1、BRITISH STANDARD BS EN 1186-12:2002 Materials and articles in contact with foodstuffs Plastics Part 12: Test methods for overall migration at low temperatures The European Standard EN 1186-12:2002 has the status of a British Standard ICS 67.250 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED B
2、Y COPYRIGHT LAWBS EN 1186-12:2002 This 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 21 May 2002 BSI 21 May 2002 ISBN 0 580 397
3、45 9 National foreword This British Standard is the official English language version of EN 1186-12:2002. It supersedes DD ENV 1186-12:1995 which is withdrawn. The UK participation in its preparation was entrusted by Technical Committee CW/47, Materials in contact with food, to Subcommittee CW/47/1,
4、 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 European publications referred to in this document may be found in
5、the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are
6、responsible for their 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 European committee any enquiries on the interpretation, or proposals for change, and keep the UK i
7、nterests 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 19 and a back cover. The BSI copyright date displayed in this document indicates when
8、 the document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN118612 April2002 ICS67.250 SupersedesENV118612:1995 Englishversion MaterialsandarticlesincontactwithfoodstuffsPlasticsPart 12:Testmethodsforoverallmigrationatlowt
9、emperatures Matriauxetobjetsencontactaveclesdenres alimentairesMatireplastiquePartie12:Mthodes dessaipourlamigrationglobalebassestempratures WerkstoffeundGegenstndeinKontaktmitLebensmitteln KunststoffeTeil12:Prfverfahrenfrdie GesamtmigrationbeitiefenTemperaturen ThisEuropeanStandardwasapprovedbyCENo
10、n4January2002. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagement
11、CentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandards
12、bodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruede
13、Stassart,36B1050Brussels 2002CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN118612:2002EEN118612:2002(E) 2 Contents page Foreword3 1 Scope 5 2 Normativereferences 5 3 Overallmigrationintodewaxedsunfloweroilbytotalimmersion.5 4 Overallmigrationintod
14、ewaxedsunfloweroilbycell 8 5 Overallmigrationintodewaxedsunfloweroilusingapouch.11 6 Overallmigrationintodewaxedsunfloweroilbyarticlefilling. 14 AnnexZA (informative) RelationshipofthisEuropeanStandardwithCouncilDirective89/109/EEC andCommissionDirective90/128/EECandassociatedDirectives17 Bibliograp
15、hy 19EN118612:2002(E) 3 Foreword ThisdocumentEN118612:2002hasbeenpreparedbyTechnicalCommitteeCEN/TC194“Utensilsincontact withfood“,thesecretariatofwhichisheldbyBSI. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationofanidenticaltextor byendorsement,atthelatestbyOctober2
16、002,andconflictingnationalstandardsshallbewithdrawnatthelatest byOctober2002. ThisdocumentsupersedesENV118612:1995. ThisEuropeanStandardisoneofaseriesofmethodsoftestforplasticsmaterialsandarticlesincontactwith foodstuffs. ThisdocumenthasbeenpreparedunderamandategiventoCENbytheEuropeanCommissionandth
17、eEuropean FreeTradeAssociation,andsupportsessentialrequirementsofECDirective(s). ForrelationshipwithECDirective(s),seeinformativeannexZA,whichisanintegralpartofthisdocument. AtthetimeofpreparationandpublicationofthisstandardtheEuropeanUnionlegislationrelatingtoplastics materialsandarticlesintendedto
18、comeintocontactwithfoodstuffsisincomplete.FurtherDirectivesand amendmentstoexistingDirectivesareexpectedwhichcouldchangethelegislativerequirementswhichthis standardsupports.Itisthereforestronglyrecommendedthatusersofthisstandardrefertothelatestrelevant publishedDirective(s)beforecommencementofanyoft
