EN 14108-2003 en Fat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of sodium content by atomic absorption spectrometry《脂肪和油的衍生物 脂肪酸甲基酯(FAME) 用原子吸收光谱法测定钠含量》.pdf

1、BRITISH STANDARD BS EN 14108:2003 Fat and oil derivatives Fatty Acid Methyl Esters (FAME) Determination of sodium content by atomic absorption spectrometry The European Standard EN 14108:2003 has the status of a British Standard ICS 67.200.10 BS EN 14108:2003 This British Standard was published unde

2、r the authority of the Standards Policy and Strategy Committee on 14 May 2003 BSI 14 May 2003 ISBN 0 580 41840 5 National foreword This British Standard is the official English language version of EN 14108:2003. The UK participation in its preparation was entrusted to Technical Committee AW/307, Oil

3、seeds 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 referred to in this document may

4、 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 provisions of a contract. Users a

5、re 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, or proposals for change, an

6、d 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 notice displayed in this documen

7、t indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN14108 April2003 ICS67.200.10 Englishversion FatandoilderivativesFattyAcidMethylEsters(FAME) Determinationofsodiumcontentbyatomicabsorption spectro

8、metry ProduitsdrivsdescorpsgrasEstersmthyliques dacidesgras(EMAG)Dterminationdelateneuren sodiumparspectromtriedabsorptionatomique ErzeugnisseauspflanzlichenundtierischenFettenund lenFettsureMethylester(FAME)Bestimmungdes NatriumgehaltesdurchAtomabsorptionsspektrometrie ThisEuropeanStandardwasapprov

9、edbyCENon2January2003. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheMa

10、nagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationals

11、tandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Slovakia,Spain,Sweden,SwitzerlandandUn ited Kingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNOR

12、MUNG ManagementCentre:ruedeStassart,36B1050Brussels 2003CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN14108:2003EEN14108:2003(E) 2 Foreword Thisdocument(EN14108:2003)hasbeenpreparedbyTechnicalCommitteeCEN/TC307“Oilseeds,vegetable andanimalfatsando

13、ilsandtheirbyproductsMethodsofsamplingandanalysis“,thesecretariatofwhichisheld byAFNOR. This EuropeanStandard shallbegiventhestatusofanationalstandard,eitherbypublicationofanidenticaltextor byendorsement,atthelatestbyOctober2003andconflictingnationalstandardsshallbewithdrawnatthelatestby October2003

14、. ThisdocumenthasbeenpreparedunderMandateM/245onFattyAcidMethylester(FAME)giventoCENbythe EuropeanCommissionandtheEuropeanFreeTradeAssociation,andsupportsessentialrequirementsofEU Directive(s). AnnexAisinformative. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefo

15、llowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal, Slovakia,Spain,Sweden,SwitzerlandandtheUnitedKingdom.EN14108:2003(E) 3 1Scope ThisEuropeanstandard

16、specifiesamethodforthedeterminationofsodiumcontentsequaltoorgreaterthan 1mg/kg. Thismethodisapplicabletofattyacidmethylestersintendedforadditiontomineraloils. WARNINGTheuseofthismethodmayinvolvehazardousequipment,materialsandoperations.This methoddoesnotpurporttoaddresstoallofthesafetyproblemsassoci

17、atedwithitsuse,butitisthe responsibilityoftheusertosearchandestablishappropriatesafetyandhealthpracticesanddetermine theapplicabilityofregulatorylimitationspriortouse. 2Principle Thevegetableoilmethylestersampleisdilutedwithaxylenesolution. Thesodiumcontentinthesampleisdirectlydeterminedbyflameatomi

18、cabsorptionspectrometryatthe wavelengthof589nm.Thecalibrationsolutionsusedarepreparedfromasodiumorganometallicsaltdissolvedin amixtureofxyleneandstockoil.Theadditionofstockoiltothecalibrationsolutionsisnecessaryinorderto improvetheirstorage(thelowelementcontentsareunstable)andthelinearityofthecalibr

19、ation. WARNINGTheestersampleshallbedilutedatleast25timeswithxylenesothatthecomparisonofthe measurementsofthesamplesolutionandstandardsisvalid. NOTE Xylenecanbereplacedbycyclohexaneorlightpetroleuminthoselaboratoriesthatarenotauthorizedtouse aromaticsolvents. 3Reagents Useonlyreagentsofrecognisedanal

20、yticalgrade,unlessotherwisespecified. 3.1 Recommendationsforwashingglassware Theglasswareusedforthepreparationofthesolutionsshallbewashedatleasttwicewithanapproximate5mol/l solutionofhydrochloricacid,rinsedwithdistilledwaterthendriedinordertoavoidsodiumpollution. 3.2 Xylene(mixtureofisomers) WARNING

