1、BRITISH STANDARD BS EN 14107:2003 Fat and oil derivatives Fatty Acid Methyl Esters (FAME) Determination of phosphorous content by inductively coupled plasma (ICP) emission spectrometry The European Standard EN 14107:2003 has the status of a British Standard ICS 67.200.10 BS EN 14107:2003 This Britis
2、h Standard was published under the authority of the Standards Policy and Strategy Committee on 15 May 2003 BSI 15 May 2003 ISBN 0 580 41838 3 National foreword This British Standard is the official English language version of EN 14107:2003. The UK participation in its preparation was entrusted to Te
3、chnical Committee AW/307, Oilseeds animal and vegetable 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 ref
4、erred to in this document may be found in the BSI Catalogue 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 prov
5、isions of a contract. Users are responsible for its correct 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
6、, 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 cover, the EN title page, pages 2 to 9 and a back cover. The BSI copyright not
7、ice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN14107 April2003 ICS67.200.10 Englishversion FatandoilderivativesFattyAcidMethylEsters(FAME) Determinationofphosphorus
8、contentbyinductivelycoupled plasma(ICP)emissionspectrometry ProduitsdrivsdescorpsgrasEstersmthyliques dacidesgras(EMAG)Dterminationdelateneuren phosphoreparspectromtriedmissiondeplasmainduit parhautefrquence(mthodeICP) ErzeugnisseauspflanzlichenundtierischenFettenund lenFettsureMethylester(FAME)Best
9、immungdes PhosphorgehaltesdurchEmissionsspektrometriemit induktivgekoppeltemPlasma(ICP) ThisEuropeanStandardwasapprovedbyCENon2January2003. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanya
10、lteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmembe
11、rintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Slovakia,Spain,Sweden,S
12、witzerlandandUn ited Kingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2003CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN14107:2003EEN14107:2003(E) 2
13、 Foreword Thisdocument(EN14107:2003)hasbeenpreparedbyTechnicalCommitteeCEN/TC307“Oilseeds,vegetable andanimalfatsandoilsandtheirbyproductsMethodsofsamplingandanalysis“,thesecretariatofwhichisheld byAFNOR. ThisEuropeanStandard shallbegiventhestatusofanationalstandard,eitherbypublicationofanidenticalt
14、extor byendorsement,atthelatestbySeptember2003,andconflictingnationalstandardsshallbewithdrawnatthe latestbySeptember2003 ThisdocumenthasbeenpreparedunderMandateM/245onFattyAcidMethylester(FAME)giventoCENbythe EuropeanCommissionandtheEuropeanFreeTradeAssociation. AnnexAisinformative. AccordingtotheC
15、EN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal, Slovakia,Spain,Sweden,Switze
16、rlandandtheUnitedKingdom.EN14107:2003(E) 3 1Scope ThisEuropeanStandardspecifiesaninductivelycoupledplasma(ICP)emissionspectrometrymethodforthe determinationofphosphoruscontentbetween4mg/kgand20mg/kginFattyAcidMethylEsters,hereinafter referredasFAME. ThismethodaimstoevaluatetheFAMEquality,intermsoftr
17、ansesterificationbyproductscontentsuchas phosphorus,whoseconcentrationmayaffectthefuelbehaviour. WARNINGTheuseofthismethodmayinvolvehazardousequipment,materialsandoperations.This methoddoesnotpurporttoaddresstoallofthesafetyproblemsassociatedwithitsuse,butitisthe responsibilityoftheusertosearchandes
18、tablishappropriatesafetyandhealthpracticesanddetermine theapplicabilityofregulatorylimitationspriortouse. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedorundatedreference,provisionsfromotherpublications.These normativereferencesarecitedattheappropriateplacesinthetext,andthepublication
