1、BRITISH STANDARD BS EN 1186-11:2002 Materials and articles in contact with foodstuffs Plastics Part 11: Test methods for overall migration into mixtures of C-labelled synthetic triglycerides The European Standard EN 1186-11:2002 has the status of a British Standard ICS 67.250 BS EN 1186-11:2002 This
2、 British Standard, having been prepared under the direction of the Consumer Products and Services Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee on 14 October 2002 BSI 14 October 2002 ISBN 0 580 40572 9 National foreword This Br
3、itish Standard is the official English language version of EN 1186-11:2002. It supersedes DD ENV 1186-11:1995 which is withdrawn. The UK participation in its preparation was entrusted by Technical Committee CW/47, Materials and articles in contact with foodstuffs, to Subcommittee CW/47/1, Migration
4、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 European publications referred to in this document may be found in the BSI Cat
5、alogue 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 are responsible for its c
6、orrect 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, and keep the UK interests
7、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 57 and a back cover. The BSI copyright date displayed in this document indicates when the docu
8、ment was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN118611 September2002 ICS67.250 Englishversion MaterialsandarticlesincontactwithfoodstuffsPlasticsPart 11:TestmethodsforoverallmigrationintomixturesofClabelled synthetictri
9、glycerides Matriauxetobjetsencontactaveclesdenres alimentairesMatireplastiquePartie11:Mthodes dessaipourlamigrationglobaledansdesmlangesde triglycridessynthtiquesmarqusauC WerkstoffeundGegenstndeinKontaktmitLebensmitteln KunststoffeTeil11:Prfverfahrenfrdie GesamtmigrationinMischungenaus14Cmarkierten
10、 synthetischenTriglyceriden ThisEuropeanStandardwasapprovedbyCENon29April2002. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcerning
11、s uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesame
12、statusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDE
13、NORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2002CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN118611:2002EEN118611:2002(E) 2 Contents page Foreword . 3 1 Scope 4 2 Normativereferences 4 3 MethodATotalim
14、mersion .4 4 MethodBCellmethod 15 5 MethodCPouch 25 6 MethodDArticlefillingmethod. 36 AnnexA (normative) Determinationoftheneedforsampleconditioning 48 AnnexB (normative) Determinationoftheneedforsampleconditioningand determinationofthemassofmoisturesensitivetestspecimens,byvacuumdrying 49 AnnexC (n
15、ormative) Determinationofchangeinmoisturecontentoftestspecimensby measurementofthetransferofwaterto,orfrommixtureof 14 Clabelledsynthetic triglycerides,byKarlFischertitration 51 AnnexD (informative) Exampleofapouchholder . 54 AnnexE (informative) Precisiondata 55 AnnexZA (informative) Relationshipof
16、thisEuropeanStandardwithCouncilDirective 89/109/EECandCommissionDirective90/128/EECandassociatedDirectives 56 Bibliography . 58EN118611:2002(E) 3 Foreword ThisdocumentEN118611:2002hasbeenpreparedbyTechnicalCommitteeCEN/TC194,“Utensils incontactwithfood“,thesecretariatofwhichisheldbyBSI. ThisEuropean
17、Standardshallbegiventhestatusofanationalstandard,eitherbypublicationofan identicaltextorbyendorsement,atthelatestbyMarch2003,andconflictingnationalstandardsshall bewithdrawnatthelatestbyMarch2003. ThisdocumentsupersedesENV118611:1995. ThisEuropeanStandardhasbeenpreparedasoneofaseriesofmethodsoftestf
18、orplasticsmaterials andarticlesincontactwithfoodstuffs. ThisdocumenthasbeenpreparedunderamandategiventoCENbytheEuropeanCommissionand theEuropeanFreeTradeAssociation. ForrelationshipwithEUDirective(s),seeinformativeannexZA,whichisanintegralpartofthis document. Atthetimeofpreparationandpublicationofth
