DSC 热分析仪培训资料

DSC６２００DSCBasicsBasicTrainingOutlineTheory/Design(Basic)InstallationInstallationProceduresHardwareSoftwareBasicAccessoriesOperationCalibrationTroubleshootingDSC(DifferentialScanningCalorimetry)Athermalanalysistechniquewhichmonitors/measurestheenergyabsorbedorliberatedfromamaterialasitissubjectedtoatemperatureprofileIsothermalorprogrammedheat/coolAllSeikoDSC’sareheatfluxinstrumentswheretheΔTbetweenthesampleandreferenceismeasuredandconvertedtoenergyunitsSampleTCReferenceTCControlTCConventionsEndothermsdownSampleonrightSIINanotechnologyDSCOperationTheoryDSCComponentsHeaterFurnaceandwindingsControlthermocoupleTemperatureSensorSensestemperatureSamplethermocoupleReferencethermocoupleHeatSinkCoverInsulatingCoverDSCDSC6200TwoconfigurationsStandardShipswithMUSEF/WAutosampler(ASD-2)ShipswithMUSEF/WInstallationConnectcablesConnectpurgegasConnectperipheriesInstallandalignAS(ifapplicable)ConnectcomputercomponentsInstallMuse/ExstarPerforminstallationprotocolchecksSignoffDSCInterconnectsAutosamplerCableComputerConnectionAutomaticCoolingAccessory(LN2)AirCoolingAccessoryDSCwithAutosamplerBaseUnitMeasurementHeadAutosampler(ASD-2)AutosamplerMountingBracketPressAdjustbuttonwhilepressingpowerontoactivatethealignmentprocedureDSCMeasurementCellModelsDSC6200OvalSensorConstantandiskSilverdiskChromel/AlumelTCDSCSensor(OvalSensor)PurgegasinletSampleTC~7.8ohmsReferenceTCCombineswithSample~12.0ohmsControl(Furnace)TC~10.6ohmsHeater~54.4ohmsDSCMeasurementHeadElectronics1)DSWCard2)CJT60Board3)DDT2ΔTBoard123DSCFurnaceDSC6200/DSC(SensorConstantan)TemperatureRange:-150to725oCMeasurementRange(Sensitivity):+/-100mW(0.4μW)AutoCoolingAccessory(LN2)ElectricalCooling(RefrigerationUnit)AutoAirCooling(GasCooling)DSCBaseUnitElectronicsLeftSideMotherBoardRightSideTASwitchBoardFirmwarechipsetASD-2InstallationInstallASD-2ontopofDSCSecurewithmountingbracketAlignfronttobackusingstringTightenbracketAlignASpositionsASD-2“AdjustingtheTransport

System”Placesamplepanontray(Position1)PlaceInnerLidandOuterLidontotheirrespectivestandsTurnonpowertotheASsimultaneouslyholdingthe[Adjust]button.AdjustpositionsInnerlidPick-upFurnaceplacementReturnOuterlidPick-upFurnaceplacementReturnSampleposition(Tray)131Sampleposition(Sensor)Referenceposition(Furnace)PanreceptacleFinish[OK](NOTE:ForcompletedetailsrefertotheusersmanualSection4.4.4)DSCPurgeGasesInert(N2orAr)RecommendedOxidative(O2orAir)O.K.butoxidationofmaterialscanoccurRecommendedflowrate20–60mL/minFlowsratesareverysimilartheDiamondDSCVerydifferentfromtheDiamondTGDTA,TMAandDMADSCCalibrationTemperature

