1、BRITISH STANDARD BS EN 1186-13:2002 Materials and articles in contact with foodstuffs Plastics Part 13: Test methods for overall migration at high temperatures The European Standard EN 1186-13:2002 has the status of a British Standard ICS 67.250 BS EN 1186-13:2002 This British Standard, having been
2、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 40569 9 National foreword This British Standard is the official
3、English language version of EN 1186-13:2002. It supersedes DD ENV 1186-13:1999 which is withdrawn.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 from plastics, which has the re
4、sponsibility 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 Catalogue under the section entitl
5、ed “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 correct application. Compliance
6、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 informed; monitor related inter
7、national 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 18, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates when the document was
8、last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN118613 September2002 ICS67.250 Englishversion MaterialsandarticlesincontactwithfoodstuffsPlasticsPart 13:Testmethodsforoverallmigrationathightemperatures Matriauxetobjetsencontacta
9、veclesdenres alimentairesMatireplastiquePartie13:Mthodes dessaipourlamigrationglobalehautestempratures WerkstoffeundGegenstndeinKontaktmitLebensmitteln KunststoffeTeil13:Prfverfahrenfrdie GesamtmigrationbeihohenTemperaturen ThisEuropeanStandardwasapprovedbyCENon29April2002. CENmembersareboundtocompl
10、ywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStan
11、dardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,De
12、nmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2002CEN Allrigh
13、tsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN118613:2002EEN118613:2002(E) 2 Contents page Foreword3 Introduction .4 1 Scope 4 2 Normativereferences 5 3 MethodAtotalimmersioninoliveoil. .5 4 MethodBadsorptionbymodifiedpolyphenyleneoxide 8 4.1 Principle8 4.2
14、Reagents.8 4.3 Apparatus .9 4.4 Samplepreparation .9 4.5 Procedure .10 4.6 Expressionofresults . .12 4.7 Testreport . .13 AnnexA (informative) Aluminiumblock . 14 AnnexB (informative) Precisiondata 15 AnnexZA (informative) RelationshipofthisEuropeanStandardwithCouncilDirective89/109/EECand Commissio
15、nDirective90/128/EECandassociatedDirectives .16 Bibliography 18EN118613:2002(E) 3 Foreword ThisdocumentEN118613:2002hasbeenpreparedbyTechnicalCommitteeCEN/TC194“Utensilsincontact withfood”,thesecretariatofwhichisheldbyBSI. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicat
16、ionofanidenticaltextor byendorsement,atthelatestbyMarch2003,andconflictingnationalstandardsshallbewithdrawnatthelatestby March2003. ThisdocumentsupersedesENV118613:1999. ThisEuropeanStandardhasbeenpreparedasoneofaseriesofmethodsoftestforplasticsmaterialsandarticles incontactwithfoodstuffs. Thisdocum
17、enthasbeenpreparedunderamandategiventoCENbytheEuropeanCommissionandtheEuropean FreeTradeAssociation. ForrelationshipwithEUDirective(s),seeinformativeannexZA,whichisanintegralpartofthisdocument. AtthetimeofpreparationandpublicationofthisstandardtheEuropeanUnionlegislationrelatingtoplastics materialsa
18、ndarticlesintendedtocomeintocontactwithfoodstuffsisincomplete.FurtherDirectivesand amendmentstoexistingDirectivesareexpectedwhichcouldchangethelegislativerequirementswhichthis standardsupports.Itisthereforestronglyrecommendedthatusersofthisstandardrefertothelatestrelevant publishedDirective(s)before