19、isstandardtheEuropeanUnionlegislationrelatingto plasticsmaterialsandarticlesintendedtocomeintocontactwithfoodstuffsisincomplete.Further DirectivesandamendmentstoexistingDirectivesareexpectedwhichcouldchangethelegislative requirementswhichthisstandardsupports.Itisthereforestronglyrecommendedthatusers
20、ofthis standardrefertothelatestrelevantpublishedDirective(s)beforecommencementofanyofthetestor testsdescribedinthisstandard. Furtherpartsofthisstandardhavebeenprepared,concernedwiththedeterminationofoverall migrationfromplasticsmaterialsintofoodsimulants.Theirtitlesareasfollows: EN1186Materialsandar
21、ticlesincontactwithfoodstuffsPlastics Part1 Guidetotheselectionofconditionsandtestmethodsforoverallmigration Part2 Testmethodsfor overallmigrationintooliveoilbytotalimmersion Part3 Testmethodsforoverallmigrationintoaqueousfoodsimulantsbytotalimmersion Part4 Testmethodsforoverallmigrationintooliveoil
22、bycell Part5 Testmethodsforoverallmigrationintoaqueousfoodsimulantsbycell Part6 Testmethodsforoverallmigrationintooliveoilusingapouch Part7 Testmethodsforoverallmigrationintoaqueousfoodsimulantsusingapouch Part8 Testmethodsforoverallmigrationintooliveoilbyarticlefilling Part9 Testmethodsforoverallmi
23、grationintoaqueousfoodsimulantsbyarticlefilling Part10 Testmethodsforoverallmigrationintooliveoil(modifiedmethodforuseincaseswhere incompleteextractionofoliveoiloccurs) Part12 Testmethodsforoverallmigrationatlowtemperatures Part13 Testmethodsforoverallmigrationathightemperatures Part14 Testmethodsfo
24、rsubstitutetestsforoverallmigrationfromplasticsintendedtocome intocontactwithfattyfoodstuffsusingtestmediaisooctaneand95%ethanol Part15 Alternativetestmethodstomigrationintofattyfoodsimulantsbyrapidextractionintoiso octaneand/or95%ethanolEN118611:2002(E) 4 EN118611shouldbereadinconjunctionwithEN1186
25、1. TheannexesA,BandCarenormative.TheannexesD,EandFareinformative. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthe followingcountriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic, Denmark,Finland,France,Germany,Greece,Iceland,Ireland,Italy,L
26、uxembourg,Malta,Netherlands, Norway,Portugal,Spain,Sweden,SwitzerlandandtheUnitedKingdom. 1Scope ThisEuropeanStandardspecifiestestmethodsforthedeterminationoftheoverallmigrationintofatty foodsimulantsfromplasticsmaterialsandarticlesintoamixtureof 14 Clabelledsynthetictriglycerides attemperaturesabov
27、e20Candupto,andincluding,121Cforselectedtimes. Thesemethodsaresuitableforplasticsintheformoffilmsandsheets,awiderangeofarticlesor containersfromwhichtestpiecesofasuitablesizecanbecutandcontainersandarticlesthatcanbe filled. Thetestmethodsdescribedareapplicabletoallplastics. 2 Normativereferences Thi
28、sEuropeanStandardincorporatesbydatedandundatedreference,provisionsfromother publications.Thesenormativereferencesarecitedattheappropriateplacesinthetextandthe publicationsarelistedhereafter.Fordatedreferences,subsequentamendmentstoandrevisionsof anyofthesepublicationsapplytothisEuropeanStandardonlyw
29、henincorporatedinitbyamendment orrevision.Forundatedreferencesthelatesteditionofthepublicationreferredtoapplies(including amendments). EN11861:2002, MaterialsandarticlesincontactwithfoodstuffsPlastics Part1:Guidetothe selectionofconditionsandtestmethodsforoverallmigration. EN100881, StainlesssteelsP
30、art1:Listofstainlesssteels. ISO648, LaboratoryglasswareOnemarkpipettes . ISO4788, LaboratoryglasswareGraduatedmeasuringcylinders. 3 MethodATotalimmersion 3.1Principle WARNING Theuseanddisposalof 14 Clabelledsubstancesaresubjecttoregulationswhichvaryfrom countrytocountry.Laboratoriesshouldensurethatt
31、heycomplywithlocallegislationrequirements. NOTE1 Thismethodismostsuitableforplasticsintheformoffilmsandsheets,butcanbeappliedtoawide rangeofarticlesorcontainersfromwhichtestpiecesofasuitablesizecanbecut. Theoverallmigrationfromasampleoftheplasticsisdeterminedasthelossinmassperunitof surfaceareainten
