1、BRITISH STANDARD BS EN 1186-10:2002 Materials and articles in contact with foodstuffs Plastics Part 10: Test methods for overall migration into olive oil (modified method for use in cases where incomplete extraction of olive oil occurs) The European Standard EN 1186-10:2002 has the status of a Briti
2、sh Standard ICS 67.250 BS EN 1186-10:2002 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 14 October 2002 BSI 14 October 200
3、2 ISBN 0 580 40573 7 National foreword This British Standard is the official English language version of EN 1186-10:2002. It supersedes DD ENV 1186-10:1994 which is withdrawn. The UK participation in its preparation was entrusted by Technical Committee CW/47, Materials and articles in contact with f
4、oodstuffs, to 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 t
5、o in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the necessary provisions
6、of a contract. Users are responsible for its 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 international/European committee any enquiries on the interpretation, or pr
7、oposals for change, 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 13 and a back cover. The BSI copyright date disp
8、layed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN118610 September2002 ICS67.250 Englishversion MaterialsandarticlesincontactwithfoodstuffsPlasticsPart 10:Testmethodsforoveral
9、lmigrationintooliveoil(modified methodforuseincaseswhereincompleteextractionofoliveoil occurs) Matriauxetobjetsencontactaveclesdenres alimentairesMatireplastiquePartie10:Mthodes dessaipourlamigrationglobaledanslhuiledolive (mthodemodifieutiliserencasdextractionincomplte delhuiledolive) Werkstoffeund
10、GegenstndeinKontaktmitLebensmitteln KunststoffeTeil10:Prfverfahrenfrdie GesamtmigrationinOlivenl(ModifiziertesVerfahrenfr dieAndwendungbeiunvollstndigerExtraktionvon Olivenl) ThisEuropeanStandardwasapprovedbyCENon2May2002. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulate
11、theconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,Ger
12、man).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland
13、Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2002CEN Allrightsofexploitationinanyformandbyanymeansreserved world
14、wideforCENnationalMembers. Ref.No.EN118610:2002EEN118610:2002(E) 2 Contents page Foreword3 1 Scope 4 2 Normativereferences 4 3 Principle5 4 Reagents.5 5 Apparatus .6 6 Preparationoftestspecimens. .6 7 Procedure .6 7.1 General6 7.2 Initialweighingoftestspecimens 6 7.3 Exposuretofoodsimulant. .6 7.4 F
15、inalweighingoftestspecimens .6 7.5 Extractionofabsorbedoliveoil .6 7.6 Determinationofextractedoliveoil .7 7.6.1 Preparationoffattyacidmethylesters . 7 7.6.2 Determinationoffattyacidmethylesters . 8 8 Expressionofresults . .8 8.1 Methodofcalculation . .8 8.2 Precision.8 9 Testreport . .8 AnnexA (nor
16、mative) Determinationofthesuitabilityofoliveoilasthefattyfoodsimulantandof triheptadecanoinastheinternalstandard 9 A.1 Principle9 A.2 Procedure .9 A.3 Conclusions9 AnnexB (informative) Precision . .10 AnnexZA (informative) RelationshipofthisEuropeanStandardwithCouncilDirective89/109/EECand Commissio
17、nDirective90/128/EECandassociatedDirectives .11 Bibliography 13EN118610:2002(E) 3 Foreword ThisdocumentEN118610:2002hasbeenpreparedbyTechnicalCommitteeCEN/TC194“Utensilsincontact withfood”,thesecretariatofwhichisheldbyBSI. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicat
18、ionofanidenticaltextor byendorsement,atthelatestbyMarch2003,andconflictingnationalstandardsshallbewithdrawnatthelatestby March2003. ThisdocumentsupersedesENV118610:1994. ThisEuropeanStandardhasbeenpreparedasoneofaseriesofmethodsoftestforplasticsmaterialsandarticles incontactwithfoodstuffs. ThisParto
