1、BRITISH STANDARD BS EN 1186-8:2002 Materials and articles in contact with foodstuffs Plastics Part 8: Test methods for overall migration into olive oil by article filling The European Standard EN 1186-8:2002 has the status of a British Standard ICS 67.250 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS
2、PERMITTED BY COPYRIGHT LAWBS EN 1186-8:2002 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
3、 0 580 39750 5 National foreword This British Standard is the official English language version of EN 1186-8:2002. It supersedes DD ENV 1186-8:1994 which is withdrawn. The UK participation in its preparation was entrusted by Technical Committee CW/47, Materials in contact with food, to Subcommittee
4、CW/47/1, 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 f
5、ound 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 Standa
6、rds are 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
7、the UK 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 31 and a back cover. The BSI copyright date displayed in this document indica
8、tes when the document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN11868 April2002 ICS67.250 SupersedesENV11868:1994 Englishversion MaterialsandarticlesincontactwithfoodstuffsPlasticsPart 8:Testmethodsforoverallmigrationi
9、ntooliveoilbyarticlefilling Matriauxetobjetsencontactaveclesdenres alimentairesMatireplastiquePartie8:Mthodes dessaipourlamigrationglobaledanslhuiledolivepar remplissage WerkstoffeundGegenstndeinKontaktmitLebensmitteln KunststoffeTeil8:Prfverfahrenfrdie GesamtmigrationinOlivenldurchFllendes Gegensta
10、ndes ThisEuropeanStandardwasapprovedbyCENon4January2002. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standard
11、smaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official v
12、ersions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISC
13、HESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2002CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN11868:2002EEN11868:2002(E) 2 Contents page Foreword3 1 Scope 5 2 Normativereferences 5 3 Principle5 4 Reagents.6 5 Apparatus .7 6
14、Preparationoftestspecimens. .9 7 Procedure .10 8 Expressionofresults . .16 9 Testreport . .17 AnnexA (normative) Determinationofthesuitabilityofoliveoilasthefattyfoodsimulantandof triheptadecanoinastheinternalstandard 18 AnnexB (normative) Determinationoftheneedforsampleconditioning.20 AnnexC (norma
15、tive) Determinationoftheneedforsampleconditioninganddeterminationofthe massofmoisturesensitivetestspecimens,byvacuumdrying.21 AnnexD (normative) Determinationofchangeinmoisturecontentoftestspecimensbymeasurement ofthetransferofwaterto,orfromoliveoil,byKarlFischertitration23 AnnexE (informative) Typi
16、calchromatogramsandcalibrationgraph25 AnnexF (informative) Precisiondata .28 AnnexZA (informative) RelationshipofthisEuropeanStandardwithCouncilDirective89/109/EEC andCommissionDirective90/128/EECandassociatedDirectives29 Bibliography 31EN11868:2002(E) 3 Foreword ThisdocumentEN11868:2002hasbeenprepa
17、redbyTechnicalCommitteeCEN/TC194“Utensilsincontactwith food”,thesecretariatofwhichisheldbyBSI. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationofanidenticaltextor byendorsement,atthelatestbyOctober2002,andconflictingnationalstandardsshallbewithdrawnatthelatest byOctob
18、er2002. ThisdocumentsupersedesENV11868:1994. ThisEuropeanStandardisoneofaseriesofmethodsoftestforplasticsmaterialsandarticlesincontactwith foodstuffs. ThisdocumenthasbeenpreparedunderamandategiventoCENbytheEuropeanCommissionandtheEuropean FreeTradeAssociation,andsupportsessentialrequirementsofECDire
