1、BRITISH STANDARD BS EN 1186-9:2002 Materials and articles in contact with foodstuffs Plastics Part 9: Test methods for overall migration into aqueous food simulants by article filling The European Standard EN 1186-9:2002 has the status of a British Standard ICS 67.250 NO COPYING WITHOUT BSI PERMISSI
2、ON EXCEPT AS PERMITTED BY COPYRIGHT LAWBS EN 1186-9:2002 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
3、May 2002 ISBN 0 580 39749 1 National foreword This British Standard is the official English language version of EN 1186-9:2002. It supersedes DD ENV 1186-9:1994 which is withdrawn. The UK participation in its preparation was entrusted by Technical Committee CW/47, Materials in contact with food, to
4、Subcommittee 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 docu
5、ment may be found 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 B
6、ritish Standards 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 chan
7、ge, and keep 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 15 and a back cover. The BSI copyright date displayed in this do
8、cument indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN11869 April2002 ICS67.250 SupersedesENV11869:1994 Englishversion MaterialsandarticlesincontactwithfoodstuffsPlasticsPart 9:Testmethodsforover
9、allmigrationintoaqueousfood simulantsbyarticlefilling Matriauxetobjetsencontactaveclesdenres alimentairesMatireplastiquePartie9:Mthodes dessaipourlamigrationglobaledanslesliquides simulateursaqueuxparremplissage WerkstoffeundGegenstndeinKontaktmitLebensmitteln KunststoffeTeil9:Prfverfahrenfrdie Gesa
10、mtmigrationinwssrigePrflebensmitteldurchFllen desGegenstandes ThisEuropeanStandardwasapprovedbyCENon4January2002. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsand
11、bibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnoti
12、fiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITT
13、EEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2002CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN11869:2002EEN11869:2002(E) 2 Contents page Foreword3 1 Scope 5 2 Normativ
14、ereferences 5 3 Principle5 4 Reagents.5 5 Apparatus .6 6 Preparationoftestspecimens. .6 7 Procedure .7 8 Expressionofresults . .9 9 Testreport . .11 AnnexA (informative) Precisiondata .12 AnnexZA (informative) RelationshipofthisEuropeanStandardwithCouncilDirective89/109/EEC andCommissionDirective90/
15、128/EECandassociatedDirectives13 Bibliography 15EN11869:2002(E) 3 Foreword ThisdocumentEN11869:2002hasbeenpreparedbyTechnicalCommitteeCEN/TC194“Utensilsincontactwith food”,thesecretariatofwhichisheldbyBSI. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationofanidenticalt
16、extor byendorsement,atthelatestbyOctober2002,andconflictingnationalstandardsshallbewithdrawnatthelatest byOctober2002. ThisdocumentsupersedesENV11869:1994. ThisEuropeanStandardisoneofaseriesofmethodsoftestforplasticsmaterialsandarticlesincontactwith foodstuffs. Thisdocumenthasbeenpreparedunderamanda
17、tegiventoCENbytheEuropeanCommissionandtheEuropean FreeTradeAssociation,andsupportsessentialrequirementsofECDirective(s). ForrelationshipwithECDirective(s),seeinformativeannexZA,whichisanintegralpartofthisdocument. AtthetimeofpreparationandpublicationofthisstandardtheEuropeanUnionlegislationrelatingt
18、oplastics materialsandarticlesintendedtocomeintocontactwithfoodstuffsisincomplete.FurtherDirectivesand amendmentstoexistingDirectivesareexpectedwhichcouldchangethelegislativerequirementswhichthis standardsupports.Itisthereforestronglyrecommendedthatusersofthisstandardrefertothelatestrelevant publish
