1、BRITISH STANDARD BS EN 1186-6:2002 Materials and articles in contact with foodstuffs Plastics Part 6: Test methods for overall migration into olive oil using a pouch The European Standard EN 1186-6:2002 has the status of a British Standard ICS 67.250 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMI
2、TTED BY COPYRIGHT LAWBS EN 1186-6:2002 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 58
3、0 39752 1 National foreword This British Standard is the official English language version of EN 1186-6:2002. It supersedes DD ENV 1186-6:1994 which is withdrawn.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
4、/1, 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
5、in 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 a
6、re 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 U
7、K interests 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 33 and a back cover. The BSI copyright date displayed in this document indicates w
8、hen the document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN11866 April2002 ICS67.250 SupersedesENV11866:1994 Englishversion MaterialsandarticlesincontactwithfoodstuffsPlasticsPart 6:Testmethodsforoverallmigrationintool
9、iveoilusingapouch Matriauxetobjetsencontactaveclesdenres alimentairesMatireplastiquePartie6:Mthodes dessaipourlamigrationglobaledanslhuiledolivelaide dunsachet WerkstoffeundGegenstndeinKontaktmitLebensmitteln KunststoffeTeil6:Prfverfahrenfrdie GesamtmigrationinOlivenlunterVerwendungeines Beutels Thi
10、sEuropeanStandardwasapprovedbyCENon4January2002. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeob
11、tainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions.
12、 CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMIT
13、EEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2002CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN11866:2002EEN11866:2002(E) 2 Contents page Foreword3 1 Scope 5 2 Normativereferences 5 3 Principle5 4 Reagents.6 5 Apparatus .7 6 Preparat
14、ionoftestspecimens. .9 7 Procedure .10 8 Expressionofresults . .16 9 Testreport . .18 AnnexA (normative) Determinationofthesuitabilityofoliveoilasthefattyfoodsimulantandof triheptadecanoinastheinternalstandard 19 AnnexB (normative) Determinationoftheneedforsampleconditioning.21 AnnexC (normative) De
15、terminationoftheneedforsampleconditioninganddeterminationofthe massofmoisturesensitivetestspecimens,byvacuumdrying.22 AnnexD (normative) Determinationofchangeinmoisturecontentoftestspecimensbymeasurement ofthetransferofwaterto,orfromoliveoil,byKarlFischertitration24 AnnexE (informative) Pouchholder,
16、typicalchromatogramsandcalibrationgraph.26 AnnexF (informative) Precisiondata .30 AnnexZA (informative) RelationshipofthisEuropeanStandardwithCouncilDirective89/109/EEC andCommissionDirective90/128/EECandassociatedDirectives31 Bibliography 33EN11866:2002(E) 3 Foreword ThisdocumentEN11866:2002hasbeen
17、preparedbyTechnicalCommitteeCEN/TC194“Utensilsincontactwith food”,thesecretariatofwhichisheldbyBSI. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationofanidenticaltextor byendorsement,atthelatestbyOctober2002,andconflictingnationalstandardsshallbewithdrawnatthelatest by
18、October2002. ThisdocumentsupersedesENV11866:1994. ThisEuropeanStandardisoneofaseriesofmethodsoftestforplasticsmaterialsandarticlesincontactwith foodstuffs. ThisdocumenthasbeenpreparedunderamandategiventoCENbytheEuropeanCommissionandtheEuropean FreeTradeAssociation,andsupportsessentialrequirementsofE
19、CDirective(s). ForrelationshipwithECDirective(s),seeinformativeannexZA,whichisanintegralpartofthisdocument. AtthetimeofpreparationandpublicationofthisstandardtheEuropeanUnionlegislationrelatingtoplastics materialsandarticlesintendedtocomeintocontactwithfoodstuffsisincomplete.FurtherDirectivesand ame