32、dedtocomeintocontactwithfoodstuffs. Theselectionoftheconditionsoftestwillbedeterminedbytheconditionsofuse,seeclauses6and7 ofEN11861:2002.EN118611:2002(E) 5 Testspecimensofknownmassareimmersedina mixtureof 14 Clabelledsynthetictriglyceridesforthe exposuretimeattemperaturesabove20Cand,uptoandincluding
33、,121C,thentakenfromthe mixtureof 14 Clabelledsynthetictriglycerides,blottedtoremovesynthetictriglyceridesadheringtothe surfaceandreweighed. Thespecimenswillusuallyretainabsorbed mixtureof 14 Clabelledsynthetictriglycerideswhichare extractedanddeterminedquantitativelybymeansofliquidscintillationcount
34、ing. Forsomeplasticsthesoxhletextractionprocessdoesnotachievecompleterecoveryoftheabsorbed mixtureof 14 Clabelledsynthetictriglycerides.Inthismethodthe mixtureof 14 Clabelledsynthetic triglyceridesthatremainsaftersoxhletextractionisreleasedbydissolutionorcombustion.The combustionmethodissuitablefora
35、llplastics,thedissolutionmethodisonlysuitableforpolymersthat aresolubleinasuitablesolvent,e.g.tetrahydrofuran. NOTE2 Goodsensitivitycanonlybeachievedforsamplesofverylowmass,e.g.forthinfilms.Thespecific radioactivityofthemixtureof 14 Clabelledsynthetictriglyceridesroutinelyusedisapproximately200dpm/m
36、g.In routineteststhelimitofdeterminationinliquidscintillationcountingisintheorderof20dpmpersample,for combustion,and10dpmpersample,fordissolution.Incombustiononlyaliquotsuptoapproximately50mgcan beused.Consequentlythedeterminationlimitforretainedsimulantisintheorderof0,1mgto50mg.Itis apparentthatfor
37、heavytestspecimensthemethodgivesonlyanestimationoftheretainedsimulant.The dissolutionmethod,whichisgenerallypreferred,resultsinsimilarfigures.Ahigherspecificradioactivityofthe simulantwouldimprovethedeterminationlimit. Migrationintothe mixtureof 14 Clabelledsynthetictriglyceridesiscalculatedbysubtra
38、ctingthemassof 14 Clabelledsynthetictriglyceridesretainedbythetestspecimenfromthemassofthetestspecimen afterremovalfromthe 14 Clabelledsynthetictriglycerides,andthensubtractingthismassfromthe initialmassofthespecimen. Thetotallossinmassisexpressedinmilligramspersquaredecimetreofsurfaceareaofthespeci
39、men andtheoverallmigrationisreportedasthemeanofaminimumofthreedeterminationsonseparate testspecimens. Toallowforinaccuracieswhichmayariseduringtheprocedureandwhichmaybedifficulttodetect, dueforexampletocontaminationorlossofthe 14 Clabelledsynthetictriglyceridesduringthesample handlingstages,quadrupl
40、icatedeterminationsarecarriedoutonthesampleallowingfortheresult fromonespecimentobediscarded. Thismethodincludesvariationswhichareapplicabletocertainplasticsandtoexperienced laboratories. 3.2Reagents NOTE Allreagentsshouldbeofrecognizedanalyticalquality,unlessotherwisespecified. 3.2.1Mixture of 14 C
41、labelledsynthetictriglycerides, simulantDasspecifiedin5.2of EN11861:2002. NOTE DetailsofsupplierscanbeobtainedfromCEN. 3.2.2 Extractionsolvent(see10.1ofEN11861:2002). 3.2.2.1 Pentane98%(mixedisomers)boilingpoint36C. WARNING Pentaneisaveryvolatileandhighlyflammablesolvent.Takecarewhenusingandhandling
42、 thissolventtopreventcontactwithsourcesofignition.Itisnotrecommendedforextractionswiththis solventtobeleftunattended,particularlyovernight. NOTE Duetolowboilingpointofthesolvent,cooledcondenserwatercanbeusedtopreventunduelossof thesolventfromthecondenser.EN118611:2002(E) 6 3.2.2.2 Othersuitablesolve
43、nt. NOTE Inpreviousmethodsfordeterminingoverallmigrationinto 14 Clabelledsynthetictriglyceridesthe extractionsolventusedhasbeen1,1,2trichlorotrifluoroethane.Forenvironmentalreasonstheuseofthissolvent shouldbeavoidedwherepossible,see10.1ofEN11861:2002.Experiencehasshownthatthissolventalthough effectiveformostplasticsrequireslongerperiodsofextraction. 3.2.3Liquid scintillation cocktail, suitableforscintillationcountingofthe 14 Clabelledsynthetic triglyceridesandinwhichthefatsimulantissol
