1、BRITISH STANDARD BS EN 1186-4:2002 Materials and articles in contact with foodstuffs Plastics Part 4: Test methods for overall migration into olive oil by cell The European Standard EN 1186-4:2002 has the status of a British Standard ICS 67.250 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED B
2、Y COPYRIGHT LAWBS EN 1186-4:2002 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 3975
3、3 X National foreword This British Standard is the official English language version of EN 1186-4:2002. It supersedes DD ENV 1186-4:1994 which is withdrawn.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, Mi
4、gration 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
5、 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 res
6、ponsible 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 inte
7、rests 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 31 and a back cover. The BSI copyright date displayed in this document indicates when th
8、e document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN11864 April2002 ICS67.250 SupercedesENV11864:1994 Englishversion MaterialsandarticlesincontactwithfoodstuffsPlasticsPart 4:Testmethodsforoverallmigrationintooliveoil
9、bycell Matriauxetobjetsencontactaveclesdenres alimentairesMatireplastiquePartie4:Mthodes dessaipourlamigrationglobaledanslhuiledoliveen cellule WerkstoffeundGegenstndeinKontaktmitLebensmitteln KunststoffeTeil4:Prfverfahrenfrdie GesamtmigrationinOlivenlmittelsZelle ThisEuropeanStandardwasapprovedbyCE
10、Non4January2002. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManageme
11、ntCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandar
12、dsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:rue
13、deStassart,36B1050Brussels 2002CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN11864:2002EEN11864:2002(E) 2 Contents page Foreword3 1 Scope 5 2 Normativereferences 5 3 Principle5 4 Reagents.6 5 Apparatus .7 6 Preparationoftestspecimens. .9 7 Procedu
14、re .9 8 Expressionofresults . .16 9 Testreport . .17 AnnexA (normative) Determinationofthesuitabilityofoliveoilasthefattyfoodsimulantandof triheptadecanoinastheinternalstandard 18 AnnexB (normative) Determinationoftheneedforsampleconditioning.20 AnnexC (normative) Determinationoftheneedforsamplecond
15、itioninganddeterminationofthe massofmoisturesensitivetestspecimens,byvacuumdrying.21 AnnexD (normative) Determinationofchangeinmoisturecontentoftestspecimensbymeasurement ofthetransferofwaterto,orfromoliveoil,byKarlFischertitration23 AnnexE (informative) Typicalchromatogramsandcalibrationgraph.25 An
16、nexF (informative) Precisiondata .28 AnnexZA (informative) RelationshipofthisEuropeanStandardwithCouncilDirective89/109/EEC andCommissionDirective90/128/EECandassociatedDirectives29 Bibliography 31EN11864:2002(E) 3 Foreword ThisdocumentEN11864:2002hasbeenpreparedbyTechnicalCommitteeCEN/TC194“Utensil
17、sincontactwith food”,thesecretariatofwhichisheldbyBSI. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationofanidenticaltextor byendorsement,atthelatestbyOctober2002,andconflictingnationalstandardsshallbewithdrawnatthelatest byOctober2002. ThisdocumentsupersedesENV11864:1
18、994. ThisEuropeanStandardisoneofaseriesofmethodsoftestforplasticsmaterialsandarticlesincontactwith foodstuffs. ThisdocumenthasbeenpreparedunderamandategiventoCENbytheEuropeanCommissionandtheEuropean FreeTradeAssociation,andsupportsessentialrequirementsofECDirective(s). ForrelationshipwithECDirective
19、s),seeinformativeannexZA,whichisanintegralpartofthisdocument. AtthetimeofpreparationandpublicationofthisstandardtheEuropeanUnionlegislationrelatingtoplastics materialsandarticlesintendedtocomeintocontactwithfoodstuffsisincomplete.FurtherDirectivesand amendmentstoexistingDirectivesareexpectedwhichco
