BS EN 1186-4-2002 Materials and articles in contact with foodstuffs - Plastics - Test methods for overall migration into olive oil by cell《与食品接触的材料和器具 塑料 用电解槽浸渍在橄榄油中的全迁移量的试验方法》.pdf

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 It supersedes DD ENV 1186-4:1994 which is withdrawn.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