1、DRAFT FOR DEVELOPMENT DD CEN/TS 14235:2002 Materials and articles in contact with foodstuffs Polymeric coatings on metal substrates Guide to the selection of conditions and test methods for overall migration ICS 67.250 DD CEN/TS 14235:2002 This Draft for Development was published under the authority
2、 of the Standards Policy and Strategy Committee on 30 January 2003 BSI 30 January 2003 ISBN 0 580 41153 2 National foreword This Draft for Development is the English language version of CEN/TS 14235:2002. This publication is not to be regarded as a British Standard. It is being issued in the Draft f
3、or Development series of publications and is of a provisional nature because of the need to develop a method of test dealing with the coatings of materials and articles in contact with food, in order to satisfy the proposed European legislation. It should be applied on this provisional basis, so tha
4、t information and experience of its practical application may be obtained. Comments arising from the use of this Draft for Development are requested so that UK experience can be reported to the European organization responsible for its conversion to a European standard. A review of this publication
5、will be initiated 2 years after its publication by the European organization so that a decision can be taken on its status at the end of its 3-year life. Notification of the start of the review period will be made in an announcement in the appropriate issue of Update Standards. According to the repl
6、ies received by the end of the review period, the responsible BSI Committee will decide whether to support the conversion into a European standard, to extend the life of the Technical Specification or to withdraw it. Comments should be sent in writing to the Secretary of BSI Subcommittee CW/47/1, Mi
7、gration from plastics, 389 Chiswick High Road, London W4 4AL, giving the document reference and clause number and proposing, where possible, an appropriate revision of the text. A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The Br
8、itish Standards which implement international or European publications referred to 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 O
9、nline. Summary of pages This document comprises a front cover, an inside front cover, the CEN/TS title page, pages 2 to 56, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. N
10、o. Date CommentsTECHNICALSPECIFICATION SPCIFICATIONTECHNIQUE TECHNISCHESPEZIFIKATION CEN/TS14235 October2002 ICS67.250 Englishversion MaterialsandarticlesincontactwithfoodstuffsPolymeric coatingsonmetalsubstratesGuidetotheselectionof conditionsandtestmethodsforoverallmigration WerkstoffeundGegenstnd
11、einKontaktmitLebensmitteln PolymerebeschichtungenaufSubstratenausMetall LeitfadenzurAuswahlderBedingungenundPrfverfahren zurBestimmungderGesamtmigration ThisTechnicalSpecification(CEN/TS)wasapprovedbyCENon28July2002forprovisionalapplication. TheperiodofvalidityofthisCEN/TSislimitedinitiallytothreeye
12、ars.AftertwoyearsthemembersofCENwillberequested tosubmittheir comments,particularlyonthequestionwhethertheCEN/TScanbeconvertedintoaEuropeanStandard. CENmembersarerequiredtoannouncetheexistenceofthisCEN/TSinthesamewayasforanENandtomaketheCEN/TSavailable .It ispermissibletokeepconflictingnationalstand
13、ardsinforce(inparalleltotheCEN/TS)untilthefinaldecisionaboutthep ossible conversionoftheCEN/TSintoanENisreached. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain,Swed
14、en,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2002CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.CEN/TS14235:2002ECEN/TS14235
15、:2002(E) 2 Contents page Foreword4 Introduction .5 1 Scope 6 2 Normativereferences 6 3 Termsanddefinitions. .6 3.1 polymericcoating . .6 3.2 finalarticle . .7 3.3 sample.7 3.4 testspecimen . 7 3.5 testpiece .7 3.6 conventionaloven . 7 3.7 foodsimulant. .7 3.8 migrationtest .7 3.9 substitutetest. 7 3
16、.10 testmedia . 7 3.11 alternativetest. .7 3.12 extractiontests. 7 3.13 overallmigration;globalmigration 7 3.14 reductionfactor. .8 3.15 pouch 8 3.16 reversepouch .8 3.17 inertsubstrate 8 3.18 pressureretortorautoclave . 8 3.19cell 8 3.20repeatabilityvaluer. 8 3.21reproducibilityvalueR . 8 3.22repea
17、tabilityconditions 8 3.23reproducibilityconditions 8 4 Typesoftest. 9 4.1 Migrationtests. .9 4.2 Substitutetests 9 4.3 Alternativetests . 9 4.4 Criteriafortheuseofsubstitutetests .9 5 Foodsimulants,testmediaandreagents 9 5.1 Aqueousfoodsimulants .9 5.2 Fattyfoodsimulants 10 5.3 Testmedia 11 5.4 Reag
18、ents.11 6 Selectionoffoodsimulants. .11 6.1 General11 6.2 Simulatingcontactwithallfoodtypes 11 6.3 Simulatingcontactwithspecificfoodtypes. 11 6.4 Simulatingcontactwithdryfoods . 18 6.5 Testingforfattycontact . .18 7 Migrationtests,substitutetestsandalternativetestconditions .19 7.1 Testconditionsfor
19、migrationtests. .19 7.2 Testconditionsforsubstitutetests .22 7.3 Testconditionsforalternativetests . .24 8 Apparatus .24 8.1 Specimensupports. .24 8.2 Tubes,glassrodsandglassbeads . 24CEN/TS14235:2002(E) 3 8.3 Cells.24 8.4 Thermostaticallycontrolledovensorincubators . .24 9 Samplesandsamplegeometry.