20、uldchangethelegislativerequirementswhichthis standardsupports.Itisthereforestronglyrecommendedthatusersofthisstandardrefertothelatestrelevant publishedDirective(s)beforecommencementofanyofthetestortestsdescribedinthisstandard. EN11864shouldbereadinconjunctionwithEN11861. FurtherPartsofthisstandardha
21、vebeenpreparedconcernedwiththedeterminationofoverallmigrationfrom plasticsmaterialsintofoodsimulants.Theirtitlesareasfollows: EN1186MaterialsandarticlesincontactwithfoodstuffsPlastics Part1 Guidetotheselectionofconditionsandtestmethodsforoverallmigration Part2 Testmethodsforoverallmigrationintoolive
22、oilbytotalimmersion Part3 Testmethodsforoverallmigrationintoaqueousfoodsimulantsbytotalimmersion Part5 Testmethodsforoverallmigrationintoaqueousfoodsimulantsbycell Part6 Testmethodsforoverallmigrationintooliveoilusingapouch Part7 Testmethodsforoverallmigrationintoaqueousfoodsimulantsusingapouch Part
23、8 Testmethodsforoverallmigrationintooliveoilbyarticlefilling Part9 Testmethodsforoverallmigrationintoaqueousfoodsimulantsbyarticlefilling Part10 Testmethodsforoverallmigrationintooliveoil(modifiedmethodforuseincaseswhere incompleteextractionofoliveoiloccurs) Part11 Testmethodsforoverallmigrationinto
24、mixturesof 14 Clabelledsynthetictriglyceride Part12 TestmethodsforoverallmigrationatlowtemperaturesEN11864:2002(E) 4 Part13 Testmethodsforoverallmigrationathightemperatures Part14 Testmethodsforsubstitutetestsforoverallmigrationfromplasticsintendedtocomeinto contactwithfattyfoodstuffsusingtestmediai
25、sooctaneand95%ethanol Part15 Alternativetestmethodstomigrationintofattyfoodsimulantsbyrapidextractionintoiso octaneand/or95%ethanol AnnexesA,B,CandDtothisstandardarenormativewhereapplicable.TheannexesEandFareinformative. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationso
26、fthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain, Sweden,SwitzerlandandtheUnitedKingdom.EN11864:2002(E) 5 1Scope ThisPartofthisEuropeanStandards
27、pecifiestestmethodsforthedeterminationoftheoverallmigrationintofatty foodsimulants,fromonesurfaceonlyofplasticsintheformofsheetandfilmattemperaturesabove20 Candup to,butnotincluding,100 Cforselectedtimes. Thismethodismostsuitableforplasticsintheformoffilmsandsheets,butisparticularlyapplicabletothose
28、 materialsconsistingofmorethanonelayerorsurfacesthatdifferintheirmigrationcharacteristics,whichhaveto betestedwithfoodsimulantincontactwiththesurfacewhichisintendedtocomeintocontactwithfoodstuffs. NOTE Thistestmethodhasbeenwrittenforusewiththefattyfoodsimulant,oliveoil.Thetestmethodcanalsobeused wit
29、happropriatemodificationswithotherfattyfoodsimulantscalledsimulantDasyntheticmixtureoftriglycerides,sun flower oilandcornoil.Theseotherfattyfoodsimulantswillproducedifferentchromatogramsforthesimulantmethylesterstothos eof themethylestersofoliveoil.Selectsuitablechromatogrampeaksofthemethylestersoft
30、heotherfattyfoodsimulantsfor the quantitativedeterminationofthesimulantextractedfromthetestspecimens. Thetestmethoddescribedisapplicabletomosttypesofplastics,althoughtherearesomeplasticsforwhichitis knownnottobeapplicable. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedandundatedrefere
31、nce,provisionsfromotherpublications.These normativereferencesarecitedattheappropriateplacesinthetext,andthepublicationsarelistedhereafter.For datedreferences,subsequentamendmentstoandrevisionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundated
32、referencesthelatesteditionofthe publicationreferredtoapplies(includingamendments). EN11861:2002, MaterialsandarticlesincontactwithfoodstuffsPlasticsPart1:Guidetotheselectionof conditionsandtestmethodsforoverallmigration. ISO648, LaboratoryglasswareOnemarkpipettes. ISO4788, LaboratoryglasswareGraduat
