EN ISO 11357-6 2025.docx

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1、ENISO11357-6June2025Plastiques-AnalyseCalorimetriquedifferentielle(DSC)-Partie6:Determinationdutempsd,inductionaFoxydation(OITisotherme)etdelatemperature(!inductionaFoxydation(OITdynamique)(ISO11357-6:2025)Kunststoffe-DynamischeDifferenzkalorimetrie(DSC)-Teil6:BestimmungderOxidations-Induktionszeit(

2、isothermischeOlT)undOxidations-Induktionstemperatur(dynamischeOlT)(ISO11357-6:2025)EuropeanstandardNormeeuropeenneEuropaischenormICS83.080.01SupersedesENISO11357-6:2018EnglishVersionPlastics-Differentialscanningcalorimetry(DSC)-Part6:DeterminationofoxidationinductiontimeisothermalOITandoxidationindu

3、ctiontemperaturedynamicOITISO11357-6:2025ThisEuropeanStandardwasapprovedbyCENon16June2025.CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEuropeanStandardthestatusofanationalstandardwithoutanyalteration.Up-to-datelistsandbibliographicalreference

4、sconcerningsuchnationalstandardsmaybeobtainedonapplicationtotheCEN-CENELECManagementCentreortoanyCENmember.ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).AversioninanyotherlanguagemadebytranslationundertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheCEN-CENEL

5、ECManagementCentrehasthesamestatusastheofficialversions.CENmembersarethenationalstandardsbodiesofAustria,Belgium,Bulgaria,Croatia,Cyprus,CzechRepublic,Denmark,Estonia,Finland,France,Germany,Greece,Hungary,Iceland,Ireland,Italy,Latvia,Lithuania,Luxembourg,Malta,Netherlands,Norway,Poland,Portugal,Repu

6、blicofNorthMacedonia,Romania,Serbia,Slovakia,Slovenia,Spain,Sweden,Switzerland,TiirkiyeandUnitedKingdom.EUROPEANCOMMITTEEFORSTANDARDIZATIONCOMITEEUROPEENDENORMALISATIONEuropaischeskomiteefurnormungCEN-CENELECManagementCentre:RuedelaScience23,B-1040BrusselsRef.No.ENISO11357-6:2025E2025CENAllrightsofe

7、xploitationinanyformandbyanymeansreservedworldwideforCENnationalMembers.ContentsPageEuropeanforeword3EuropeanforewordThisdocument(ENISO11357-6:2025)hasbeenpreparedbyTechnicalCommitteeISO/TC61PlasticsincollaborationwithTechnicalCommitteeCEN/TC249Plastics“thesecretariatofwhichisheldbySIS.ThisEuropeanS

8、tandardshallbegiventhestatusofanationalstandard,eitherbypublicationofanidenticaltextorbyendorsement,atthelatestbyDecember2025,andconflictingnationalstandardsshallbewithdrawnatthelatestbyDecember2025.Attentionisdrawntothepossibilitythatsomeoftheelementsofthisdocumentmaybethesubjectofpatentrights.CENs

9、hallnotbeheldresponsibleforidentifyinganyorallsuchpatentrights.ThisdocumentsupersedesENISO11357-6:2018.Anyfeedbackandquestionsonthisdocumentshouldbedirectedtotheusersnationalstandardsbody/nationalcommittee.AcompletelistingofthesebodiescanbefoundontheCENwebsite.AccordingtotheCEN-CENELECInternalRegula

10、tions,thenationalstandardsorganizationsofthefollowingcountriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,Bulgaria,Croatia,Cyprus,CzechRepublic,Denmark,Estonia,Finland,France,Germany,Greece,Hungary,Iceland,Ireland,Italy,Latvia,Lithuania,Luxembourg,Malta,Netherlands,Norway,Poland,Portugal

11、RepublicofNorthMacedonia,Romania,Serbia,Slovakia,Slovenia,Spain,Sweden,Switzerland,TiirkiyeandtheUnitedKingdom.EndorsementnoticeThetextofISO11357-6:2025hasbeenapprovedbyCENasENISO11357-6:2025withoutanymodification.ISOInternationalStandardISO11357-6Fourthedition2025-06PlasticsDifferentialscanningcal

12、orimetry(DSC)Part6:Determinationofoxidationinductiontime(isothermalOIT)andoxidationinductiontemperature(dynamicOIT)PlastiquesAnalyseCalorimetriquedifferentielle(DSC)Partie6:Determinationdutempsd,inductionaUoxydation(OlTisotherme)etdelatemperature(!inductionaUoxydation(OITdynamiquejReferencenumberISO

