1、BRITISH STANDARD BS EN 14481:2003 Materials and articles in contact with foodstuffs Plastics Test methods for the determination of fatty contact The European Standard EN 14481:2003 has the status of a British Standard ICS 67.250; 83.080.01 BS EN 14481:2003 This British Standard was published under t
2、he authority of the Standards Policy and Strategy Committee on 4 June 2003 BSI 4 June 2003 ISBN 0 580 41990 8 National foreword This British Standard is the official English language version of EN 14481:2003. The UK participation in its preparation was entrusted by Technical Committee CW/47, Materia
3、ls and articles in contact with foodstuffs, to Subcommittee CW/47/1, Migration from plastics, which has the responsibility to: A list of organizations represented on this subcommittee can be obtained on request to its secretary. Cross-references The British Standards which implement international or
4、 European publications referred 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 incl
5、ude all the necessary provisions 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 enqui
6、ries 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 cover, the EN title page, pages 2 to 13 and a back c
7、over. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN14481 May2003 ICS67.250;83.080.01 Englishversion Materialsandarticlesincontactwithfoodstuffs
8、PlasticsTest methodsforthedeterminationoffattycontact Matriauxetarticlesencontactaveclesdenres alimentairesPlastiquesMthodesdessaipourla dterminationduncontactgras WerkstoffeundGegenstndeinKontaktmitLebensmitteln KunstoffePrfverfahrenzurBestimmungdesfettigen Kontaktes ThisEuropeanStandardwasapproved
9、byCENon9January2003. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheMana
10、gementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalsta
11、ndardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Slovakia,Spain,Sweden,SwitzerlandandUn ited Kingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMU
12、NG ManagementCentre:ruedeStassart,36B1050Brussels 2003CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN14481:2003EEN14481:2003(E) 2 Contents Page Foreword3 1 Scope 5 2 Principle5 3 Reagents.5 4 Apparatus .5 5 Preparationofstandardsandsamples .6 5.1 P
13、reparationofstandards 6 5.1.1 StocksolutionofDPBDat1mg/ml .6 1.1.2 WorkingstandardsolutionofDPBDinnhexaneat1 g/ml.6 1.1.3 StocksolutionofDPHTat1mg/ml .6 1.1.4 CalibrationsolutionofDPHTinnhexaneat100 g/ml.6 1.2 Preparationofsamples .7 6 HPLCanalysis . .8 6.1 Calibrationstandards . .8 1.2 Analysis 8 1
14、.3 Calibrationgraph . 8 1.4 Checkforanalyticalbias. 8 7 Expressionofresults . .9 7.1 Methodofcalculation . .9 7.2 Interpretation10 7.3 Performanceofthemethod . .10 8 Testreport . .10 AnnexA (informative) TypicalHPLCchromatogramforstandard1,4diphenyl1,3butadieneand1,6 diphenyl1,3,5hexatriene 11 Annex
15、ZA (informative) RelationshipofthisEuropeanStandardwithCouncilDirective85/572/EEC.12 Bibliography 13EN14481:2003(E) 3 Foreword Thisdocument(EN14481:2003)hasbeenpreparedbyTechnicalCommitteeCEN/TC194“Utensilsincontact withfood“,thesecretariatofwhichisheldbyBSI. ThisEuropeanStandardshallbegiventhestatu
16、sofanationalstandard,eitherbypublicationofanidenticaltextor byendorsement,atthelatestbyNovember2003,andconflictingnationalstandardsshallbewithdrawnatthelatest byNovember2003. ThisdocumenthasbeenpreparedunderamandategiventoCENbytheEuropeanCommissionandtheEuropean FreeTradeAssociation. ThisEuropeanSta
17、ndardcontainsaninformativeAnnexA. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherla
18、nds,Norway,Portugal, Slovakia,Spain,Sweden,SwitzerlandandtheUnitedKingdom.EN14481:2003(E) 4 Introduction Forcertainspecifiedfoodtypes,ifitcanbedemonstrated,bymeansofanappropriatetest,thatthereisnofatty contactwiththeplastic,themigrationtestwithsimulantD(oliveoiloralternatives)maybedispensedwith.The