20、 .25 9.1 Samples 25 9.2 Surfacetovolumeratio. 25 9.3 Singlesurfaceversusdoublesurfacetesting(bytotalimmersion) 25 9.4 Singlesurfacetestingusingacell. 26 9.5 Singlesurfacetestingbypouch .26 9.6 Singlesurfacetestingusingareversepouch 27 9.7 Singlesurfacetestingbyfilling. .27 9.8 Articlesintendedforrep
21、eateduse .27 9.9 Caps,closuresandothersealingdevices 28 9.10 Foodandbeveragecans. 28 9.11 Nonstickcoatings. 29 9.12 Flexiblefilms . .29 9.13 Largecontainers. .29 9.14 Inertsubstrates. .29 9.15 Tubing,taps,valvesandfilters . .29 9.16 Articlesofirregularshape 29 10 Overallmigrationtestmethodswithfatty
22、foodsimulants . .30 10.1 Extractionsolvents 30 10.2 Incompleteextractionoffat. .30 10.3 Substanceswhichinterferewithgaschromatography. 30 10.4 Lossofvolatilesubstances 30 10.5 Gaschromatographiccolumns 31 10.6 ChangesintheC18/C16ratio . 31 10.7 Initialmassofthetestspecimen .32 10.8 Finalmassofthetes
23、tspecimen 33 10.9 Selectionoftheappropriateconditioningprocedure 33 10.10 Lossofsimulantduetopermeation 34 11 Precision.34 12 Testreports . .34 12.1 Surfacetovolumeratiosinactualuse. .34 12.2 Reductionfactors 35 12.3 Validityofresults .36 12.4 Testreport 36 12.5 Statementsofcompliance . .36 13 Testm
24、ethodforoverallmigrationintoaqueoussimulantsbyarticlefillingfrompolymeric coatingsonfoodandbeveragecansandnonstickcoatings37 13.1 Scope 37 13.2 Principle37 13.3 Reagents.37 13.4 Apparatus .37 13.5 Preparationoftestspecimens .38 13.6 Procedure .39 13.7 Expressionofresults 40 13.8 Testreport 43 AnnexA
25、 (normative) Characteristicsoffattyfoodsimulantsandtestmedia44 AnnexB (normative) Limitdeviationsoncontacttimesandcontacttemperaturesapplicabletoall clausesofthisTechnicalSpecification .46 AnnexC (normative) Supportsandcells. .48 Bibliography 56CEN/TS14235:2002(E) 4 Foreword Thisdocument(CEN/TS14235
26、:2002)hasbeenpreparedbyCEN/TC194“Utensilsincontactwithfood“,the secretariatofwhichisheldbyBSI. ThisdocumenthasbeenpreparedunderamandategiventoCENbytheEuropeanCommissionandtheEuropean FreeTradeAssociation. InthisTechnicalSpecificationtheannexesA,BandCarenormative. ThisTechnicalSpecificationincludesaB
27、ibliography. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoannouncethisTechnicalSpecification:Austria,Belgium,CzechRepublic,Denmark, Finland,France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal, Spa
28、in,Sweden,SwitzerlandandtheUnitedKingdom.CEN/TS14235:2002(E) 5 Introduction Nosingletestmethodhasbeendevisedwhichcanbeusedtodetermineoverallmigration,atalltemperatures,in allfoodsimulants.Indeed,owingtothepracticaldifficultiesinherentintestingwithinvolatileextractantssuchas fatsandthemultitudeofappl
29、icationsinwhichpolymericcoatingsonmetalsubstratescomeintocontactwithfood, therearemanymethodsandpermittedvariationstomethodsinthisTechnicalSpecification. ThisTechnicalSpecificationisintendedtogiveadviceontheselectionofthemostappropriatetypeoftest,test conditionsandtestmethodforagivenapplicationofapo
30、lymericcoatingonametalsubstrateandisintendedtobe readinitsentiretybeforetestingprotocolsarefinalized.Atestmethodforoverallmigrationintoaqueoussimulants byarticlefillingfrompolymericcoatingsonfoodandbeveragecansandnonstickcoatingsisgiveninclause12. FormanypolymericcoatedarticlesmethodsinEN11862toEN11
31、869aresuitable,accordingtotheformin whichthearticleistested. Thegeneralcriteriafortheoperationandassessmentoftestinglaboratoriesaswellasthegeneralcriteriafor laboratoryaccreditationbodiesaresetoutinEN45001,EN45002andEN45003.Itisrecommendedthat laboratoriesusingthisTechnicalSpecificationvalidatetheir
32、proceduresbytestingcertifiedreferencesamplesand bytakingpartinaproficiencyscheme.SuitableproficiencyschemesareoperatedinGermanyandintheUnited Kingdom,forexampletheGermanAssessmentSchemeforFoodTesting(GAFT)andtheFoodAnalysis PerformanceAssessmentScheme(FAPAS)conductedbytheCentralScienceLaboratoryofth