19、hetestortestsdescribedinthisstandard. EN118612shouldbereadinconjunctionwithEN11861,EN11862,EN11864,EN11866andEN11868. FurtherPartsofthisstandardhavebeenpreparedconcernedwiththedeterminationofoverallmigrationfrom plasticsmaterialsintofoodsimulants. Theirtitlesareasfollows: EN1186Materialsandarticlesi
20、ncontactwithfoodstuffsPlastics Part1 Guidetotheselectionofconditionsandtestmethodsforoverallmigration Part2 Testmethodsforoverallmigrationintooliveoilbytotalimmersion Part3 Testmethodsforoverallmigrationintoaqueousfoodsimulantsbytotalimmersion Part4 Testmethodsforoverallmigrationintooliveoilbycell P
21、art5 Testmethodsforoverallmigrationintoaqueousfoodsimulantsbycell Part6 Testmethodsforoverallmigrationintooliveoilusingapouch Part7 Testmethodsforoverallmigrationintoaqueousfoodsimulantsusingapouch Part8 Testmethodsforoverallmigrationintooliveoilbyarticlefilling Part9 Testmethodsforoverallmigrationi
22、ntoaqueousfoodsimulantsbyarticlefilling Part10 Testmethodsforoverallmigrationintooliveoil(modifiedmethodforuseincaseswhere incompleteextractionofdewaxedsunfloweroiloccurs)EN118612:2002(E) 4 Part11 Testmethodsforoverallmigrationintomixturesof 14 Clabelledsynthetictriglyceride Part13 Testmethodsforove
23、rallmigrationathightemperatures Part14 Testmethodsforsubstitutetestsforoverallmigrationfromplasticsintendedtocomeinto contactwithfattyfoodstuffsusingtestmediaisooctaneand95%ethanol Part15 Alternativetestmethodstomigrationintofattyfoodsimulantsbyrapidextractionintoiso octaneand/or95%ethanol According
24、totheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain, Sweden,Switzerlandandthe
25、UnitedKingdom.EN118612:2002(E) 5 1Scope ThisPartofthisEuropeanStandardspecifiestestmethodsforthedeterminationoftheoverallmigrationintofatty foodsimulantsfromplasticsmaterialsandarticles,bytotalimmersionoftestspecimensinafattyfoodsimulantat temperaturesfrom5 C,uptoandincluding20 C,forselectedtimes. T
26、hismethodismostsuitableforplasticsintheformoffilmsandsheets,butcanbeappliedtoawiderangeof articlesorcontainersfromwhichtestpiecesofasuitablesizecanbecut. Thefattyfoodsimulantusedinthesetestmethodsisdewaxedsunfloweroilsince,unlikeoliveoil,remainsliquidat thelowertesttemperature. Thetestmethoddescribe
27、disapplicabletomosttypesofplastics,althoughtherearesomeplasticsforwhichitis knownnottobeapplicable. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedandundatedreference,provisionsfromotherpublications.These normativereferencesarecitedattheappropriateplacesinthetext,andthepublicationsarel
28、istedhereafter.For datedreferences,subsequentamendmentstoandrevisionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthelatesteditionofthe publicationreferredtoapplies(includingamendments). EN11861:2002, Materialsandarticlesincont
29、actwithfoodPlasticsPart1:Guidetotheselectionofconditions andtestmethodsforoverallmigration. EN11862:2002, MaterialsandarticlesincontactwithfoodPlasticsPart2:Testmethodsforoverallmigration intooliveoilbytotalimmersion. EN11864:2002, MaterialsandarticlesincontactwithfoodPlasticsPart4:Testmethodsforove
30、rallmigration intooliveoilbycell. EN11866:2002, MaterialsandarticlesincontactwithfoodPlasticsPart6:Testmethodsforoverallmigration intooliveoilusingapouch. EN11868:2002, MaterialsandarticlesincontactwithfoodPlasticsPart8:Testmethodsforoverallmigration intooliveoilbyarticlefilling. 3 Overallmigrationi
31、ntodewaxedsunfloweroilbytotalimmersion 3.1Principle Theoverallmigrationfromasampleoftheplasticsisdeterminedasthelossinmassperunitofsurfacearea intendedtocomeintocontactwithfoodstuffs. Theselectionoftheconditionsoftestwillbedeterminedbytheconditionsofuse,seeclauses4,5and6ofEN 11861:2002. Testspecimen
