Diamond DSC 实用培训手册(新)

PyrisDiamondDSCPerkinElmer--------------------------------------------------------------------------------1PyrisDiamondDSC----------------------------------------------------1PyrisSoftware5.0-----------------------------------------------------5--------------------------------------------------------------------------18---------------------------------------------------------------------------55---------------------------------------------------65-------------------------------------------------------------------------------------------67•——PyrisDiamondDSCPerkinElmer1PEDSCPEPEPEPyrisDiamondDSCICTAICTAC[1]ICTA9171(TG)(EGD)EGA2DTA3DSC45(TMA)DMA6789DifferentialScanningCalorimetryDSC•——PyrisDiamondDSCPerkinElmerDifferentialScanningCalorimeterDSCDSC∆QDSC∆T∆T∆QDSC1g30~200g-170~730-170~750()2•——PyrisDiamondDSCPerkinElmerDSCDSCDSCDSCDSCDSCDSCDSCPEDSCDSCPyrisDiamondDSCPE-170~7303•——PyrisDiamondDSCPerkinElmer4DSC30~200gDiamondDSCPyris(melting)(glasstransition)(solid-statetransition)(crystallizations)DiamondDSCzzDSCzDSCzaircurtainzDiamondDSCambientmode(subambientmode)purgegas3001DiamondDSC500/min/min10-17020-165100-135200-85300-80DiamondDSCPyrisSoftware5.0PyrisDSC•——PyrisDiamondDSCPerkinElmerPyrisSoftware5.0StartPyrisPyrisDataAnalysisPyrisPyrisConfigureAnalyzerDSCPyrisDiamondDSCDiamondDSCPyrisPyrisDSCDSCHeating(Cooling)(Equilibrating)(Holding)DSCDSCSampleTemperatureOfflineAtTemperatureAtLoadTemperatureGoToLoadCalibratingEquilibratingHoldingHeatingCooling----5•——PyrisDiamondDSCPerkinElmerStatusPanel(Controlpanel)6•——PyrisDiamondDSCPerkinElmerInstrumentViewerMethodEditorDataAnalysisPyrisPlayerPyris14SampleTempProgramTempHeatFlowElapsedTimeTimeRemainingStatusCurrentStepStepTimeAutosamplerApprox.GasFlow7•——PyrisDiamondDSCPerkinElmerPurgeGasGasPressureSampleCoverClosedOpenFurnaceControl/Start/StopGototemperatureratesDSCPyrisDiamondDSCDSC8•——PyrisDiamondDSCPerkinElmerGotoTemperatureGototemperatureratesPreferenceGotoLoadPreferenceHoldTemperatureCleanFurnace600AutosamplerControlCoverHeaterDSCDockhand10sCryoFillDSCResetMonitor9•——PyrisDiamondDSCPerkinElmerSetHeatFlowtoZero010•——PyrisDiamondDSCPerkinElmer11•——PyrisDiamondDSCPerkinElmerBrownDataCollectionFast20Standard5DiamondDSCProgramPagePre-RunActionAddanActionStartRunSwitchGasesStartRunASignalEquilibrates12•——PyrisDiamondDSCPerkinElmerSampleTemperatureProgramTemperatureHeatFlowCriterionUseaSetpointASpecifiedTimeisreachedActionoccursImmediatelySwitchGasesOKAddanEventASignalEquilibratesASpecifiedTimeisreachedActionoccursImmediatelyEditanItemDeleteanItemChangeanItemExpandAllItems13•——PyrisDiamondDSCPerkinElmerCollapseAllItems14•——PyrisDiamondDSCPerkinElmerTemperatureScanFromToRateToFromIsothermalStepScanScanIsoStepScan5Rate2ndTemp.IsothermalReps15•——PyrisDiamondDSCPerkinElmerStepScan30s~60sStepScanStepScanStepScanRepeatStepsStepscanInsertaStepAddaStepDeleteItemItemStepActionEventAddActionSwitchGasesOK16•——PyrisDiamondDSCPerkinElmerASignalEquilibratesASignalCrossesaBoundaryASpecifiedTimeisReachedActionOccursImmediatelyStopRun4NextProgramStepAddEventEndCondition17•——PyrisDiamondDSCPerkinElmer18zDSCDSC--DiamondDSCE-ZcalibrationadvancedcalibrationDSCindium(PE•——PyrisDiamondDSCPerkinElmer)1.1DSCDSCDiamondDSCAutotuneslope(curvature)10/min50~45043~512192Pyrissoftware5.01InstrumentviewermethodeditorViewCalibrate:•——PyrisDiamondDSCPerkinElmer3RestoreAllDefault.pdicOpenDefault.pdic20•——PyrisDiamondDSCPerkinElmerDefault20/min50~650AdvancedCalDefaultDefaultDefaultDefault21•——PyrisDiamondDSCPerkinElmerEnterRangeOKStartAuto22•——PyrisDiamondDSCPerkinElmerOKDSC323•——PyrisDiamondDSCPerkinElmer24StartAutoDSCChangeinautotunevalueChangetobaseline+1-11mWFine+1-0.25mWSlope+1-6.5mW3EnterValues3AcceptValues3DSCDiamondDSC50~300-5035030050501002/min100/min100125102040•——PyrisDiamondDSCPerkinElmer25/min40/min40/min100/min51020/min2.1DSConset3412•——PyrisDiamondDSCPerkinElmer3±[1]0DSConset402~3DSC00DSCDSC-2defaultonsetH∆H∆DiamondDSCPE3PEISO9000CertifiedreferencematerialsCRM26•——PyrisDiamondDSCPerkinElmer27PEindium(zinc)onset156.6419.47Pyris2003J/g156.6028.45231.8860.46327.4723.01419.47108.37585.0+0.533.26670.5+0.535.56-151.1669.45-135.064.94-87.0679.586.5431.250.00333.88-90.56140.16-56.76182.0-29.66202.09-9.65216.7328.24241.4272.1418.7475.94175.3151.64a)•——PyrisDiamondDSCPerkinElmer28125102040/min,10/min20/min0.55/min0.5b)02~3-130~0-135.06PE99%12•——PyrisDiamondDSCPerkinElmerAddStandardDeleteStandardAddStandardIndiumZincDefaultEditStandardAddStandardEditStandardStandardTemperatureExpectedMeasuredDefaultScanRateWeightOK29•——PyrisDiamondDSCPerkinElmer30AcceptStandardStartAutoStartAuto3.10.01K50305030Pyris9nine-pointcalibration8990.01K250/minholding12