19、ctive(s). ForrelationshipwithECDirective(s),seeinformativeannexZA,whichisanintegralpartofthisdocument. AtthetimeofpreparationandpublicationofthisstandardtheEuropeanUnionlegislationrelatingtoplastics materialsandarticlesintendedtocomeintocontactwithfoodstuffsisincomplete.FurtherDirectivesand amendmen
20、tstoexistingDirectivesareexpectedwhichcouldchangethelegislativerequirementswhichthis standardsupports.Itisthereforestronglyrecommendedthatusersofthisstandardrefertothelatestrelevant publishedDirective(s)beforecommencementofanyofthetestortestsdescribedinthisstandard. EN11868shouldbereadinconjunctionw
21、ithEN11861. Theirtitlesareasfollows: EN1186MaterialsandarticlesincontactwithfoodstuffsPlastics Part1 Guidetotheselectionofconditionsandtestmethodsforoverallmigration Part2 Testmethodsforoverallmigrationintooliveoilbytotalimmersion Part3 Testmethodsforoverallmigrationintoaqueousfoodsimulantsbytotalim
22、mersion Part4 Testmethodsforoverallmigrationintooliveoilbycell Part5 Testmethodsforoverallmigrationintoaqueousfoodsimulantsbycell Part6 Testmethodsforoverallmigrationintooliveoilusingapouch Part7 Testmethodsforoverallmigrationintoaqueousfoodsimulantsusingapouch Part9 Testmethodsforoverallmigrationin
23、toaqueousfoodsimulantsbyarticlefilling Part10 Testmethodsforoverallmigrationintooliveoil(modifiedmethodforuseincaseswhere incompleteextractionofoliveoiloccurs) Part11 Testmethodsforoverallmigrationintomixturesof 14 Clabelledsynthetictriglyceride Part12 Testmethodsforoverallmigrationatlowtemperatures
24、 Part13 TestmethodsforoverallmigrationathightemperaturesEN11868:2002(E) 4 Part14 Testmethodsforsubstitutetestsforoverallmigrationfromplasticsintendedtocome into contactwithfattyfoodstuffsusingtestmediaisooctaneand95%ethanol Part15 Alternativetestmethodstomigrationintofattyfoodsimulantsbyrapidextract
25、ionintoiso octaneand/or95%ethanol TheannexesAtoDarenormative.TheannexesEandFareinformative. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Gree
26、ce,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain, Sweden,SwitzerlandandtheUnitedKingdom.EN11868:2002(E) 5 1Scope ThisPartofthisEuropeanStandardspecifiestestmethodsforthedeterminationoftheoverallmigrationintofatty foodsimulantsfromplasticsmaterialsandarticles,byfillingoftes
27、tspecimenswithafattyfoodsimulantat temperaturesabove20 Candupto,butnotincluding,100 Cforselectedtimes. Thismethodismostsuitableforplasticsintheformofcontainersandarticlesthatcanbefilled. Testingsamplesbythismethodenablestestingofnonhomogenousarticlesprovidedtheyarenottoolarge. NOTE Thistestmethodhas
28、beenwrittenforusewiththefattyfoodsimulant,oliveoil.Thetestmethodcanalsobeused withappropriatemodificationswithotherfattyfoodsimulantscalledsimulantDasyntheticmixtureoftriglycerides,sun flower oilandcornoil.Theseotherfattyfoodsimulantswillproducedifferentchromatogramsforthesimulantmethylesterstothos
29、eof themethylestersofoliveoil.Selectsuitablechromatogrampeaksofthemethylestersoftheotherfattyfoodsimulantsfor the quantitativedeterminationofthesimulantextractedfromthetestspecimens. Thetestmethoddescribedisapplicabletomosttypesofplastics,althoughtherearesomeplasticsforwhichitis knownnottobeapplicab
30、le. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedandundatedreference,provisionsfromotherpublications.These normativereferencesarecitedattheappropriateplacesinthetext,andthepublicationsarelistedhereafter.For datedreferences,subsequentamendmentstoandrevisionsofanyofthesepublicationsapp
31、lytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthelatesteditionofthe publicationreferredtoapplies(includingamendments). EN11861:2002, MaterialsandarticlesincontactwithfoodPlasticsPart1:Guidetotheselectionofconditions andtestmethodsforoverallmigration. ISO6