20、ndmentstoexistingDirectivesareexpectedwhichcouldchangethelegislativerequirementswhichthis standardsupports.Itisthereforestronglyrecommendedthatusersofthisstandardrefertothelatestrelevant publishedDirective(s)beforecommencementofanyofthetestortestsdescribedinthisstandard. EN11866:2002shouldbereadinco
21、njunctionwithEN11861:2002. FurtherPartsofthisstandardhavebeenprepared,andothersareinpreparation,concernedwiththedetermination ofoverallmigrationfromplasticsmaterialsintofoodsimulants. Theirtitlesareasfollows: EN1186MaterialsandarticlesincontactwithfoodstuffsPlastics Part1 Guidetotheselectionofcondit
22、ionsandtestmethodsforoverallmigration Part2 Testmethodsforoverallmigrationintooliveoilbytotalimmersion Part3 Testmethodsforoverallmigrationintoaqueousfoodsimulantsbytotalimmersion Part4 Testmethodsforoverallmigrationintooliveoilbycell Part5 Testmethodsforoverallmigrationintoaqueousfoodsimulantsbycel
23、l Part7 Testmethodsforoverallmigrationintoaqueousfoodsimulantsusingapouch Part8 Testmethodsforoverallmigrationintooliveoilbyarticlefilling Part9 Testmethodsforoverallmigrationintoaqueousfoodsimulantsbyarticlefilling Part10 Testmethodsforoverallmigrationintooliveoil(modifiedmethodforuseincaseswhere i
24、ncompleteextractionofoliveoiloccurs) Part11 Testmethodsforoverallmigrationintomixturesof 14 ClabelledsynthetictriglycerideEN11866:2002(E) 4 Part12 Testmethodsforoverallmigrationatlowtemperatures Part13 Testmethodsforoverallmigrationathightemperatures Part14 Testmethodsforsubstitutetestsforoverallmig
25、rationfromplasticsintendedtocome into contactwithfattyfoodstuffsusingtestmediaisooctaneand95%ethanol Part15 Alternativetestmethodstomigrationintofattyfoodsimulantsbyrapidextractionintoiso octaneand/or95%ethanol AnnexesA,B,CandDtothisstandardarenormativewhereapplicable.AnnexesEandFareinformative. Acc
26、ordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain, Sweden,Switzerland
27、andtheUnitedKingdom.EN11866:2002(E) 5 1Scope ThisPartofthisEuropeanStandardspecifiestestmethodsforthedeterminationoftheoverallmigrationintofatty foodsimulantsfromonesurfaceonlyofplasticsintheformoffilmorsheet,whichisintendedtocomeintocontact withfoodstuffs,byformingtheplasticsfilmorsheetintostandard
28、pouchesandexposingthembyfillingat temperaturesabove20 Candupto,butnotincluding,100 Cforselectedtimes. Astandardpouchisapouchwithdimensionsasdefinedin6.3. Thismethodismostsuitableforplasticsintheformoffilmsandsheets,whicharesealablebyheatorpressure,but itisparticularlyapplicabletothosematerialsconsis
29、tingofmorethanonelayer,whichhastobetestedwiththefood simulantincontactonlywiththesurfacewhichisintendedtocomeintocontactwiththefoodstuffs. NOTE Thistestmethodhasbeenwrittenforusewiththefattyfoodsimulant,oliveoil.Thetestmethodcanalsobeused withappropriatemodificationswithotherfattyfoodsimulantscalled
30、simulantDasyntheticmixtureoftriglycerides,sun flower oilandcornoil.Theseotherfattyfoodsimulantswillproducedifferentchromatogramsforthesimulantmethylesterstothos eof themethylestersofoliveoil.Selectsuitablechromatogrampeaksofthemethylestersoftheotherfattyfoodsimulantsfor the quantitativedetermination
31、ofthesimulantextractedfromthetestspecimens. Thetestmethoddescribedisapplicabletomosttypesofplastics,althoughtherearesomeplasticsforwhichitis knownnottobeapplicable. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedandundatedreference,provisionsfromotherpublications.These normativereferen
32、cesarecitedattheappropriateplacesinthetext,andthepublicationsarelistedhereafter.For datedreferences,subsequentamendmentstoandrevisionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthelatesteditionofthe publicationreferredtoappli