19、sarelistedhereafter.For datedreferences,subsequentamendmentstoorrevisionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthelatesteditionofthe publicationreferredtoapplies(includingamendments). ENISO661, Animalandvegetablefatsando
20、ilsPreparationoftestportion(ISO661:1989). 3 Termsanddefinitions ForthepurposesofthisEuropeanStandard,thefollowingtermanddefinitionapplies. 3.1 phosphoruscontent residualphosphorusremaininginFAMEfromphospholipidsafterthevegetableoiltransesterificationreaction 4Principle Aweighedtestportionofsampleisd
21、ilutedinxylene.Thestandardsarepreparedfromaphosphorusorganic compounddissolvedinamineraloilanddilutedinamixtureofxyleneandstockoil.Theadditionofstockoilmakes itpossibletoreducethedifferencesinviscositybetweensamplesandstandardsandimprovestheirstorage. Thesolutionsareintroducedinaerosolformintoanindu
22、ctivelycoupledargonplasma.Thephosphoruscontentis determinedbycomparingtheemissionoftheelementinthesolutionofthetestportionofthesamplewiththe emissionofthestandardsatthesamewavelength. NOTE1 Thewavelengthscommonlyusedare213,6nmand178,3nm. Thesampleshallbedilutedatleasttentimeswithxyleneinordertoallow
23、aproperintroductionoftheaerosolinto theplasma. NOTE2 Xylenemaybereplacedbyothersuitablesolventsincaseofinstableplasmaorspecificlaboratorysafetyuse.EN14107:2003(E) 4 5Reagents Useonlyreagentsofrecognizedanalyticalgrade,unlessotherwisespecified. 5.1 Recommendationforwashingglassware :inordertoavoidpho
24、sphoruspollutionduetothephosphates containedinthedetergentsusedforwashingtheglassware,rinsethelatteratleasttwice withanapproximate 5mol/lsolutionofhydrochloricacid.Nextrinsewithdistilledwaterthendry. 5.2 Xylene (mixtureofisomers). WARNING Inflammableandnoxious. 5.3 Stockoil75 1) (viscosity75mm 2 /s)
25、. 5.4 Stabilizer 1) ,optional,tostabilisethestocksolution. 5.5 Phosphorusorganicstandard 1) , 1000mg/kg. NOTE Othersuitablecommerciallyavailablestandardcanalsobeused. 5.6 Phosphorus,intermediatedilutionsolutionforpreparationofthesetofcalibrationsolutions : 100mg/lphosphorussolutioncontaining0,6%of s
26、tabilizer(5.4):weightowithin0,001gapproximately5gofthe phosphorussolution(5.5)ina50mlvolumetricflask.Add approximately0,3gofstabilizer(5.4),dilutetothemark withxyleneandhomogenisethesolution.Theexacttitreofthissolutionwillbecalculatedandsubsequentlyused forthestandards.Thissolutionmaybekeptduringone
27、month,ifthestabilizer(5.4)isused. Incasestabilizerisnotused,theintermediatedilutionsolutionofphosphoruscannotbekept. NOTE Thevolumetricflaskscanbereplacedbydisposablenoncalibratedflasks;inthiscase,thedilutionsofthesamples arepreparedandexpressedinmass/massinsteadofmass/volume. 6Apparatus 6.1 Aninduc
28、tivelycoupledplasmaemissionspectrometer equippedwiththefollowingelements: 6.1.1 Aquartztorch. 6.1.2 Anebulizer(devicewhichtransformsthesolutionintoanaerosol). 6.1.3 Aperistalticpumpisnecessary.Thepumpingspeedshallbebetween0,5ml/minand3ml/mininclusive. Viton 2) flowratetubesarerecommendedinordertowit
29、hstandthexylene. 6.2 Balance,withanaccuracyof0,1mg. 6.3 Glassware :25mland50mlvolumetricflasks. 6.4 Graduatedpipettes,of1mland5mlcapacityorVariablevolumeautomaticpipettesfittedwith disposablepolypropylenetips. 1) Possiblesuppliers: CONOSTANDivision,ContinentalOilCo,PoncaCity,OK74706USA SPEXIndustrie
30、s,Inc.ChemicalSalesDepartment,3880ParkAvenue,EdisonNJ08820USA ThisinformationisgivenfortheconvenienceofusersofthisEuropeanstandardanddoesnotconstituteanendorsementby CENoftheseproducts.Equivalentproductsmaybeusediftheycanbeshowntoleadtothesameresults. 2) Vitonisatradenameofflowratetubes. Thisinforma
31、tionisgivenfortheconvenienceofusersofthisEuropeanstandardanddoesnotconstituteanendorsementby CENofthisproduct.Equivalentproductsmaybeusediftheycanbeshowntoleadtothesameresults.EN14107:2003(E) 5 7Sampling Itisimportantthatthelaboratoryreceiveasample,whichistrulyrepresentativeandhasnotbeendamagedor ch