33、eMinistryof Agriculture,FisheriesandFood.CEN/TS14235:2002(E) 6 1Scope ThisTechnicalSpecificationgivesguidelinesfortheselectionoftheappropriateconditionsandtestmethodsfor thedeterminationofoverallmigrationintofoodsimulantsandtestmediafrompolymericcoatingsonmetal substrateswhichareintendedtocomeintoco
34、ntactwithfoodstuffsandatestmethodforoverallmigrationinto aqueoussimulantsbyarticlefillingfrompolymericcoatingsonfoodandbeveragecansandnonstickcoatings. NOTE PolymericcoatingsonmetalsubstratesarenotyetincludedinthescopeofanyEuropeanUnionDirective.This TechnicalSpecificationhasbeenpreparedtoassistinth
35、edevelopmentofsuchaDirective. 2 Normativereferences ThisTechnicalSpecificationincorporatesbydatedorundatedreference,provisionsfromotherpublications.These normativereferencesarecitedattheappropriateplacesinthetextandthepublicationsarelistedhereafter.For datedreferences,subsequentamendmentstoorrevisio
36、nsofanyofthesepublicationsapplytothisTechnical Specificationonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthelatesteditionof thepublicationreferredtoapplies(includingamendments). EN11862, MaterialsandarticlesincontactwithfoodstuffsPlasticsPart2:Testmethodsforoverallmigration into
37、oliveoilbytotalimmersion. EN11863, MaterialsandarticlesincontactwithfoodstuffsPlasticsPart3:Testmethodsforoverallmigration intoaqueousfoodsimulantsbytotalimmersion. EN11864, MaterialsandarticlesincontactwithfoodstuffsPlasticsPart4:Testmethodsforoverallmigration intooliveoilbycell. EN11865, Materials
38、andarticlesincontactwithfoodstuffsPlasticsPart5:Testmethodsforoverallmigration intoaqueousfoodsimulantsbycell. EN11866, MaterialsandarticlesincontactwithfoodstuffsPlasticsPart6:Testmethodsforoverallmigration intooliveoilusingapouch EN11867, MaterialsandarticlesincontactwithfoodstuffsPlasticsPart7:Te
39、stmethodsforoverallmigration intoaqueousfoodsimulantsusingapouch. EN11868; MaterialsandarticlesincontactwithfoodstuffsPlasticsPart8:Testmethodsforoverallmigration intooliveoilbyarticlefilling. EN118612, MaterialsandarticlesincontactwithfoodstuffsPlasticsPart12:Testmethodsforoverallmigration atlowtem
40、peratures. EN118613, MaterialsandarticlesincontactwithfoodstuffsPlasticsPart13:Testmethodsforoverallmigration athightemperatures. ISO648 LaboratoryglasswareOnemarkpipettes 3 Termsanddefinitions ForthepurposesofthisTechnicalSpecificationthefollowingtermsanddefinitionsapply. 3.1 polymericcoating organ
41、icmaterialappliedintheformofacontinuousfilmonasubstrateinsuchawayastoformaprotectivelayer and/orafunctionalbarrierbetweenfoodandsubstrate.Theymaybeappliedtothesubstrateintheformof solution,dispersions,powders,orsolventfreepreparations. NOTE Thismaybedifferenttothedefinitionwhichisexpectedtobeinclude
42、dinCommissionDirective90/128/EECwhen itsscopeisextendedtoincludepolymericcoatingsCEN/TS14235:2002(E) 7 3.2 finalarticle articleinitsreadyforusestateorassold 3.3 sample materialorarticleunderinvestigation 3.4 testspecimen portionofthesampleonwhichatestisperformed 3.5 testpiece portionofthetestspecime
43、n 3.6 conventionaloven ovenwheretheairwithintheovenisheatedandthisheatisthentransferredtothefoodthroughthefinalarticleas opposedtoamicrowaveovenwherethefooditselfisheateddirectlybymicrowaveirradiation 3.7 foodsimulant mediumintendedtosimulateafoodstuff(seeclauses3and4) 3.8 migrationtest testforthede
44、terminationofoverallmigrationusingfoodsimulantsunderconventionaltestconditions 3.9 substitutetest testcarriedoutwhichusestestmediaunderconventionalsubstitutetestconditionswhentheuseofamigration testisnotfeasible 3.10 testmedia substancesusedin“substitutetests“,isooctane,95%ethanolinaqueoussolutionandmodifiedpolyphenylene oxide 3.11 alternativetest tests,withvolatilemedia,thatmaybeusedinsteadofmigrationtestswithfattyfoodsimulants 3.12 extractiontests testsinwhichmediahavingstro