33、edmeasuringcylinders. 3Principle Theoverallmigrationfromasampleoftheplasticsisdeterminedasthelossinmassperunitofsurfacearea intendedtocomeintocontactwithfoodstuffs. Theselectionoftheconditionsoftestwillbedeterminedbytheconditionsofuse,seeclauses4,5and6of EN11861:2002. Testspecimensofknownmassareexpo
34、sedinacelltooliveoilfortheexposuretime,attemperaturesabove 20 Candbelow100 C,thentakenfromthecell,blottedtoremoveoiladheringtothesurface,andreweighed. Thespecimenswillusuallyretainabsorbedoliveoilthatextractedanddeterminedquantitativelybymeansofgas chromatographyafterconversiontomethylesters.Methyla
35、tioniscarriedoutbyreactingaboron trifluoride/methanolcomplexwithfattyacidsformedbyhydrolysingtheoilwithpotassiumhydroxide.Aninternal standard,triheptadecanoin,isaddedpriortotheextractionoftheabsorbedoliveoilfromthetestspecimens.This ensuresthatanyactiveorextractablecomponentsoftheplasticsreactwithth
36、einternalstandard,aswellaswith theextractedoliveoil.Theinternalstandardisalsosubjectedtothehydrolysisandmethylationreactions,providing compensationforanyinefficienciesinthehydrolysisandmethylationprocesses. Migrationintotheoliveoiliscalculatedbysubtractingthemassofoliveoilretainedbythetestspecimenfr
37、omtheEN11864:2002(E) 6 massofthetestspecimenafterremovalfromtheoliveoil,thensubtractingthismassfromtheinitialmassofthe specimen. Thetotallossinmassisexpressedinmilligramspersquaredecimetreofsurfaceareaofthespecimenandthe overallmigrationisreportedasthemeanofaminimumofthreedeterminationsonseparatetes
38、tspecimens. Toallowforinaccuracieswhichmayariseduringtheprocedureandwhichmaybedifficulttodetect,duefor exampletocontaminationorlossofoilduringthesamplehandlingstages,fourdeterminationsarecarriedouton thesampleallowingfortheresultfromonespecimentobediscarded. Thismethodincludesvariationsthatapplicabl
39、etocertainplastics. NOTE Beforestartingamigrationexercise,thetestsampleshouldbeexaminedforthepresenceofcomponentsinterfering inthedeterminationoftheamountofoliveoilextracted,see7.1.Ifanunacceptableamountofinterferenceispresentthen suitabilityofoneoftheotherfattyfoodsimulantsshouldbeexamined,seeannex
40、Aand9.3and9.5ofEN11861:2002.Ifa n interferenceispresentwhichwouldinterferewiththetriheptadecanoininternalstandardanalternativeinternalstandardshou ld beused,seeannexA,and9.3ofEN11861:2002. 4Reagents NOTE Allreagentsshouldbeofrecognizedanalyticalquality,unlessotherwisespecified. 4.1 Oliveoil,referenc
41、esimulantD,asspecifiedin5.2ofEN11861:2002. 4.2 Extractionsolvent(see10.1ofEN11861:2002). 4.2.1 Fornonpolarplastics,suchaspolyethyleneandpolypropylene: Pentane98%boilingpoint36 C. Forpolarplastics,suchaspolyamideandpolyacetal: 95/5byvolumeazeotropicmixtureofpentane98%andethanol99%. NOTE1 Pentaneisave
42、ryvolatileandhighlyflammablesolvent.Careshouldthereforebetakenwhenhandlingthissolvent topreventcontactwithsourcesofignition.Ethanolisalsoaflammablesolvent.Itisnotrecommendedthatextractionswith eitherpentaneorthepentane/ethanolmixturebeleftunattended,particularlyovernight. NOTE2 Duetothelowboilingpoi
43、ntsofthesesolvents,cooledcondenserwatercanberequiredtopreventunduelossofthe solventfromthecondenser. or 4.2.2 Othersuitablesolvent. NOTE1 Inpreviousmethodsfordeterminingoverallmigrationintooliveoiltheextractionsolventusedhasbeen1,1,2 trichlorotrifluoroethane.Forenvironmentalreasonstheuseofthissolventshouldbeavoidedwherepossible,see9.1ofEN 11861:2002.Experiencehasshownthatthissolvent,althougheffectiveformostplasticsrequireslongerperiodsofextractio n. NOTE2 Somesolventscancontainnonvolatilesubstanceswhich,afterhydr