19、fthisEuropeanStandardhasbeenpreparedbyaSubcommittee(SC1)ofTC194Utensilsincontact withfoodasoneofaseriesofmethodsoftestforplasticsmaterialsandarticlesincontactwithfoodstuffs. ThisdocumenthasbeenpreparedunderamandategiventoCENbytheEuropeanCommissionandtheEuropean FreeTradeAssociation. Forrelationshipw
20、ithEUDirective(s),seeinformativeannexZA,whichisanintegralpartofthisdocument. AtthetimeofpreparationandpublicationofthisstandardtheEuropeanUnionlegislationrelatingtoplastics materialsandarticlesintendedtocomeintocontactwithfoodstuffsisincomplete.FurtherDirectivesand amendmentstoexistingDirectivesaree
21、xpectedwhichcouldchangethelegislativerequirementswhichthis standardsupports.Itisthereforestronglyrecommendedthatusersofthisstandardrefertothelatestrelevant publishedDirective(s)beforecommencementofanyofthetestortestsdescribedinthisstandard. EN118610shouldbereadinconjunctionwithEN11861,EN11862,EN1186
22、4,EN11866,EN11868,prEN 118612andEN118613. FurtherPartsofthisstandardhavebeenpreparedconcernedwiththedeterminationofoverallmigrationfrom plasticsmaterialsintofoodsimulants.Theirtitlesareasfollows: EN1186MaterialsandarticlesincontactwithfoodstuffsPlastics Part1 Guidetotheselectionofconditionsandtestme
23、thodsforoverallmigration Part2 Testmethodsforoverallmigrationintooliveoilbytotalimmersion Part3 Testmethodsforoverallmigrationintoaqueousfoodsimulantsbytotalimmersion Part4 Testmethodsforoverallmigrationintooliveoilbycell Part5 Testmethodsforoverallmigrationintoaqueousfoodsimulantsbycell Part6 Testm
24、ethodsforoverallmigrationintooliveoilusingapouch Part7 Testmethodsforoverallmigrationintoaqueousfoodsimulantsusingapouch Part8 Testmethodsforoverallmigrationintooliveoilbyarticlefilling Part9 Testmethodsforoverallmigrationintoaqueousfoodsimulantsbyarticlefilling Part11 Testmethodsforoverallmigration
25、intomixturesof 14 Clabelledsynthetictriglyceride Part12 Testmethodsforoverallmigrationatlowtemperatures Part13 Testmethodsforoverallmigrationathightemperatures Part14 TestmethodsforsubstitutetestsforoverallmigrationfromplasticsintendedtocomeintoEN118610:2002(E) 4 contactwithfattyfoodstuffsusingtestm
26、ediaisooctaneand95%ethanol Part15 Alternativetestmethodstomigrationintofattyfoodsimulantsbyrapidextractionintoiso octaneand/or95%ethanol AnnexAofthisstandardisnormativewhereapplicable.AnnexBisinformative. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing co
27、untriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain, Sweden,SwitzerlandandtheUnitedKingdom. 1Scope ThisEuropeanStandardspecifiestestmethodsforthedeterminationofthe
28、overallmigrationintofattyfood simulantsfromplasticsmaterialsandarticles,bytotalimmersionoftestspecimensinafattyfoodsimulantatany temperaturesabove5 Cuptoandincluding175 Cforselectedtimes. WhensomeplasticsaretestedbythemethodsinEN11862,EN11864,EN11866,EN11868,prEN118612 andEN118613,thesoxhletextracti
29、onprocessdoesnotachievecompleterecoveryoftheabsorbedoliveoilfrom thetestspecimens.Inthismethod,theoliveoilisreleasedfromtheplasticstestspecimensbydissolvingthemin chloroform,toluene,xyleneortetrahydrofuran. ThismethodissuitableforplasticswhenexposuretooliveoilisbytotalimmersionasdescribedinEN11862,i
30、na cell,asdescribedinEN11864,inapouch,asdescribedinEN11866,andbyfilling,asdescribedinEN11868 andtotestscarriedoutatlowandhightemperature,asdescribedinprEN118612andEN118613. Thisisprovidedtheplasticsaresolubleinchloroform,toluene,xyleneortetrahydrofuranandinsolubleinmethanol andthatwheneverprEN11862i
31、sreferredtointhismethodtheappropriateclauseoftherelevantpartofEN1186 issubstituted. Themethodcanalsobesuitableforplasticswhichareonlypartiallysolubleinchloroform,toluene,xyleneor tetrahydrofuranandinsolubleinmethanol. NOTE1 Thistestmethodhasbeenwrittenforusewiththefattyfoodsimulant,oliveoil.Thetestm