33、es(includingamendments). EN11861:2002, MaterialsandarticlesincontactwithfoodPlasticsPart1:Guidetotheselectionofconditions andtestmethodsforoverallmigration. ISO648, LaboratoryglasswareOnemarkpipettes . ISO4788, LaboratoryglasswareGraduatedmeasuringcylinders. 3Principle Theoverallmigrationfromasample
34、oftheplasticsisdeterminedasthelossinmassperunitofsurfacearea intendedtocomeintocontactwithfoodstuffs. Theselectionoftheconditionsoftestwillbedeterminedbytheconditionsofuse,seeclauses4,5and6ofEN 11861:2002. Testspecimensofknownmassandintheformofpouchesarefilledwitholiveoilfortheexposuretime,at temper
35、aturesabove20 Candbelow100 C,thentheoliveoilisremoved,thepouchescutopenandtheoliveoil adheringtothesurfaceisremovedbyblotting.Thecutportionofeachpouchisthenreweighed, Thespecimenswillusuallyretainabsorbedoliveoilwhichisextractedanddeterminedquantitativelybymeansof gaschromatographyafterconversiontom
36、ethylesters.Methylationiscarriedoutbyreactingaboron trifluoride/methanolcomplexwithfattyacidsformedbyhydrolysingtheoilwithpotassiumhydroxide.Aninternal standard,triheptadecanoin,isaddedpriortotheextractionoftheabsorbedoliveoilfromthetestspecimens.This ensuresthatanyactiveorextractablecomponentsofthe
37、plasticsreactwiththeinternalstandard,aswellaswithEN11866:2002(E) 6 theextractedoliveoil.Theinternalstandardisalsosubjectedtothehydrolysisandmethylationreactions,providing compensationforanyinefficienciesinthehydrolysisandmethylationprocesses. Migrationintotheoliveoiliscalculatedbysubtractingthemasso
38、foliveoilretainedbythetestspecimenfromthe massofthetestspecimenafterremovalfromtheoliveoil,thensubtractingthismassfromtheinitialmassofthe specimen. Thetotallossinmassisexpressedinmilligramspersquaredecimetreofsurfaceareaofthespecimenandthe overallmigrationisreportedasthemeanofaminimumofthreedetermin
39、ationsonseparatetestspecimens. Toallowforinaccuracieswhichmayariseduringtheprocedureandwhichmaybedifficulttodetect,duefor exampletocontaminationorlossofoilduringthesamplehandlingstages,fourdeterminationsarecarriedouton thesampleallowingfortheresultfromonespecimentobediscarded. Thismethodincludesvari
40、ationsthatareapplicabletocertainplastics. NOTE Beforestartingamigrationexercise,thetestsampleshouldbeexaminedforthepresenceofcomponentsinterfering inthedeterminationoftheamountofoliveoilextracted,see7.1.Ifanunacceptableamountofinterferenceispresentthen suitabilityofoneoftheotherfattyfoodsimulantssho
41、uldbeexamined,seeannexAand9.3and9.5ofEN11861:2002.Ifa n interferenceispresentwhichwouldinterferewiththetriheptadecanoininternalstandardanalternativeinternalstandardshou ld beused,seeannexA,and9.3ofEN11861:2002. 4Reagents NOTE Allreagentsshouldbeofrecognizedanalyticalquality,unlessotherwisespecified.
42、 4.1 Oliveoil,simulantD,asspecifiedin5.2ofEN11861:2002. 4.2 Extractionsolvent(see10.1ofEN11861:2002). 4.2.1 Fornonpolarplastics,suchaspolyethyleneandpolypropylene: Pentane98%boilingpoint36 C. Forpolarplastics,suchaspolyamideandpolyacetal: 95/5byvolumeazeotropicmixtureofpentane98%andethanol99%. NOTE1
43、 Pentaneisaveryvolatileandhighlyflammablesolvent.Careshouldthereforebetakenwhenhandlingthissolvent topreventcontactwithsourcesofignition.Ethanolisalsoaflammablesolvent.Itisnotrecommendedthatextractionswith eitherpentaneorthepentane/ethanolmixturebeleftunattended,particularlyovernight. NOTE2 Duetothelowboilingpointsofthesesolvents,cooledcondenserwatercanberequiredtopreventunduelossofthe solventfromthecondenser. or 4.2.2 Othersuitablesolvent. NOTE1 Inpreviousmethodsfordeterminingoverallmigrationintoolive