19、commencementofanyofthetestortestsdescribedinthisstandard. EN118613MethodAandMethodBshouldbereadinconjunctionwithEN11861.Also,EN118613MethodA shouldbereadinconjunctionwithEN11862. FurtherPartsofthisstandardhavebeenpreparedconcernedwiththedeterminationofoverallmigrationfrom plasticsmaterialsintofoodsi
20、mulants.Theirtitlesareasfollows: EN1186MaterialsandarticlesincontactwithfoodstuffsPlastics Part1 Guidetotheselectionofconditionsandtestmethodsforoverallmigration Part2 Testmethodsforoverallmigrationintooliveoilbytotalimmersion Part3 Testmethodsforoverallmigrationintoaqueousfoodsimulantsbytotalimmers
21、ion Part4 Testmethodsforoverallmigrationintooliveoilbycell Part5 Testmethodsforoverallmigrationintoaqueousfoodsimulantsbycell Part6 Testmethodsforoverallmigrationintooliveoilusingapouch Part7 Testmethodsforoverallmigrationintoaqueousfoodsimulantsusingapouch Part8 Testmethodsforoverallmigrationintool
22、iveoilbyarticlefilling Part9 Testmethodsforoverallmigrationintoaqueousfoodsimulantsbyarticlefilling Part10 Testmethodsforoverallmigrationintooliveoil(modifiedmethodforuseincaseswhere incompleteextractionofoliveoiloccurs) Part11 Testmethodsforoverallmigrationintomixturesof 14 Clabelledsynthetictrigly
23、ceride Part12 Testmethodsforoverallmigrationatlowtemperatures Part14 Testmethodsforsubstitutetestsforoverallmigrationfromplasticsintendedtocomeinto contactwithfattyfoodstuffsusingtestmediaisooctaneand95%ethanolEN118613:2002(E) 4 Part15 Alternativetestmethodstomigrationintofattyfoodsimulantsbyrapidex
24、tractionintoiso octaneand/or95%ethanol TheannexesAandBareinformative. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Iceland,Ireland,Ita
25、ly,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain, Sweden,SwitzerlandandtheUnitedKingdom. Introduction Migrationtestingwitholiveoilathightemperaturesintroducesanumberofanalyticaldifficulties.Experiencehas shownthatitisdifficulttoachievereproducibleresultsowingtodifferentlaboratorieshavingdiffere
26、ntequipment whichgiverisetovariationsinthetimetakentoreachtheexposuretemperature.Amethodisdescribedfor determiningoverallmigrationbytotalimmersionusinganaluminiumblockwithaconsistentthermalcapacity. Otheranalyticaldifficultieswitholiveoilincludepossibleoxidationofoilatelevatedtemperaturesandthehazar
27、dto personnelworkingwithhotoil.Replacementofoliveoilbyanappropriateadsorbentmaterial,inprincipal,cansolve orreducetheseproblemsandoffersfurtherexperimentaladvantages. 1Scope ThisEuropeanStandardspecifiestestmethodsforthedeterminationoftheoverallmigrationintofattyfood simulantsfromplasticsmaterialsan
28、darticles,bytotalimmersionoftestspecimensinafattyfoodsimulantat temperaturesfrom100 Cuptoandincluding,175 Cforselectedtimes.Alsodescribedisaprocedurewitha substitutetestmedium.Inthissubstituteprocedurethemassofcomponentsadsorbedonmodifiedpolyphenylene oxide(MPPO)istakenasameasurefortheassessmentofth
29、eoverallmigrationintooliveoil. NOTE1 Thetotalimmersiontestmethodhasbeenwrittenforusewiththefattyfoodsimulant,oliveoil.Thetestmethodcan alsobeusedwithappropriatemodificationswithotherfattyfoodsimulantscalledsimulantDasyntheticmixtureof triglycerides,sunfloweroilandcornoil.Theseotherfattyfoodsimulants
30、producedifferentchromatogramsforthesimulant methylesterstothoseofthemethylestersofoliveoil.Suitablechromatogrampeaksofthemethylestersoftheotherfatty food simulantsshouldbeselectedforthequantitativedeterminationofthesimulantextractedfromthetestspecimens. NOTE2 Acomparativemigrationtestcarriedoutwithp
31、olypropyleneandpolyethyleneterephthalatehightemperature applicationcontainersastestsamplesatconditions2hat100 Cand2hat175 C,respectively,incontactwith 14 Clabelled synthetictriglycerideandMPPOprovidedtestresultscomparablewithintheanalyticaltoleranceofthemethods. NOTE3 Toobtainreproducibleandrepeatab