19、edDirective(s)beforecommencementofanyofthetestortestsdescribedinthisstandard. EN11869shouldbereadinconjunctionwithEN11861. FurtherPartsofthisstandardhavebeenprepared,andothersareinpreparation,concernedwiththedetermination ofoverallmigrationfromplasticsmaterialsintofoodsimulants.Theirtitlesareasfollo
20、ws: EN1186MaterialsandarticlesincontactwithfoodstuffsPlastics Part1 Guidetotheselectionofconditionsandtestmethodsforoverallmigration Part2 Testmethodsforoverallmigrationintooliveoilbytotalimmersion Part3 Testmethodsforoverallmigrationintoaqueousfoodsimulantsbytotalimmersion Part4 Testmethodsforovera
21、llmigrationintooliveoilbycell Part5 Testmethodsforoverallmigrationintoaqueousfoodsimulantsbycell Part Testmethodsforoverallmigrationintooliveoilusingapouch Part7 Testmethodsforoverallmigrationintoaqueousfoodsimulantsusingapouch Part8 Testmethodsforoverallmigrationintooliveoilbyarticlefilling Part10
22、Testmethodsforoverallmigrationintooliveoil(modifiedmethodforuseincaseswhere incompleteextractionofoliveoiloccurs) Part11 Testmethodsforoverallmigrationintomixturesof 14 Clabelledsynthetictriglyceride Part12 TestmethodsforoverallmigrationatlowtemperaturesEN11869:2002(E) 4 Part13 Testmethodsforoverall
23、migrationathightemperatures Part14 Testmethodsforsubstitutetestsforoverallmigrationfromplasticsintendedtocomeinto contactwithfattyfoodstuffsusingtestmediaisooctaneand95%ethanol Part15 Alternativetestmethodstomigrationintofattyfoodsimulantsbyrapidextractionintoiso octaneand/or95%ethanol AnnexAisinfor
24、mative. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain, Sweden,
25、SwitzerlandandtheUnitedKingdom.EN11869:2002(E) 5 1Scope ThisPartofthisEuropeanStandardspecifiestestmethodsforthedeterminationoftheoverallmigrationfromone surfaceonlyofplasticsarticlesintheformofcontainers,whichareintendedtocomeintocontactwithfoodstuffs, intoaqueousbasedfoodsimulants,byfillingarticle
26、swithaselectedfoodsimulantattesttemperaturesuptoand including70 Cforselectedtesttimes. Thismethodismostsuitableforplasticsintheformofcontainersandarticlesthatcanbefilled. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedandundatedreference,provisionsfromotherpublications.These normativer
27、eferencesarecitedattheappropriateplacesinthetext,andthepublicationsarelistedhereafter.For datedreferences,subsequentamendmentstoandrevisionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthelatesteditionofthe publicationreferredt
28、oapplies(includingamendments). EN11861:2002, MaterialsandarticlesincontactwithfoodPlasticsPart1:Guidetotheselectionofconditions andtestmethodsforoverallmigration . ISO648, LaboratoryglasswareOnemarkpipettes . 3Principle Theoverallmigrationofnonvolatilesubstancesfromasampleoftheplasticsisdeterminedas
29、themassofnon volatileresidueafterevaporationofthefoodsimulantsfollowingfillingthetestspecimen. Theselectionoftheconditionsoftestandthefoodsimulant(s)willbedeterminedbytheconditionsofuseas specifiedinclauses4,5and6ofEN11861:2002(3and6). Testspecimensarefilledwiththefoodsimulantfortheexposuretimeattem
30、peraturesaboveuptoandincluding 70 C.Attheendofthetestperiodeachtestspecimenisemptied.Thefoodsimulantfromeachtestspecimenis evaporatedtodryness,themassofthenonvolatileresidueisdeterminedandexpressedasmilligramspersquare decimetreofsurfaceareaexposedtothefoodsimulant. NOTE Insomecircumstancestheproced
31、uredescribedinthisstandardcanbeusedforexposureattemperaturesabove 70 C. Overallmigrationisreportedasthemeanofthreedeterminationsonseparatetestspecimens. 4Reagents Fordetailsofthepreparationandpurityofthesereagentsseeclause4ofEN11861:2002. 4.1 Distilledwaterorwaterofequivalentquality(simulantA) 4.2 A
32、ceticacid3%(w/v)inaqueoussolution(simulantB) 4.3 Ethanol10%(v/v)inaqueoussolution(simulantC) 4.4 Alcoholicsimulantsforliquidsorbeveragesofanalcoholicstrengthexceeding10%(v/v). NOTE Inthecaseofmaterialsandarticlesintendedtocomeintocontactwithliquidsorbeveragesofanalcoholicstrength exceeding10%(v/v)th
