability Theabsolutedifferencebetweentwoindependentsingletestresults,obtainedusingthesamemethodonidentical testma


    注意事项

    本文(BS EN 14110-2003 Fat and oil derivatives - Fatty acid methyl esters (FAME) - Determination of methanol content《脂肪和油的衍生物 脂肪酸甲基酯(FAME) 测定甲醇含量》.pdf)为本站会员(jobexamine331)主动上传,麦多课文档分享仅提供信息存储空间,仅对用户上传内容的表现方式做保护处理,对上载内容本身不做任何修改或编辑。 若此文所含内容侵犯了您的版权或隐私,请立即通知麦多课文档分享(点击联系客服),我们立即给予删除!




    关于我们 - 网站声明 - 网站地图 - 资源地图 - 友情链接 - 网站客服 - 联系我们

    copyright@ 2008-2019 麦多课文库(www.mydoc123.com)网站版权所有
    备案/许可证编号:苏ICP备17064731号-1 

    收起
    展开