19、methoddescribedherecanbeusedtodeterminewhetherafoodmakesfattycontactwithplastics. NOTE1 ThefoodtypesarespecifiedinCouncilDirective85/572/EEC1. NOTE2 Guidanceontheselectionofconditionsandtestmethodsforoverallmigration,andthetestmethodsforthespecific migrationofsubstancesfromplasticsintofoodandfoodsim
20、ulantsandthedeterminationofsubstancesinplasticsandthe selectionofconditionsofexposuretofoodsimulantsisgiveninEN11861andEN131301respectivelyEN14481:2003(E) 5 1Scope ThisPartofthisEuropeanStandardspecifiesatestmethodtodeterminewhetherthereisfattycontactandis applicabletoallfoods.Testingsomefoodscanreq
21、uiremodificationstothemethod.Themethodisapplicableto contactsituationsfrom20Cto100 C. 2Principle Fattycontactbetweenafoodandaplasticmaterialorarticleisdeterminedbyplacingfoodincontactwitha polyethylenefilmcontainingafatsolublefluorescentdye.Afterexposure,thedyeisextractedfromthefoodand determinedbyh
22、ighperformanceliquidchromatography(HPLC)withfluorescencedetection.Themethodemploys 1,6diphenyl1,3,5hexatrieneasinternalstandard.Thedegreeoftransferisrelatedtotheextentoffattycontact made,andisusedtodeterminewhethersimulantDbeemployedornotinsubsequenttestsofplasticsintendedto comeintocontactwiththatf
23、ood. Thefoodusedinthetestshouldbethesameas,orsimilarincompositionto,thefoodwhichwillcomeintocontact withtheplasticinactualuse.Toallowforpossibledifficultiesencounteredinobtainingreproduciblefilmtofood contact,thetestiscarriedoutonfivereplicatesamplesofthefood. 3Reagents Allreagentsshallbeofrecognise
24、danalyticalquality,unlessotherwisespecified. 3.1 Lowdensitypolyethylenefilmcontaining1,4diphenyl1,3butadiene,fluorescentdye,at17,3 g/dm 2 0,9 g/dm 2 ,intheformofalayflattubeofwidth20cm,e.g.thecertifiedreferencematerialBCR.593,PlasticfilmE, certifiedonthebasisofthemassfractionofDPBD(12,58mg/kg0,63mg/
25、kg)andonthefilmthickness(149,7m 0,7m). 3.2 1,4diphenyl1,3butadiene(DPBD) 3.3 1,6diphenyl1,3,5hexatriene(DPHT) NOTE AsDPBDandDPHTareslightlylightsensitive,thefilmandstandardsshouldbestoredwiththeexclusionoflight. 3.4 nHexane,C 6 H 14 ,HPLCgrade NOTE Asnhexaneisconsideredtobeharmfulbyinhalation,ingest
26、ionandthroughskincontact,correctsafetyprocedures shouldbefollowedatalltimeswhenusingthissolvent. 3.5 Dichloromethane,CH 2 Cl 2 ,HPLCgrade NOTE Asdichloromethaneisconsideredtobeharmfulbyinhalation,ingestionandthroughskincontactandasapotential carcinogen,correctsafetyproceduresshouldbefollowedatalltim
27、eswhenusingthissolvent. 4Apparatus 4.1 Heatsealersuitableforsealingthepolyethylenefilm(3.1) 4.2 Dispersionhomogenizer 4.3 Centrifuge,benchtop 4.4 Centrifugetubes,10mlto20mlcapacity 4.5 Filterpaper,15,0cmdiametercircles,WhatmanGrade2orequivalent 4.6 Volumetricflasks,25ml,50mland100mlcapacityEN14481:2
28、003(E) 6 4.7 Glassvials,2mland20mlcapacitywithscreworcrimpcapclosuresandpolytetrafluoroethylene(PTFE) linedsealingdisks 4.8 Pasteurpipettes 4.9 Syringes,glassbarrelled,withneedles,50 l,100 l,500 l,1ml,2,5mland10mlcapacity 4.10 Filterfunnels,glass 4.11 HPLCequipment NOTE Witha20 linjectionloopandapum
29、pingsystemcapableofgeneratingagradientat0,5ml/minofnhexane(held for7min)switchedtodichloromethaneover1min(heldfor5min),returnedtonhexaneover1minandthenequilibratedfor 6min. 4.11.1 Fluorescencedetector,withexcitationwavelengthof346nmandemissionwavelengthof374nmand linkedtoachromatographicrecorderandi
30、ntegrator 4.11.2 HPLCcolumn NOTE Thefollowingcolumnhasbeenfoundsuitable.Stainlesssteel,100mmx3mminternaldiameter,silica,5 m particlesize. 4.12 Vacuumlinewithattachedneedle 4.13 Beakers,glass,tallform,400mlcapacity 4.14 Thermostaticallycontrolledcabinet(s)capableofmaintainingatemperatureof20 C2 C,5 C