33、etestcanbecarriedoutwithaqueoussolutionsofethanolofasimilarstrength.EN11869:2002(E) 6 5Apparatus 5.1 Analyticalbalancecapableofdeterminingachangeinmassof0,1mg. 5.2 Lintfreeclothorsoftbrush. 5.3 Beaker,2l. 5.4 Glassbeads,2mmto3mmdiameter. 5.5 Thermostaticallycontrolledovenorincubatororrefrigeratorcap
34、ableofmaintainingthesettemperature withinthetolerancesspecifiedinTableB.2ofEN11861:2002. 5.6 Dishes,stainlesssteel,nickel,platinum,platinumalloy,gold50mmto90mmdiameterandmaximummass 100g,forevaporationoffoodsimulantsandweighingofresidues.Glass,glassceramicorceramicdishesmaybe used,providedthatthesur
35、facecharacteristicsaresuchthatthemassesofthedishesafterevaporationofany specifiedfoodsimulantsfollowedbyconditioninginthedesiccatorused,achievesaconstancyof 0,5mg. Stainlesssteelandnickeldishesaresuitableonlyfordistilledwaterandethanolsolutions.Glass,glassceramic, glazedceramic,platinum,platinumallo
36、yorgolddishesaresuitableforallthreesimulants. 5.7 Steambath,hotplate,distillationapparatusorrotaryevaporatorforevaporationoffoodsimulantattheend oftestperiod. 5.8 Desiccatorwithanhydrouscalciumchlorideorselfindicatingsilicagel. 5.9 Beakers,250ml. 5.10 Pipette,200ml,complyingwiththeminimumrequirement
37、sofISO648. 6 Preparationoftestspecimens 6.1General Itisessentialthattestspecimensarecleanandfreefromsurfacecontamination(manyplasticscanreadilyattract dustduetostaticcharges).Beforepreparingtestspecimens,removeanysurfacecontaminationfromthesample bygentlywipingitwithalintfreecloth,orbybrushingwithas
38、oftbrush.Undernocircumstanceswashthesample withwaterorsolvent.Ifitisspecifiedintheinstructionsforuseofthearticlethatitshouldbewashedorcleaned beforeusesee8.1ofEN11861:2002.Minimizehandlingofthesamplesand,wherenecessary,wearcotton gloves. 6.2 Numberoftestspecimens 6.2.1 Volumeofarticles Determineandr
39、ecordthevolumeoffoodsimulantrequiredtofillanarticletoitsnominalfoodstuffvolume.Ifthe nominalvolumeoffoodstufftofillthearticleisnotknown,determinethesurfaceareathatwillbeincontactwiththe foodsimulantwhenfilledto5mmfromthetopofthetestspecimen. 6.2.2 Articleswithanominalvolumeofmorethan200ml Fivearticl
40、esarerequiredtoprovidefivetestspecimens.Thesetestspecimensareutilizedasfollows: a)threetestspecimensforthemigrationtest; b)twotestspecimensforthedeterminationofsurfacearea.EN11869:2002(E) 7 6.2.3 Articleswithanominalvolumeoflessthan200ml Thenumberofarticlesrequiredtoprovideatestspecimenisdependenton
41、theirvolume.Atestspecimenshallbe madeupofsufficientarticlestocontainaminimumof200mlofthefoodsimulant. Fivetestspecimensarerequired.Thesetestspecimensareutilizedasfollows: a)threetestspecimensforthemigrationtest; b)twotestspecimensforthedeterminationofsurfacearea. Recordthenumberofarticlesusedtoprovi
42、dethetestspecimen. 6.3 Surfaceareaoftestspecimenexposedtofoodsimulant Determineandrecordthesurfaceareaofthetestspecimenwhichisintendedtocomeintocontactwithitsnominal volumeoffoodstuff.Ifthenominalvolumeoffoodstufftofillthearticleisnotknown,determinethesurfacearea whichwillbeincontactwiththefoodsimul
43、antwhenfilledto5mmfromthetopofthetestspecimen. NOTE1 Forsomearticlesitisrecognizedthatitisimpracticaltomeasurethesurfaceareaintendedtocomeintocontact withfoodstuff.Forsucharticlestheoverallmigrationismeasuredasmilligramsofsubstancereleasedperkilogramoffood simulant. NOTE2 Inthecaseofarticleswithavolumeoflessthan200mlthiswillbethesurfaceareaofonearticlemultipliedbythe numberofarticlesusedtoprovideatestspecimen. 6.4 Articleswithacapacityofnotlessthan500mlandnotmorethan10l Itisnotnecessarytodetermi
