1、BRITISH STANDARD BS EN 1186-2:2002 Materials and articles in contact with foodstuffs Plastics Part 2: Test methods for overall migration into olive oil by total immersion The European Standard EN 1186-2:2002 has the status of a British Standard ICS 67.250 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS
2、PERMITTED BY COPYRIGHT LAWBS EN 1186-2:2002 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 39747 5 National foreword This British Standard is the official English language version of EN 1186-2:2002. It supersedes DD ENV 1186-2:1994 which is withdrawn.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 32, an inside back cover and a back cover. The BSI copyright date displayed i
8、n this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN11862 April2002 ICS67.250 SupersedesENV11862:1994 Englishversion MaterialsandarticlesincontactwithfoodstuffsPlasticsPart 2:Testmetho
9、dsforoverallmigrationintooliveoilbytotal immersion Matriauxetobjetsencontactaveclesdenres alimentairesMatireplastiquePartie2:Mthodes dessaipourlamigrationglobaledanslhuiledolivepar immersiontotale WerkstoffeundGegenstndeinKontaktmitLebensmitteln KunststoffeTeil2:Prfverfahrenfrdie GesamtmigrationinOl
10、ivenldurchvlligesEintauchen ThisEuropeanStandardwasapprovedbyCENon4January2002. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernin
11、gs uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesam
12、estatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPEND
13、ENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2002CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN11862:2002EEN11862:2002(E) 2 Contents page Foreword3 1 Scope 5 2 Normativereferences 5 3 Principle5 4 Reage
14、nts.6 5 Apparatus .7 6 Preparationoftestspecimens. .9 7 Procedure .10 8 Expressionofresults . .17 8.1 Methodofcalculation . .17 9 Testreport . .18 AnnexA (normative) Determinationofthesuitabilityofoliveoilasthefattyfoodsimulantandof triheptadecanoinastheinternalstandard 19 AnnexB (normative) Determi
15、nationoftheneedforsampleconditioning.21 AnnexC (normative) Determinationoftheneedforsampleconditioninganddeterminationofthe massofmoisturesensitivetestspecimens,byvacuumdrying.22 AnnexD (normative) Determinationofchangeinmoisturecontentoftestspecimensby measurementofthetransferofwaterto,orfromoliveo
16、il,byKarlFischertitration .24 AnnexE (informative) Typicalchromatogramsandcalibrationgraph.26 AnnexF (informative) Precisiondata .29 AnnexZA (informative) RelationshipofthisEuropeanStandardwithCouncilDirective89/109/EEC andCommissionDirective90/128/EECandassociatedDirectives30 Bibliography 32EN11862
17、:2002(E) 3 Foreword ThisdocumentEN11862:2002hasbeenpreparedbyTechnicalCommitteeCEN/TC194“Utensilsincontactwith food“,thesecretariatofwhichisheldbyBSI . ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationofanidenticaltextor byendorsement,atthelatestbyOctober2002,andconfli
18、ctingnationalstandardsshallbewithdrawnatthelatest byOctober2002. ThisdocumentsupersedesENV11862:1994. ThisEuropeanStandardisoneofaseriesofmethodsoftestforplasticsmaterialsandarticlesincontactwith foodstuffs. ThisdocumenthasbeenpreparedunderamandategiventoCENbytheEuropeanCommissionandtheEuropean Free
19、TradeAssociation,andsupportsessentialrequirementsofECDirective(s). ForrelationshipwithECDirective(s),seeinformativeannexZA,whichisanintegralpartofthisdocument. AtthetimeofpreparationandpublicationofthisstandardtheEuropeanUnionlegislationrelatingtoplastics materialsandarticlesintendedtocomeintocontac