32、ethodcanalsobeused withappropriatemodificationswithotherfattyfoodsimulantscalledsimulantDasyntheticmixtureoftriglycerides,sunf lower oilandcornoil.Theseotherfattyfoodsimulantswillproducedifferentchromatogramsforthesimulantmethylesterstothos eof themethylestersofoliveoil.Selectsuitablechromatogrampea
33、ksofthemethylestersoftheotherfattyfoodsimulantsfor the quantitativedeterminationofthesimulantextractedfromthetestspecimens. NOTE2 Ifithasbeenestablishedthattheoverallmigrationintooliveoilfromtheplasticscannotbedeterminedbyuseof eitherthismethodorthemethodsdescribedinEN11862,EN11864,EN11866andEN11868
34、thentheuseofsubstitute testsshouldbeconsidered,seeclause6ofEN11861:2001. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedandundatedreference,provisionsfromotherpublications.These normativereferencesarecitedattheappropriateplacesinthetext,andthepublicationsarelistedhereafter.For datedref
35、erences,subsequentamendmentstoandrevisionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthelatesteditionofthe publicationreferredtoapplies,includingamendments(includingamendments). EN11861:2002, Materialsandarticlesincontactwith
36、foodstuffsPlasticsPart1:Guidetotheselectionof conditionsandtestmethodsforoverallmigration. EN11862:2002, MaterialsandarticlesincontactwithfoodstuffsPlasticsPart2:Testmethodsforoverall migrationintooliveoilbytotalimmersion.EN118610:2002(E) 5 3Principle Theoverallmigrationfromasampleoftheplastic,sucha
37、spolystyrene,isdeterminedasthelossinmassof specimensafterimmersioninoliveoil. Theselectionofthetestconditionswillbedeterminedbytheconditionsofuse,seeclauses4,5and6of EN11861:2002. Testspecimensofknownmassareexposedtooliveoilfortheexposuretime,attemperaturesvaryingfrom5 Cto 175 C,thentakenfromtheoliv
38、eoil,blottedtoremoveoiladheringtothesurface,andreweighed. Thespecimenswillusuallyretainabsorbedoliveoilwhichisextractedbyadissolutionandprecipitationprocedure anddeterminedquantitativelybygaschromatography,afterconversiontomethylesters.Methylationiscarriedout byreactingaborontrifluoride/methanolcomp
39、lexwithfattyacidsformedbyhydrolysingtheoilwithpotassium hydroxide. Incasetheplasticdoesnotdissolvecompletely,swellingoftheplasticinthesolventshouldbesuchthattheolive oilabsorbedcanbereleasedfromtheplastic. Dependingonthetypeofplasticanappropriateorganicsolventisselectedinordertodissolveorswellthepla
40、stic. Forchloroformsolubleplasticslikepolystyreneandpolycarbonate,chloroformisusedtoreleasetheoliveoil absorbed. Forpolyolefins,tolueneandxyleneareusedaslowdensitypolyethyleneshowsgoodsolubilityintolueneandhigh densitypolyethyleneandpolypropylenedissolveorswellsufficientlyinxylene. Forpolyvinylchlor
41、ideorpolyvinylidenechloride,tetrahydrofurancanbeapplied. Overallmigrationintotheoliveoiliscalculatedbysubtractingthemassofoliveoilretainedbythetestspecimen fromthemassofthetestspecimenafterremovalfromtheoliveoil,andthensubtractingthismassfromtheinitial massofthetestspecimen. Thetotallossinmassisexpr
42、essedinmilligramspersquaredecimetreofsurfaceareaofthetestspecimen intendedtocomeintocontactwithfoodstuffsandtheoverallmigrationisreportedasthemeanofaminimumof threedeterminationsonseparatetestspecimens. Toallowforinaccuracieswhichmayariseduringtheprocedureandwhichmaybedifficulttodetect,duefor exampl
43、etocontaminationorlossofoilduringthesamplinghandlingstages,quadruplicatedeterminationsare carriedoutonthesampleallowingfortheresultfromonespecimentobediscarded. NOTE Beforestartingamigrationexercise,thetestsampleshouldbeexaminedforthepresenceofcomponentsinterfering inthedeterminationoftheamountofoliveoilextracted,see7.1ofEN11862:2002.Ifanunacceptableamountofinterferenc e ispresentthensuitabilityofoneoftheotherfattyfoodsimulantsshouldbeexamined,seeanne