21、Inflammableandnoxious. 3.3 Stockoil75 (75mm 2 /s) 1) 3.4 Stockoilsolution inxylene(200g/l);diluteina200mlvolumetricflask,40gofstockoil(3.3)withxylene. Storethissolutioninapolypropylenebottle. 3.5 Sodium,solutioninoil(5000mg/kg) 1) .Readytousesolutionofasodiumorganometallicsaltinstockoil, havingacert

22、ifiedtitre. 3.6 Sodium,solutionsofintermediarydilutionsforthepreparationofthesetofcalibrationsolutions. 1) ProductsavailablecommerciallyfromCONOSTANStandard,suppliedbyConostanDivision,ContinentalOilCo,Ponca City,OK74601USA. SPEXStandardsuppliedbySPEXIndustries,Inc.ChemicalSalesDepartment,3880ParkAve

23、nue,Edison,NJ08820USA. ThisinformationisgivenfortheconvenienceofusersofthisEuropeanStandardanddoesnotconstituteanendorsementby CENoftheseproducts .EN14108:2003(E) 4 3.6.1 Sodium,solutioninxylene(500mg/l):weigh,towithin0,001g,approximately2,5gofthesodiumsolution (3.5)ina25mlvolumetricflaskanddiluteto

24、themarkwithxylene. Thissolutionmaybestoredforamonth. 3.6.2 Sodium,solutioninxylene(5mg/l):sample,usingapipette,0,50mlofthesodiumstandardsolution (3.6.1),transferintoa50mlvolumetricflaskanddilutetothemarkwithxylene. Prepareanewsolutioneachday. NOTE Thesolutionsofintermediarydilutionsmaybepreparedingl

25、assflasks(thesodiumpollutionbeingnegligibleat thesecontents). 4Apparatus 4.1 Atomicabsorptionspectrometer Anyatomicabsorptionspectrometermaybeusedprovidedthatitisequippedwith: 4.1.1 Ahollowsodiumcathodelamp. 4.1.2 Anebulizationsystemsuitedfortheorganicsolutions,ofwhichthematerialsaresolventresistant

26、. 4.1.3 Aburnerheadcapableofbeingusedwithorganicsolutionsandanairacetyleneflame. 4.2 Balance,withanaccuracyof1mg. 4.3 Glassware 4.3.1 25mland50mlvolumetricflasks. 4.3.2 0,5mlgraduatedprecisionpipette. 4.4 Polypropyleneware 4.4.1 50mland200mlvolumetricflasks. 4.4.2 10mlpipette. 4.4.3 250mlbottles 4.4

27、.4 Automaticpipettehavingavariablevolumeof1mlto5ml,fittedwithejectableanddisposable polypropylenetips. 5Procedure WARNING In order to avoid polluting the sodium solutions, it is recommended to prepare all the determinationsolutionsinpolypropyleneflasksandtoconductallthesamplingoperationsusing polypr

28、opylenepipettesorpipetteshavingdisposablepolypropylenetips.Itishoweverpossibletouse glasswaretakingcleaningprecautionsinordertoavoidpollutionbytheelementsbeinganalysed. 5.1Sampling SamplingisnotpartofthemethodspacifiedinthisEuropeanStandard.Arecommendedsamplingmethodisgiven inENISO55551.EN14108:2003

29、(E) 5 5.2 Preparationofthesample 5.2.1 Weightowithin0,001gapproximately2g(massming)ofestersampleina50mlvolumetricflask (volume Vinml)anddilutetothemarkwithxylene. 5.2.2 Sampletwotestportionspersample. 5.3 Preparationofthesetofcalibrationsolutions 5.3.1 Preparethecalibrationssolutionshavingthefollowi

30、ngsodiumcontents: 0,1mg/l0,2mg/l0,3mg/l. 5.3.2 Usingavariablevolumeautomaticpipette,transfer1,00ml,2,00mland3,00mlofthe5mg/lsodium solution(3.6.2)into50mlvolumetricflasks. 5.3.3 Withapolypropylenepipette,addtoeachflask10mlofthe200g/lsolutionofstockoilinxylene(3.4)and dilutetothemarkwithxylene. 5.3.4

31、 Preparethezeromemberorblanktestinthesamemannerwithoutaddinganysodiumsolution. 5.3.5 Preparethecalibrationsolutionsjustpriortotheirmeasurementonaccountoftheirinstability. 5.4Spectrometric measurements 5.4.1 Preparationofthespectrometer Setthewavelengthat589,0nmandthebandpassat0,5nm; conducttheaspira