32、48, LaboratoryglasswareOnemarkpipettes . ISO4788, LaboratoryglasswareGraduatedmeasuringcylinders. 3Principle Theoverallmigrationfromasampleoftheplasticsisdeterminedasthelossinmassperunitofsurfacearea intendedtocomeintocontactwithfoodstuffs. Theselectionoftheconditionsoftestwillbedeterminedbythecondi
33、tionsofuse,seeclauses4,5and6ofEN 11861:2002. Testspecimensofknownmassarefilledwitholiveoilfortheexposuretime,attemperaturesabove20 Cand below100 C,thenemptiedandblottedtoremoveoiladheringtothesurface,andreweighed. Thespecimenswillusuallyretainabsorbedoliveoilthatisextractedanddeterminedquantitativel
34、ybymeansofgas chromatographyafterconversiontomethylesters.Methylationiscarriedoutbyreactingaboron trifluoride/methanolcomplexwithfattyacidsformedbyhydrolysingtheoilwithpotassiumhydroxide.Aninternal standard,triheptadecanoin,isaddedpriortotheextractionoftheabsorbedoliveoilfromthetestspecimens.This en
35、suresthatanyactiveorextractablecomponentsoftheplasticsreactwiththeinternalstandard,aswellaswith theextractedoliveoil.Theinternalstandardisalsosubjectedtothehydrolysisandmethylationreactions,providing compensationforanyinefficienciesinthehydrolysisandmethylationprocesses.EN11868:2002(E) 6 Migrationin
36、totheoliveoiliscalculatedbysubtractingthemassofoliveoilretainedbythetestspecimenfromthe massofthetestspecimenafterremovingtheoliveoil,thensubtractingthismassfromtheinitialmassofthe specimen. Thetotallossinmassisexpressedinmilligramspersquaredecimetreofsurfaceareaofthespecimenandthe overallmigrationi
37、sreportedasthemeanofaminimumofthreedeterminationsonseparatetestspecimens. Toallowforinaccuracieswhichmayariseduringtheprocedureandwhichmaybedifficulttodetect,duefor exampletocontaminationorlossofoilduringthesamplehandlingstages,fourdeterminationsarecarriedouton thesampleallowingfortheresultfromonesp
38、ecimentobediscarded. Thismethodincludesvariationswhichareapplicabletocertainplastics. NOTE Beforestartingamigrationexercise,thetestsampleshouldbeexaminedforthepresenceofcomponentsinterfering inthedeterminationoftheamountofoliveoilextracted,see7.1.Ifanunacceptableamountofinterferenceispresentthen sui
39、tabilityofoneoftheotherfattyfoodsimulantsshouldbeexamined,seeannexAand9.3and9.5ofEN11861:2002.Ifa n interferenceispresentwhichwouldinterferewiththetriheptadecanoininternalstandardanalternativeinternalstandardshou ld beused,seeannexA,and9.3ofEN11861:2002. 4Reagents NOTE Allreagentsshouldbeofrecognize
40、danalyticalquality,unlessotherwisespecified. 4.1 Oliveoil,simulantD,asspecifiedin4.2ofEN11861:2002. 4.2 Extractionsolvent(see9.1ofprEN11861:2001). 4.2.1 Fornonpolarplastics,suchaspolyethyleneandpolypropylene: Pentane98%boilingpoint36 C. Forpolarplastics,suchaspolyamideandpolyacetal: 95/5byvolumeazeo
41、tropicmixtureofpentane98%andethanol99%. NOTE1 Pentaneisaveryvolatileandhighlyflammablesolvent.Careshouldthereforebetakenwhenhandlingthissolvent topreventcontactwithsourcesofignition.Ethanolisalsoaflammablesolvent.Itisnotrecommendedthatextractionswith eitherpentaneorthepentane/ethanolmixturebeleftuna
42、ttended,particularlyovernight. NOTE2 Duetothelowboilingpointsofthesesolvents,cooledcondenserwatercanberequiredtopreventunduelossof thesolventfromthecondenser. or 4.2.2 Othersuitablesolvent. NOTE1 Inpreviousmethodsfordeterminingoverallmigrationintooliveoiltheextractionsolventusedhasbeen1,1,2 trichlor
43、otrifluoroethane.Forenvironmentalreasonstheuseofthissolventshouldbeavoidedwherepossible,see9.1of EN11861:2002.Experiencehasshownthatthissolvent,althougheffectiveformostplasticsrequireslongerperiodsof extraction. NOTE2 Somesolventscancontainnonvolatilesubstanceswhich,afterhydrolysisandmethylationprocesses,producegas chromatographypeakswithretentiontimessimilartotheretentiontimesofoliveoilmethylestersandmethylheptadecanoate fromtheinternalstandard.Solventsfoundtocontainsuchsubstancesshouldberedistilledbeforeuse. 4.3 Internalst