20、twithfoodstuffsisincomplete.FurtherDirectivesand amendmentstoexistingDirectivesareexpectedwhichcouldchangethelegislativerequirementswhichthis standardsupports.Itisthereforestronglyrecommendedthatusersofthisstandardrefertothelatestrelevant publishedDirective(s)beforecommencementofanyofthetestortestsd
21、escribedinthisstandard. EN11862shouldbereadinconjunctionwithEN11861. FurtherPartsofthisstandardhavebeenpreparedconcernedwiththedeterminationofoverallmigrationfrom plasticsmaterialsintofoodsimulants. Theirtitlesareasfollows: EN1186MaterialsandarticlesincontactwithfoodstuffsPlastics Part1 Guidetothese
22、lectionofconditionsandtestmethodsforoverallmigration Part3 Testmethodsforoverallmigrationintoaqueousfoodsimulantsbytotalimmersion Part4 Testmethodsforoverallmigrationintooliveoilbycell Part5 Testmethodsforoverallmigrationintoaqueousfoodsimulantsbycell Part6 Testmethodsforoverallmigrationintooliveoil
23、usingapouch Part7 Testmethodsforoverallmigrationintoaqueousfoodsimulantsusingapouch Part8 Testmethodsforoverallmigrationintooliveoilbyarticlefilling Part9 Testmethodsforoverallmigrationintoaqueousfoodsimulantsbyarticlefilling Part10 Testmethodsforoverallmigrationintooliveoil(modifiedmethodforuseinca
24、seswhere incompleteextractionofoliveoiloccurs) Part11 Testmethodsforoverallmigrationintomixturesof 14 Clabelledsynthetictriglyceride Part12 TestmethodsforoverallmigrationatlowtemperaturesEN11862:2002(E) 4 Part13 Testmethodsforoverallmigrationathightemperatures Part14 Testmethodsforsubstitutetestsfor
25、overallmigrationfromplasticsintendedtocome into contactwithfattyfoodstuffsusingtestmediaisooctaneand95%ethanol Part15 Alternativetestmethodstomigrationintofattyfoodsimulantsbyrapidextractionintoiso octaneand/or95%ethanol AnnexesA,B,CandDtothisstandardarenormativewhereapplicable.TheannexesEandFareinf
26、ormative. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain, Swede
27、n,SwitzerlandandtheUnitedKingdom.EN11862:2002(E) 5 1Scope ThisPartofthisEuropeanStandarddescribestestmethodsforthedeterminationoftheoverallmigrationintofatty foodsimulantsfromplasticsmaterialsandarticles,bytotalimmersionoftestspecimensinafattyfoodsimulantat temperaturesabove20 Candupto,butnotincludi
28、ng,100 Cforselectedtimes. Thismethodismostsuitableforplasticsintheformoffilmsandsheets,butcanbeappliedtoawiderangeof articlesorcontainersfromwhichtestpiecesofasuitablesizecanbecut. NOTE Thistestmethodhasbeenwrittenforusewiththefattyfoodsimulant,oliveoil.Thetestmethodcanalsobeused withappropriatemodi
29、ficationswithotherfattyfoodsimulantscalledsimulantDasyntheticmixtureoftriglycerides,sun flower oilandcornoil.Theseotherfattyfoodsimulantswillproducedifferentchromatogramsforthesimulantmethylesterstothos eof themethylestersofoliveoil.Selectsuitablechromatogrampeaksofthemethylestersoftheotherfattyfood
30、simulantsfor the quantitativedeterminationofthesimulantextractedfromthetestspecimens. Thetestmethoddescribedisapplicabletomosttypesofplastics,althoughtherearesomeplasticsforwhichitis knownnottobeapplicable. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedandundatedreference,provisionsfr
31、omotherpublications.These normativereferencesarecitedattheappropriateplacesinthetext,andthepublicationsarelistedhereafter.For datedreferences,subsequentamendmentstoandrevisionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthelat
32、esteditionofthe publicationreferredtoapplies(includingamendments). EN11861:2002,MaterialsandarticlesincontactwithfoodstuffsPlastics Part1:Guidetotheselectionof conditionsandtestmethodsforoverallmigration. EN10088, Stainlesssteels. ENISO84422:1997, MaterialsandarticlesincontactwithfoodstuffsCutleryan