32、angedduringtransportorstorage. SamplingisnotpartofthemethodspecifiedinthisEuropeanStandard.Arecommendedsamplingmethodisgiven inENISO55551. 8 Preparationoftestportion PreparethetestportioninaccordancewithENISO661.Thetestportionshallnotbeheatedand/orfiltered. 9Procedure 9.1 Samplepreparation:inorderto
33、avoidphosphoruspollutionofthesolutions,allsamplingoperationsare carriedoutusingpolypropylenepipettesorautomaticpipetteshavingdisposabletips. Weightowithin0,001gapproximately2,5g(massming)ofsampleina25mlvolumetricflask(volume Vinml), dilutetothemarkwithxyleneandshakemanuallytohomogenise. Taketwotestp
34、ortionspersample. NOTE Thevolumetricflasksmaybereplacedbydisposablenoncalibratedflasks;inthiscase,thedilutionsofthesamples arepreparedandexpressedinmass/massinsteadofmass/volume. 9.2 Preparationofthestandards :preparecalibrationsolutionshavingthefollowingphosphoruscontents: 0mg/l,0,5mg/l,1mg/l,2mg/l
35、,4mg/l. Theexactcontentsofeachstandardsshallbecalculatedaccordingtotheexactconcentrationofphosphorus intermediatesolution(see5.6). NOTE1 Thefollowingprocedureisgivenasanexample: Infive100mlvolumetricflasks,weigh10gofstockoil(5.3).Usinggraduatedpipettes,transfer0ml,0,5ml,1ml,2ml,4 mlof the100mg/lphos
36、phorussolution(see5.6).Filluptothemarkwithxyleneandhomogenisethesolutions. WARNINGThesolutionsshallbefreshlypreparedforeachseriesofanalyses. NOTE2 Whendilutionsofthesamplesareexpressedin%( m/m)(seeNotein5.6),thecalibrationsolutionsarepreparedin ordertobeexpressedinthesameway. 9.3 Preparationoftheapp
37、liance:sinceappliancesstemmingfromdiversemanufacturershavedifferent configurationsandsettings,itisdifficulttospecifyanexactprocedure.Followthemanufacturersinstructionsfor usingtheinstrumentwithorganicsolvents. Thechoiceoftheinstrumentalparametersisdeterminedsoastoobtainthebestsignal/backgroundratio.
38、 9.4 Measurement:themeasurementoftheintensityoftheanalyticallinecorrespondstothecountingofthe maximumofthelinedeductedfromthecountingofthebackground.Certaininstrumentsareequippedwith softwarewhichallowstheautomaticcorrectionofthebackground. 9.5 Calibration:conducttheaspirationofboththeblankandcalibr
39、ationsolutions.Carryoutthree measurementsforeachofthem. Calculateforeachsolutionthearithmeticalmeanofthethreemeasurements. Constructthecalibrationcurvefromthesemeasurementsusinglinearregression,byplottingtheemissionintensity valuesagainstthevaluesoftherespectivephosphorusconcentrationsexpressedinmg/
40、l.EN14107:2003(E) 6 NOTE Iftheplotoftheemissionintensityvaluesagainstthevaluesofthephosphoruscontentsisnotlinear,theprocedure shouldbeinspectedforerrorsand,ifnecessary,thecalibrationprocedureshouldberepeatedstartingwithclause9.2. 9.6 Sampleanalysis :conducttheaspirationofthesolutionofthesample.Carry
41、outthemeasurementsinthe samewayasforthestandards. NOTE Thedrifthastobecheckedregularly. 10Results Determine,accordingtothecalibrationcurve,thephosphorusconcentration c(mg/l)ofthetwotestportionsofa samesample. Calculatethephosphorusconcentration Cofthesample,expressedinmg/kg,usingtheequation: m V c C
42、 = where V isthevolumeofthesamplesolution(millilitres); c isthephosphorusconcentrationofthesamplesolution(milligramsperlitre); m isthemassofthesampletestportion(grams). Calculatethephosphoruscontent Cofthesamplebytakingthearithmeticalmeanofthetwovaluesobtained. Expresstheresultinmg/kgtothenearest0,1
43、mg/kg. NOTE Whenthesolutionsareexpressedinasmassfractioninpercent(seeNotein5.6andNote2in9.2),thecalculation ofthephosphoruscontent Cofthesampleismadeusingtheequation: m P c C p = where c p istheconcentrationofthesamplesolution(milligramsperkilogram); P isthetotalmassofthesolution(grams). 11Precision 11.1 Interlaboratorytest DetailsofaninterlaboratoryaregiveninannexA.Thevaluesderivedfromthesetestsmaynotbeappl