13、11357-6:2025(en)COPYRIGHTPROTECTEDDOCUMENTISO2025Allrightsreserved.Unlessotherwisespecified,orrequiredinthecontextofitsimplementation,nopartofthispublicationmaybereproducedorutilizedotherwiseinanyformorbyanymeans,electronicormechanical,includingphotocopying,orpostingontheinternetoranintranet,without

14、priorwrittenpermission.PermissioncanberequestedfromeitherISOattheaddressbeloworISO,smemberbodyinthecountryoftherequester.ISOcopyrightofficeCP401Ch.deBlandonnet8CH-1214Vernier,GenevaPhone:+4122749Ol11Email:copyrightiso.orgWebsite:www.iso.orgPublishedinSwitzerlandPageivContentsForewordIntroduction1 Sc

15、ope12 Normativereferences13 Termsanddefinitions14 Principle24.1 General24.2 Oxidationinductiontime(isothermalOITJ24.3 Oxidationinductiontemperature(dynamicOITJ25 Apparatusandmaterials2.234,5,6,7,8S5.S5.5.5.5.DSCinstrument3Crucibles3Flowmeter3Oxygen3Air3Nitrogen3Gas-selectorswitchandregulators36 Test

16、specimens46.1 General46.2 Specimensfromcompression-mouldedplates46.3 Specimensfrominjection-mouldedplatesormeltflowextrudates46.4 Specimensfromfinishedparts47 Testconditionsandspecimenconditioning58 Calibration58.1 Oxidationinductiontime(isothermalOITJ58.1.1 General58.1.2 Dynamictemperaturecalibrati

17、on58.1.3 Isothermalstepwisetemperaturecalibration58.2 Oxidationinductiontemperature(dynamicOITJ59 Procedure69.1 Settinguptheinstrument69.2 Loadingthetestspecimenintothecrucible69.3 Insertionofcrucibles69.4 Nitrogen,airandoxygenflow69.5 Sensitivityadjustment69.6 Performanceofmeasurement69.6.1 Oxidati

18、oninductiontime(isothermalOITJ69.6.2 Oxidationinductiontemperature(dynamicOITJ79.7 Cleaning810 Expressionofresults811 Precisionandbias1012 Testreport10Bibliography12ForewordISO(theInternationalOrganizationforStandardization)isaworldwidefederationofnationalstandardsbodies(ISOmemberbodies).Theworkofpr

19、eparingInternationalStandardsisnormallycarriedoutthroughISOtechnicalcommittees.Eachmemberbodyinterestedinasubjectforwhichatechnicalcommitteehasbeenestablishedhastherighttoberepresentedonthatcommittee.Internationalorganizations,governmentalandnon-governmentabinliaisonwithISO,alsotakepartinthework.ISO

20、collaboratescloselywiththeInternationalElectrotechnicalCommission(IEC)onallmattersofelectrotechnicalstandardization.TheproceduresusedtodevelopthisdocumentandthoseintendedforitsfurthermaintenancearedescribedintheISO/IECDirectives,Part1.Inparticular,thedifferentapprovalcriterianeededforthedifferenttyp

21、esofISOdocumentsshouldbenoted.ThisdocumentwasdraftedinaccordancewiththeeditorialrulesoftheISO/IECDirectives,Part2(seewww.iso.org/directives).ISOdrawsattentiontothepossibilitythattheimplementationofthisdocumentmayinvolvetheuseof（八）patent(三).ISOtakesnopositionconcerningtheevidence,validityorapplicabil

22、ityofanyclaimedpatentrightsinrespectthereof.Asofthedateofpublicationofthisdocument,ISOhadnotreceivednoticeof（八）patent(三)whichmayberequiredtoimplementthisdocument.However,implementersarecautionedthatthismaynotrepresentthelatestinformation,whichmaybeobtainedfromthepatentdatabaseavailableatwww.iso.org/

23、patents.ISOshallnotbeheldresponsibleforidentifyinganyorallsuchpatentrights.Anytradenameusedinthisdocumentisinformationgivenfortheconvenienceofusersanddoesnotconstituteanendorsement.Foranexplanationofthevoluntarynatureofstandards,themeaningofISOspecifictermsandexpressionsrelatedtoconformityassessment

24、aswellasinformationaboutISOsadherencetotheWorldTradeOrganization(WTo)principlesintheTechnicalBarrierstoTrade(TBT),seeWWW.isoQrgisoforeword.htmLThisdocumentwaspreparedbyTechnicalCommitteeISO/TC61,Plastics,SubcommitteeSC5,Physicalchemicalproperties,incollaborationwiththeEuropeanCommitteeforStandardiz