31、1 C, 25 C1 Cand70 C2 C. 4.15 Foodprocessor 4.16 Volumetricglasspipette,5mlcapacity 5 Preparationofstandardsandsamples 5.1 Preparationofstandards 5.1.1 StocksolutionofDPBDat1mg/ml Weigh0,050g 0,001gofDPBD(3.2)intoa50mlvolumetricflaskandmaketothemarkwithnhexane(3.4). 5.1.2 WorkingstandardsolutionofDPB
32、Dinnhexaneat1 g/ml Placeapproximately50mlofnhexaneintoa100mlvolumetricflask.Add,bysyringe,100 lofthestocksolution (5.1.1).Maketothemarkwithnhexane. 5.1.3 StocksolutionofDPHTat1mg/ml Weigh0,050g 0,001gofDPHT(3.3)intoa50mlvolumetricflaskandmaketothemarkwithdichloromethane (3.5). 5.1.4 Calibrationsolut
33、ionofDPHTinnhexaneat100 g/ml Placeapproximately30mlofnhexaneintoa50mlvolumetricflask.Add,bypipette(4.16),5mlofthestock solution(5.1.3).Maketothemarkwithnhexane. NOTE AsDPBDandDPHTaresensitivetolight,standardsolutionsshouldbestoredwiththeexclusionoflight.EN14481:2003(E) 7 5.2 Preparationofsamples 5.2
34、.1 Thereferencefilmisintheformofalayflatpolyethylenetubewoundonacardboardcore,wrappedin aluminiumfoilandthenheatsealedinabarrierpack.Unpackthefilm.Unrolltheouterturnfromthereel,cutoff anddiscard.Cuta220mmlengthofthefilm.Usetheheatsealer(4.1)tocloseoneofthecutedges.Placethe foodsampleinthepouchsoform
35、edandthensealtheopeningtogivea200mmx200mmpouch. Prepareafurtherfourreplicatepouchescontainingfood. NOTE Thequantityoffoodusedandtheplastictofoodcontact,shouldberepresentativeofthatinactualuse.Some foodscanneedmodificationtogiverepresentativecontacte.g.fornonhomogeneousfoodswithdifferingsurfaces,itco
36、uldbe necessarytocutthefoodsuchthatonlythefoodsurfacewhichwillcontacttheplasticinactualusecomesintocontactwith the polyethylenefilm.Alternatively,thenonrepresentativesurface(s)canbeshieldedfromcontactbyintroducinganinterlayer ofn hexanewashedaluminiumfoilbetweenthesurface(s)andthefilm. Whereafoodisn
37、onhomogeneousandanactualusesizeportionwillnotfitinthepouch,itissuggestedthatthefoodsample bemodifiedbycuttingorotherwisereducinginsize,ensuringthattheportiontakenforexposureisrepresentativeofthefoo das awhole.Forexample,foracutoffish,theratioofskintoleanfleshinthecutportionshouldbethesameasthatforth
38、e whole portion.Cautionshouldbetakentoensurethatcutedgesdonotmodifythenatureofthefood.Ifnecessary,theymaybe shieldedfromcontactbytheuseofaluminiumfoil. Forhomogeneousfoodssuchaspowdersandliquids,a100mmx100mmpouchcanbeusedandthequantityoffood reducedaccordingly. 5.2.2 Aftersealingthefoodinthebag,inse
39、rtthevacuumneedle(4.12)atonecornerandusevacuumsuctionto removethetrappedair.Whenthemajorityoftheairisremovedandthefoodsamplemakesgoodcontactwiththe film,withdrawtheneedleslightlyandresealthepouchacrossthecornerwithoutallowingingressofair. NOTE Thecontactbetweenthefoodandthetestplasticshouldbesimilar
40、tothatwhichoccursinactualuse.Samples shouldnotbeevacuatedsostronglythatthefoodiscrushedandabnormalcontactisobtained. 5.2.3 Usingapenmarktheoutlineofthefoodonbothwallsofthepouch.Measuretheareawithinthisoutline. Thisisthecontactarea. 5.2.4 Placethefilledpouchesinthethermostaticallycontrolledcabinet(4.
41、14).Exposefortherequiredtime periodandtemperaturechosenaccordingtoTable1. Table1Testtimesandtemperatures Intended application Testtimeandtemperature Contactupto100 o C 30 1 0 minat70 o C2 o C Ambientstorage 30 1 0 dat25 o C1 o C Refrigeratedstorage 168 6 0 hat5 o C1 o C Frozenstorage 28 1 0 dat20 o
42、C2 o C NOTE1 Indicationsonly.Forspecificapplications,thetimeandtemperatureofthetestcanbevariedfromthoseshownin table1,tocorrespondmorecloselywiththoseexpectedforthatapplication,whereknown. NOTE2 AsDPBDisslightlylightsensitive,thefilledpouchesshouldbetestedinsubduedlight.Subsequentextraction procedur
43、esshouldbeconductedawayfromdirectsunlightandthefinalextractsshouldbestoredeitherinambervialsorwith theexclusionoflight.EN14481:2003(E) 8 Thefoodshallbeexaminedaftertheexposureperiodtocheckforanychangeinnaturee.g.mould,desiccation, separationoffoodconstituents.Ifthefoodhaschangedinawaythatdoesnotoccurinactual