32、tionofthe0,3mg/lcalibrationsolutioninordertooptimizethedifferentinstrumentsettings. Seekthemaximumresponseofthesignalbyadjusting: theairacetylenegaseousmixture; theaspirationspeedofthesolution; theburnerposition. conducttheaspirationofthexyleneplacedinapolypropylenebottleinordertosettheinstrumentatz

33、ero absorbance. 5.4.2Calibration Conducttheaspirationoftheblank(orzeromember)andcalibrationsolutionsandcarryoutthreemeasurements foreachofthem. Calculateforeachsolutionthearithmeticalmeanofthethreemeasurements. Plotthecalibrationcurvefromthemeansobtained. Bywayofindication,thevalueoftheopticaldensit

34、yobtainedfora0,3mg/lconcentrationisapproximately0,290 andthecurveismoreorlessastraightlineintherangeconsidered. 5.4.3Samples Conducttheaspirationofthesolutionsofthesamplesandcarryoutthemeasurementsinthesamewayasforthe standards.EN14108:2003(E) 6 NOTE Inthecasewherethemeasurementofthesampleexceedsthe

35、setofcalibrationsolutionsgivenin5.3,prepare standardshavinghighersodiumcontents,themaximumcontentbeing1mg/l. 6 Expressionofresults Determinethesodiumcontentsc 1 andc 2 inmg/lofthetwotestportionsofthesample,byreferringtothe calibrationcurve. Calculatethesodiumcontents C 1 and C 2 ofthesample,expresse

36、dinmg/kg,usingtheequation: m V c C = where m isthemass(ingrams)ofthesampletestportion; V isthevolumeofthesamplesolution(inmillilitres). Calculatethemeancontent Cofsodiuminthesamplefrom C 1 and C 2 . Expresstheresultinmg/kg,tothenearest0,1mg/kg. 7Precision Aninterlaboratorytestorganizedin2000atEurope

37、anlevelwiththeparticipationof13laboratories,eachhaving carriedouttwodeterminationsoneachsample,gavethestatisticalresultsindicatedinannexA. 7.1Repeatability Theabsolutedifferencebetweentwoindependentsingletestresults,obtainedusingthesamemethodonidentical testmaterialinthesamelaboratorybythesameoperat

38、orusingthesameequipmentwithinashorttimeinterval, shallnotbegreaterthan: r=0,086X+0,242 morethanonceoutof20determinations. 7.2Reproducibility Theabsolutedifferencebetweentwosingletestresults,obtainedusingthesamemethodonidenticaltestmaterial indifferentlaboratoriesbydifferentoperatorsusingdifferentequ

39、ipment,shallnotbegreaterthan: R=0,263X+1,355 morethanonceoutof20determinations. 8 Testreport Thetestreportshallspecify: allinformationnecessaryforthecompleteidentificationofthesample; thesamplingmethodusedifknown; thetestmethodused,withreferencetothisEuropeanstandard;EN14108:2003(E) 7 alloperatingde

40、tailsnotspecifiedinthisEuropeanStandard,orregardedasoptional,togetherwithdetailsof anyincidentswhichmayhaveinfluencedthetestresult(s); thetestresult(s)obtained,oriftherepeatabilityhasbeenchecked,thefinalquotedresultobtained.EN14108:2003(E) 8 Annex A (informative) Resultsofaninterlaboratorytrial Resu

41、ltsofaninterlaboratorytrial. AEuropeancollaborativetestinvolving13laboratoriesin6countrieswascarriedouton5samples: Sample1: FAMEpreparedfromrapeseedoil; Sample2: FAMEpreparedfromsunfloweroil; Sample3: FAMEpreparedfromamixtureofrapeseedandsunfloweroils(80:20); Sample4: FAMEpreparedfromamixtureofrapes

42、eedandsunfloweroils(60:40); Sample5: FAMEpreparedfromrapeseedoil. ThetestwasorganizedbyCENTC307/WG1in2000andtheresultsobtainedweresubjectedtostatistical analysisinaccordancewithENISO42592togivetheprecisiondatashowninTableA.1. TableA.1Sodiumcontent S a m p l e 12345 Nofparticipatinglaboratories 13 13

43、 13 13 13 Nofparticipatinglaboratoriesaftereliminatingoutliers 13 12 13 12 12 Meanvalue (mg/kg) 4,96 1,14 3,14 1,00 3,01 Repeatabilitystandarddeviation(mg/kg) 0,23 0,10 0,21 0,13 0,11 Reproducibilitystandarddeviation(mg/kg) 0,88 0,53 0,69 0,54 0,69 Repeatabilitylimit, r(mg/kg) 0,70 0,32 0,64 0,39 0,32 Reproducibilitylimit R(mg/kg) 2,70 1,64 2,10 1,67 2,13EN14108:2003(E) 9 Bibliography 1 ENISO5555, AnimalandVegetabl