25、ation(CEN)TechnicalCommitteeCEN/TC249,Plastics,inaccordancewiththeAgreementontechnicalcooperationbetweenISOandCEN(ViennaAgreement).Thisfourtheditioncancelsandreplacesthethirdedition(ISO11357-6:2018),whichhasbeentechnicallyrevised.Themainchangesareasfollows:一theisothermalstepwisetemperaturecalibratio

26、nhasbeenaddedforisothermalOIT.AlistofallpartsintheISO11357seriescanbefoundontheISOwebsite.Anyfeedbackorquestionsonthisdocumentshouldbedirectedtotheusersnationalstandardsbody.Acompletelistingofthesebodiescanbefoundatwww.iso.org/membnrs.htmLIntroductionThemeasurementofoxidationinductiontimeortemperatu

27、redescribedinthisdocumentprovidesatooltoassesstheconformityofthematerialtestedtoagivenformulationofplasticscompounds.However,itisnotintendedtoprovidetheconcentrationofantioxidant.Differentantioxidantscanhavedifferentoxidationinductiontimesortemperatures.Duetointeractionoftheantioxidantwithothersubst

28、ancesintheformulation,differentoxidationinductiontimesortemperaturescanresultevenwithproductshavingthesametypeandconcentrationofantioxidant.PlasticsDifferentialscanningcalorimetry(DSC)一Part6:Determinationofoxidationinductiontime(isothermalOIT)andoxidationinductiontemperature(dynamicOIT)1 ScopeThisdo

29、cumentspecifiesmethodsforthedeterminationofoxidationinductiontime(isothermalOITJandoxidationinductiontemperature(dynamicOITJofpolymericmaterialsbymeansofdifferentialscanningcalorimetry(DSC).Itisapplicabletopolyolefinresinsthatareinafullystabilizedorcompoundedform,eitherasrawmaterialsorfinishedproduc

30、ts.Itcanbeapplicabletootherplastics.2 NormativereferencesThefollowingdocumentsarereferredtointhetextinsuchawaythatsomeoralloftheircontentconstitutesrequirementsofthisdocument.Fordatedreferences,onlytheeditioncitedapplies.Forundatedreferences,thelatesteditionofthereferenceddocument(includinganyamendm

31、ents)applies.ISO472,PlasticsVocabularyISO11357-1,PlasticsDifferentialscanningcalorimetry(DSC)Part1:GeneralprinciplesISO17855-2,PlasticsPolyethylene(PE)mouldingandextrusionmaterialsPart2:PreparationoftestspecimensanddeterminationOfpropertiesISO19069-2,PlasticsPolypropylene(PP)mouldingandextrusionmate

32、rialsPart2:PreparationoftestspecimensanddeterminationOfpropertiesISO21302-2,PlasticsPolybutene-I(PB-I)mouldingandextrusionmaterialsPart2:PreparationoftestspecimensanddeterminationOfproperties3 TermsanddefinitionsForthepurposesofthisdocument,thetermsanddefinitionsgiveninISO472,ISO11357-1andthefollowi

33、ngapply.ISOandIECmaintainterminologydatabasesforuseinstandardizationatthefollowingaddresses:一ISOOnlinebrowsingplatform:availableathttps:WWW.iso.org/obp一IECElectropedia:availableathttps:WWW.electropedia.org/3.1oxidationinductiontimeisothermalOITrelativemeasureofastabilizedmaterialsresistancetooxidati

34、vedecomposition,determinedbythecalorimetricmeasurementofthetimeintervaltotheonsetofexothermicoxidationofthematerialataspecifiedtemperatureinanoxygenorairatmosphere,underatmosphericpressureNote1toentry:Itisexpressedinminutes(min).3.2oxidationinductiontemperaturedynamicOITrelativemeasureofastabilizedm

35、aterialsresistancetooxidativedecomposition,determinedbythecalorimetricmeasurementofthetemperatureoftheonsetofexothermicoxidationofthematerialwhensubjectedtoaspecifiedheatingrateinanoxygenorairatmosphere,underatmosphericpressureNote1toentry:ItisexpressedindegreesCelsius().Note2toentry:Theoxidationind

36、uctiontemperatureisalsocalledoxidationonsettemperature(OOT).4 Principle4.1 GeneralThetimeforwhich,orthetemperatureuptowhich,anantioxidantstabilizersystempresentinatestspecimeninhibitsoxidationismeasuredwhilethespecimenisheldisothermallyataspecifiedtemperatureorheatedataconstantrateinanoxygenorairatm

