ASTM-D-3418-2015-DSC-测转变温度

Designation:D3418−15StandardTestMethodforTransitionTemperaturesandEnthalpiesofFusionandCrystallizationofPolymersbyDifferentialScanningCalorimetry1ThisstandardisissuedunderthefixeddesignationD3418;thenumberimmediatelyfollowingthedesignationindicatestheyearoforiginaladoptionor,inthecaseofrevision,theyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.Asuperscriptepsilon(´)indicatesaneditorialchangesincethelastrevisionorreapproval.ThisstandardhasbeenapprovedforusebyagenciesoftheU.S.DepartmentofDefense.1.Scope*1.1Thistestmethodcoversdeterminationoftransitiontemperaturesandenthalpiesoffusionandcrystallizationofpolymersbydifferentialscanningcalorimetry.NOTE1—Trueheatsoffusionaretobedeterminedinconjunctionwithstructureinvestigation,andfrequently,specializedcrystallizationtech-niquesareneeded.1.2Thistestmethodisapplicabletopolymersingranularformortoanyfabricatedshapefromwhichitispossibletocutappropriatespecimens.1.3Thenormaloperatingtemperaturerangeisfromthecryogenicregionto600°C.Certainequipmentallowsthetemperaturerangetobeextended.1.4ThevaluesstatedinSIunitsarethestandard.NOTE2—Thistestmethoddoesnotapplytoalltypesofpolymersaswritten(see6.8).1.5Thisstandarddoesnotpurporttoaddressallofthesafetyconcerns,ifany,associatedwithitsuse.Itistheresponsibilityoftheuserofthisstandardtoestablishappro-priatesafetyandhealthpracticesanddeterminetheapplica-bilityofregulatorylimitationspriortouse.NOTE3—ThisstandardissimilarbutnotequivalenttoISO11357-1,-2,-3.TheISOproceduresprovideadditionalinformationnotsuppliedbythistestmethod.2.ReferencedDocuments2.1ASTMStandards:2E473TerminologyRelatingtoThermalAnalysisandRhe-ologyE691PracticeforConductinganInterlaboratoryStudytoDeterminethePrecisionofaTestMethodE967TestMethodforTemperatureCalibrationofDifferen-tialScanningCalorimetersandDifferentialThermalAna-lyzersE968PracticeforHeatFlowCalibrationofDifferentialScanningCalorimetersE1142TerminologyRelatingtoThermophysicalPropertiesE1953PracticeforDescriptionofThermalAnalysisandRheologyApparatus2.2ISOStandards:3ISO11357-1Plastics—DifferentialScanningCalorimetry(DSC)—Part1:GeneralPrinciplesISO11357-2Plastics—DifferentialScanningCalorimetry(DSC)—Part2:DeterminationofGlassTransitionTem-peratureISO11357-3Plastics—DifferentialScanningCalorimetry(DSC)—Part3:DeterminationofTemperatureandEn-thalpyofMeltingandCrystallization3.Terminology3.1SpecializedtermsusedinthistestmethodaredefinedinTerminologiesE473andE1142.4.SummaryofTestMethod4.1Thistestmethodconsistsofheatingorcoolingthetestmaterialatacontrolledrateunderaspecifiedpurgegasatacontrolledflowrateandcontinuouslymonitoringwithasuitablesensingdevicethedifferenceinheatinputbetweenareferencematerialandatestmaterialduetoenergychangesinthematerial.Atransitionismarkedbyabsorptionorreleaseofenergybythespecimenresultinginacorrespondingendother-micorexothermicpeakorbaselineshiftintheheatingorcoolingcurve.Areasunderthecrystallizationexothermorfusionendothermofthetestmaterialsarecomparedagainsttherespectiveareasobtainedbythetreatmentofawell-characterizedstandard.1ThistestmethodisunderthejurisdictionofASTMCommitteeD20onPlasticsandisthedirectresponsibilityofSubcommitteeD20.30onThermalProperties(SectionD20.30.07).CurrenteditionapprovedMay1,2015.PublishedJune2015.Originallyapprovedin1975.Lastpreviouseditionapprovedin2012asD3418-12ε1.DOI:10.1520/D3418-15.2ForreferencedASTMstandards,visittheASTMwebsite,@astm.org.ForAnnualBookofASTMStandardsvolumeinformation,refertothestandard’sDocumentSummarypageontheASTMwebsite.3AvailablefromAmericanNationalStandardsInstitute(ANSI),25W.43rdSt.,4thFloor,NewYork,NY10036,*ASummaryofChangessectionappearsattheendofthisstandardCopyright©ASTMInternational,100BarrHarborDrive,POBoxC700,WestConshohocken,PA19428-2959.UnitedStates1Afnor,WEBPORTle20/04/2017à09:31Pour:TOTALASTMD3418(Revision2015):2015-05+5.SignificanceandUse5.1Thermalanalysisprovidesarapidmethodformeasuringtransitionsduetomorphologicalorchemicalchanges,inapolymerasitisheated/cooledthroughaspecifiedtemperaturerange.Changeinspecificheatcapacity,heatflowandtempera-turevaluesaredeterminedforthesetransitions.Differentialscanningcalorimetryisusedtoassistinidentifyingspecificpolymers,polymeralloys,andcertainpolymeradditives,whichexhibitthermaltransitions.Chemicalreactionsthatcauseoraffectcertaintransitionshavebeenmeasuredwiththeaidofthistechnique;suchreactionsincludeoxidation,curingofthermosettingresins,andthermaldecomposition.5.2Thistestmethodisusefulforspecificationacceptance,processcontrol,andresearch.6.Interferences6.1Differencesinheatingorcoolingrateaswellasthefinalheatingandcoolingtemperaturehaveaneffectonthemea-suredresults,especiallyontheenthalpyoffusionorcrystalli-zation.Therefore,departurefromconditionsspecifiedforagivenpolymerisnotpermitted.6.2Thepresenceofimpuritiesisknowntoaffectthetransitiontemperature,particularlyifanimpuritytendstoformsolidsolutions,ortobemiscibleinthemeltphase.6.3Uncertainradiationlossesattemperatureshigherthan400°Chavebeenknown