32、sofknownmassareimmersedindewaxedsunfloweroilfortheexposuretime,attemperaturesfrom 5 Cuptoandincluding20 C,thentakenfromthedewaxedsunfloweroil,blottedtoremoveoiladheringtothe surface,andreweighed.EN118612:2002(E) 6 Thespecimenscanusuallyretainabsorbeddewaxedsunfloweroilthatisextractedanddeterminedqua
33、ntitatively bymeansofgaschromatographyafterconversiontomethylesters.Methylationiscarriedoutbyreactingaboron trifluoride/methanolcomplexwithfattyacidsformedbyhydrolysingtheoilwithpotassiumhydroxide.Aninternal standard,triheptadecanoin,isaddedpriortotheextractionoftheabsorbeddewaxedsunfloweroilfromthe
34、test specimens.Thisensuresthatanyactiveorextractablecomponentsoftheplasticsreactwiththeinternalstandard, aswellaswiththeextracteddewaxedsunfloweroil.Theinternalstandardisalsosubjectedtothehydrolysisand methylationreactions,providingcompensationforanyinefficienciesinthehydrolysisandmethylationprocess
35、es. Migrationintothedewaxedsunfloweroiliscalculatedbysubtractingthemassofdewaxedsunfloweroilretainedby thetestspecimenfromthemassofthetestspecimenafterremovalfromthedewaxedsunfloweroil,then subtractingthismassfromtheinitialmassofthespecimen. Thetotallossinmassisexpressedinmilligramspersquaredecimetr
36、eofsurfaceareaofthespecimenandthe overallmigrationisreportedasthemeanofaminimumofthreedeterminationsonseparatetestspecimens. Toallowforinaccuracieswhichmayariseduringtheprocedureandwhichmaybedifficulttodetect,duefor exampletocontaminationorlossofoilduringthesamplehandlingstages,fourdeterminationsare
37、carriedouton thesampleallowingfortheresultfromonespecimentobediscarded. Thismethodincludesvariationsthatareapplicabletocertainplastics. NOTE Beforestartingamigrationexercise,thetestsampleshouldbeexaminedforthepresenceofcomponentsinterfering inthedeterminationoftheamountofdewaxedsunfloweroilextracted
38、,see7.1ofEN11862:2002.Ifanunacceptableamount ofinterferenceispresentthensuitabilityofoneoftheotherfattyfoodsimulantsshouldbeexamined,seeannexAofEN11 86 2:2002and9.3and9.5ofEN11861:2002.Ifaninterferenceispresentwhichwouldinterferewiththetriheptadecanoinintern al standardanalternativeinternalstandards
39、houldbeused,seeannexAofEN11862:2002,and9.3ofEN11861:2002. 3.2Reagents Thereagentsshallbeasdescribedinclause4ofEN11862:2002,exceptthatoliveoil,referencesimulantD,as specifiedin4.1ofEN11861:2002isreplacedbydewaxedsunfloweroil,simulantD. 3.3Apparatus Theapparatusshallbeasdescribedinclause5ofEN11862:200
40、2. 3.4 Preparationoftestspecimens Thetestspecimensshallbepreparedasdescribedinclause6ofEN11862:2002. 3.5Procedure 3.5.1General DeterminetheapplicabilityofthemethodbycarryingouttheproceduredescribedinannexAofEN11862:2002. IfpriortestshaveestablishedthatthemethodisapplicablethenannexAofEN11862:2002may
41、beomitted. Beforeweighing,dischargeanybuildupofstaticelectricitywithanantistaticgunorothersuitablemeans. 3.5.2 Initialweighingoftestspecimens Performtheinitialweighinginaccordancewith7.2ofEN11862:2002.EN118612:2002(E) 7 3.5.3 Exposuretofoodsimulant Takesixoftheglasstubes(5.11ofEN11862:2002),markthem
42、foridentificationpurposes.Measure 100ml 5mlofdewaxedsunfloweroil(4.1ofEN11862:2002,see3.2)intoeachtubebymeasuringcylinderand stopperthetube. NOTE.1 IftheproceduredescribedinannexDofEN11862:2002isused,itcanbenecessarytodryallofthedewaxed sunfloweroilusedforthemigrationtest,seeD.3.2.ofEN11862:2002. Al
43、ternativelymarkthetubesforavolumeof100mlandfillwithdewaxedsunfloweroiltothemark.Placeintoone ofthetubesathermometerorthermocoupleandstopperthetubes.Twoextratubeswithaminimumof50mlof dewaxedsunfloweroilarerequiredasblanksimulant,iftheproceduredescribedinannexDofEN11862:2002is used.Placethesixoreighttubes,andtwoemptytubes,inthethermostaticallycontrolledovenorincubator(5.12 ofEN11862:2002)setatthetesttemperature.Leaveuntilthedewaxedsunfloweroilhasattainedthet