37、osphere.Theoxidationinductiontimeortemperatureisanassessmentofthelevel(ordegree)ofstabilizationofthematerialtested.Highertesttemperatureswillresultinshorteroxidationinductiontimes;fasterheatingrateswillresultinhigheroxidationinductiontemperatures.Theoxidationinductiontimeandtemperaturearealsodepende

38、ntonthesurfaceareaofthespecimenavailableforoxidation.Itshouldbenotedthattestscarriedoutinpureoxygenwillresultinaloweroxidationinductiontimeortemperaturethantestsperformedundernormalatmospheric-airconditions.NOTETheoxidationinductiontimeortemperaturecanbeindicativeoftheeffectiveantioxidantlevelpresen

39、tinthetestspecimen.However,deviationsbetweenoxidationinductiontimeortemperatureresultsandoxidationstabilityatapplicationconditionscanoccursinceoxidationreactionkineticsareafunctionoftemperatureandtheinherentpropertiesoftheadditivescontainedinthesample.Forexample,oxidationinductiontimeortemperaturere

40、sultsareoftenusedtoselectoptimumresinformulations.Volatileantioxidantsordifferencesinactivationenergiesofoxidationreactionscangeneratepooroxidationinductiontimeortemperatureresults,eventhoughtheantioxidantscanperformadequatelyattheintendedtemperatureofuseofthefinishedproduct.4.2 Oxidationinductionti

41、me(isothermalOIT)Thespecimenandareferencematerialareheatedataconstantrateinaninertgaseousenvironment(aflowofnitrogen).Whenthespecifiedtemperaturehasbeenreached,theatmosphereischangedtooxygenorairmaintainedatthesameflowrate.Thespecimenisthenheldatconstanttemperatureuntiltheoxidativereactionisdisplaye

42、donthethermalcurve.TheisothermalOITisthetimeintervalbetweentheinitiationofoxygenorairflowandtheonsetoftheoxidativereaction.Theonsetofoxidationisindicatedbyanabruptincreaseinthespecimensevolvedheatandcanbeobservedbyadifferentialscanningcalorimeter(DSC).TheisothermalOITisdeterminedinaccordancewith9.6.

43、1.4.3 Oxidationinductiontemperature(dynamicOIT)Thespecimenandareferencematerialareheatedataconstantrateinanoxygenorairatmosphereuntiltheoxidativereactionisdisplayedonthethermalcurve.ThedynamicOITisthetemperatureoftheonsetoftheoxidativereaction.Theonsetofoxidationisindicatedbyanabruptincreaseinthespe

44、cimensevolvedheatandcanbeobservedbyadifferentialscanningcalorimeter(DSC).ThedynamicOITisdeterminedinaccordancewith9.6.2.5 Apparatusandmaterials5.1 GeneralAccordingtoISO11357-1.SUbClaUSeS5.5to5i8shallbefollowedasapplicable(subclauses5.7and5i8arerequiredonlyforoxidationinductiontimemeasurements).5.2 D

45、SCinstrumentTheDSCinstrumentshallbeabletoachieveamaximumtemperatureofatleast500.Foroxidationinductiontimemeasurements,itshallbecapableofmaintaininganisothermalstabilityof0,3Katthetesttemperatureoverthedurationofthetest,typically60min.Forhigh-precisionmeasurements,anisothermalstabilityof0,1Kisrecomme

46、nded.5.3 CruciblesSpecimensshallbeplacedinopenorclosedventilatedcruciblesthatallowunperturbedcontactwiththesurroundingatmosphere.Preferably,cruciblesshallbemadeofaluminium.Cruciblesmadeofdifferentmaterialsmaybeusedbyagreementbetweentheinterestedparties.NOTEThecompositionofthecruciblematerialcaninflu

47、encetheoxidationinductiontimeortemperaturetestresultsignificantly(thatis,includinganyassociatedcatalyticeffects).Thetypeofcontainmentsystemuseddependsontheintendedapplicationofthematerialbeingtested.Polyolefinresinsusedinthewireandcableindustrytypicallyrequirecopperoraluminiumcrucibleswhereas,forpol

48、yolefinresinsusedingeomembraneandvapour-barrierfilmapplications,onlyaluminiumcruciblesareused.5.4 FlowmeterForgasflowcalibration,aflowratemeasuringdevicesuchasarotameterorsoap-filmflowmeteroragravimetricmethodshallbeusedtogetherwithaflow-adjustingvalve.Massflowcontrollingdevicesshallbecalibratedagainstapositive-displacementdevice.NOTESuitablefactory-providedgasflowratecalibrationisalsoacceptable.5.5 OxygenTheoxygenusedshallbe