32、leresultsusingtheMPPOmethoditmaybenecessarytomeasurethe temperatureofthetestspecimenbeforestartingthemigrationperiod.Anappropriatemethodformeasuringthetemperatureof thetestspecimenneedstobeestablished. Thedescribedmethodsaremostsuitableforfoodcontactarticlesintheformofsheetsandfilms,butcanalsobe app
33、liedtoawiderangeofarticlesandcontainers.EN118613:2002(E) 5 2 Normativereferences ThisEuropeanStandardincorporatesbydatedandundatedreference,provisionsfromotherpublications.These normativereferencesarecitedattheappropriateplacesinthetext,andthepublicationsarelistedhereafter.For datedreferences,subseq
34、uentamendmentstoandrevisionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthelatesteditionofthe publicationreferredtoapplies,includingamendments(includingamendments). EN11861:2002, MaterialsandarticlesincontactwithfoodstuffsPlas
35、ticsPart1:Guidetotheselectionof conditionsandtestmethodsforoverallmigration. EN11862:2002, MaterialsandarticlesincontactwithfoodstuffsPlasticsPart2:Testmethodsforoverall migrationintooliveoilbytotalimmersion. 3 MethodAtotalimmersioninoliveoil 3.1Principle Theoverallmigrationfromasampleoftheplasticsi
36、sdeterminedasthelossinmassperunitofsurfacearea intendedtocomeintocontactwithfoodstuffs. Theselectionoftheconditionsoftestwillbedeterminedbytheconditionsofuse,seeclauses4,5and6of EN11861:2002. Testspecimensofknownmassareimmersedinoliveoilfortheexposuretime,attemperaturesfrom100 Cupto 175 C,thentakenf
37、romtheoliveoil,blottedtoremoveoiladheringtothesurface,andreweighed. Thespecimensusuallyretainabsorbedoliveoilwhichisextractedanddeterminedquantitativelybymeansofgas chromatographyafterconversiontomethylesters.Methylationiscarriedoutbyreactingaboron trifluoride/methanolcomplexwithfattyacidsformedbyhy
38、drolysingtheoilwithpotassiumhydroxide.Aninternal standard,triheptadecanoin,isaddedpriortotheextractionoftheabsorbedoliveoilfromthetestspecimens.This ensuresthatanyactiveorextractablecomponentsoftheplasticsreactwiththeinternalstandard,aswellaswith theextractedoliveoil.Theinternalstandardisalsosubject
39、edtothehydrolysisandmethylationreactions,providing compensationforanyinefficienciesinthehydrolysisandmethylationprocesses. Migrationintotheoliveoiliscalculatedbysubtractingthemassofoliveoilretainedbythetestspecimenfromthe massofthetestspecimenafterremovalfromtheoliveoil,thensubtractingthismassfromth
40、einitialmassofthe specimen. Thetotallossinmassisexpressedinmilligramspersquaredecimetreofsurfaceareaofthespecimenandthe overallmigrationisreportedasthemeanofaminimumofthreedeterminationsonseparatetestspecimens. Toallowforinaccuracieswhichmayariseduringtheprocedureandwhichmaybedifficulttodetect,duefo
41、r exampletocontaminationorlossofoilduringthesamplehandlingstages,fourdeterminationsarecarriedouton thesampleallowingfortheresultfromonespecimentobediscarded. Thismethodincludesvariationswhichareapplicabletocertainplastics. NOTE Beforestartingamigrationexercise,thetestsampleshouldbeexaminedforthepres
42、enceofcomponentsinterfering inthedeterminationoftheamountofoliveoilextracted,see9.3ofEN11861:2002.Ifanunacceptableamountofinterference ispresentthensuitabilityofoneoftheotherfattyfoodsimulantsshouldbeexamined,seeannexAand9.3and9.5ofEN 11861:2002.Ifaninterferenceispresentwhichwouldinterferewiththetri
43、heptadecanoininternalstandardanalternative internalstandardshouldbeused,seeannexA,and9.3ofEN11861:2002. 3.2Reagents Thereagentsshallbeasdescribedinclause4ofEN11862:2002.EN118613:2002(E) 6 3.3Apparatus Theapparatusshallbeasdescribedinclause5ofEN11862:2002,withtheadditionof: Aluminiumblockorblockswithwellsforholdinguptotenglasstubes,see5.11ofEN11862:2002,duringthe exposuretimeperiodintheovenorincubator. NOTE AdiagramofasuitableblockisshowninFigureA.1