33、dtablehollowarePart2: Requirementsforstainlesssteelandsilverplatedcutlery(ISO84422:1997) . ISO648, LaboratoryglasswareOnemarkpipettes. ISO4788, LaboratoryglasswareGraduatedmeasuringcylinders. 3Principle Theoverallmigrationfromasampleoftheplasticsisdeterminedasthelossinmassperunitofsurfacearea intend
34、edtocomeintocontactwithfoodstuffs. Theselectionoftheconditionsoftestwillbedeterminedbytheconditionsofuse,seeclauses4,5and6ofEN 11861:2002. Testspecimensofknownmassareimmersedinoliveoilfortheexposuretime,attemperaturesabove20 Cand below100 C,thentakenfromtheoliveoil,blottedtoremoveoiladheringtothesur
35、face,andreweighed. Thespecimenswillusuallyretainabsorbedoliveoilthatisextractedanddeterminedquantitativelybymeansofgas chromatographyafterconversiontomethylesters.Methylationiscarriedoutbyreactingaboron trifluoride/methanolcomplexwithfattyacidsformedbyhydrolysingtheoilwithpotassiumhydroxide.Anintern
36、al standard,triheptadecanoin,isaddedpriortotheextractionoftheabsorbedoliveoilfromthetestspecimens.ThisEN11862:2002(E) 6 ensuresthatanyactiveorextractablecomponentsoftheplasticsreactwiththeinternalstandard,aswellaswith theextractedoliveoil.Theinternalstandardisalsosubjectedtothehydrolysisandmethylati
37、onreactions,providing compensationforanyinefficienciesinthehydrolysisandmethylationprocesses. Migrationintotheoliveoiliscalculatedbysubtractingthemassofoliveoilretainedbythetestspecimenfromthe massofthetestspecimenafterremovalfromtheoliveoil,thensubtractingthismassfromtheinitialmassofthe specimen. T
38、hetotallossinmassisexpressedinmilligramspersquaredecimetreofsurfaceareaofthespecimenandthe overallmigrationisreportedasthemeanofaminimumofthreedeterminationsonseparatetestspecimens. Toallowforinaccuracieswhichmayariseduringtheprocedureandwhichmaybedifficulttodetect,duefor exampletocontaminationorlos
39、sofoilduringthesamplehandlingstages,fourdeterminationsarecarriedouton thesampleallowingfortheresultfromonespecimentobediscarded. Thismethodincludesvariationsthatareapplicabletocertainplastics. NOTE Beforestartingamigrationexercise,thetestsampleshouldbeexaminedforthepresenceofcomponentsinterfering in
40、thedeterminationoftheamountofoliveoilextracted,see7.1.Ifanunacceptableamountofinterferenceispresentthen suitabilityofoneoftheotherfattyfoodsimulantsshouldbeexamined,seeannexAand9.3and9.5ofEN11861:2002.Ifa n interferenceispresentwhichwouldinterferewiththetriheptadecanoininternalstandardanalternativei
41、nternalstandardshou ld beused,seeannexAand9.3ofEN11861:2002. 4Reagents NOTE Allreagentsshouldbeofrecognizedanalyticalquality,unlessotherwisespecified. 4.1 Oliveoil,referencesimulantD,asspecifiedin5.2ofEN11861:2002. 4.2 Extractionsolvent(see10.1ofEN11861:2002). 4.2.1 Fornonpolarplastics,suchaspolyeth
42、yleneandpolypropylene: Pentane98%boilingpoint36 C. Forpolarplastics,suchaspolyamideandpolyacetal: 95/5byvolumeazeotropicmixtureofpentane98%andethanol99%. NOTE1 Pentaneisaveryvolatileandhighlyflammablesolvent.Careshouldthereforebetakenwhenhandlingthissolvent topreventcontactwithsourcesofignition.Etha
43、nolisalsoaflammablesolvent.Itisnotrecommendedthatextractionswith eitherpentaneorthepentane/ethanolmixturebeleftunattended,particularlyovernight. NOTE2 Duetothelowboilingpointsofthesesolvents,cooledcondenserwatercanberequiredtopreventunduelossofthe solventfromthecondenser. 4.2.2 Othersuitablesolvent. NOTE1 Inpreviousmethodsfordeterminingoverallmigrationintooliveoiltheextractionsolventusedhasbeen1,1,2 trichlorotrifluoroethane.Forenvironmentalreasonstheuseofthissolventshouldbeavoidedwherepossible,see9.1ofEN 11861.Experie