PrecalibrationTemperaturePrecalibrationNotnormallyrequiredoninstallation(doneatfactoryandvaluesareretainedinbatterybackedRAM)ErasePrecalvaluesbyremovingbatteriesandpoweroffVerifycorrectPIDvaluesaresetintheCalibrationWindowMatchesprogramtemperatureandsampletemperaturekeepingthedifferenceatminimumduringanexperimentPrecalibrationmethodmustcontainaminimumof7stepsWhenpurgegasisusedPrecalshouldbeperformedusingsameconditionsasexperimentalconditionsWhenusingacoolanti.e.Cjacket,thePrecalshouldbeperformedusingthecoolantandatsubambienttemperaturesRefertoo“DifferentialScanningCalorimeterMeasurementProcedureOperationsManual”DSCAdvancedSoftwareFeaturesformoreinformationDSCCalibrationVerifyPIDvaluesarecorrectfortheanalyzeri.e.DSC6200VerifyallcalibrationcorrectionsaresettodefaultvaluesDSCBaselineCorrectionCorrectsforaslopingorcurvedbaselineIfnecessary,thisshouldbedonebeforethetemperatureandheatflowcalibrationsCollectdataforIndiumandTinandcalculatetheonsetandheatoffusionvalues“TemperatureCorrection”usingtheonsetvaluesobtained“DSCSensitivityCorrection”usingtheheatflowvaluesobtainedNOTES:Indiumshouldbeheatedoncetoconditionthe sampleTinshouldonlybeusedonceItisbesttoruntinfirstthenindium,leavingtheindiuminplaceforverificationRefertoo“DifferentialScanningCalorimeterMeasurementProcedureOperationsManual”DSCCalibrationformoreinformationDSCInstallationChecklistComponentItemDescriptionExterior

Housing

Paint,scratchesetc.

Label

ControllabelsAuxillarypartsInstallation

Cables

Baseunittomeasurementhead,baseunit-computer

Gastubing

Gasandgassupply

Level

AnalyzerlevelFunctionsMeasurementOperatespersettingsAnalysisOperatespersettingsFileManagerOperatespersettingsCoolingJacket(C)CoolsPerformanceIndiummeasurementTemperature&HeatFlow156.6+/-0.2oC28.45+/-0.3J/gDocumentationManualsDSCOQChecksParameterSpecificationActualValueIndiumvaluefor:J/gram28.45+/-0.3Temperatureonset156.6+/-0.2Noise@200oC8uWRMSBaselinerepeatabilityuW100DSCOperationStandardDSCiscontrolledusingtheMUSESoftwareinstrumentcontrolsoftwareAutosampleroperationisavailablewiththeMUSESoftwareinstrumentcontrol(Version2.9)ExperimentsmustberuninNormalTemperatureControlModeDataanalysiscanbeperformedwitheitherMUSEorExstarApplicationsMeltingGlasstransitionHeatcapacityCuringOxidativeinductionDSCTypicalResultsDSCTypicalResultsTroubleshootingPower“On”LampLampdoesnotlightwhenpowerswitchpressedLampisburnedoutShortin5VlineTroubleshootingLCDDisplayLCDdoesnotlightBadLCDCables,badconnection,badcableIForCPUboardsBadconnectionatmotherboardBadboardsLCDbrightnesssetincorrectly12VPowerSupplyTroubleshootingCommunicationsNocommunicationwithstation(computer)SignalcableIFboardCPUboardJumperpinsonCPU15VPowerSupplyIncorrectfirmwareBadcommunicationsportTroubleshootingTemperatureSampleandControlTemperaturesnear0oCSW2SwitchonCJTis“OFF”ControlTemperatureapproximately700oCSW1onCJTboardsetto“No”,shouldbeatAGCpositionNeithersampleorcontroltemperatureschangeafterstartFurnaceheaterwireBrokenpinsBadconnectionBrokenwireBadIFboardBadenamelresistorSampletemperaturedoesnotchangeThermocoupleWeldislooseSampletempsensingTCisshortedinsidethefurnaceCircuitonsamplesideofCJTboardisbadSampletempsensingwirenotsolderedtoCJTboardTroubleshootingTemperatureControltemperaturedoesn’tchangeafterstartThermocoupleweldlooseTemperaturecontrolthermocouplesensingwirebrokeninfurnaceBadcircuitoncontrolsideofCJTboardControlsignalwirenotsolderedtoCJTboardTemperatureballisticallyheatsSeeabove“Controltempdoesn’tchange”BadTRIAC30oCormoredifferencebetweenProgramTemperatureandSampleTemperatureProgramHeatingratetoofast(<20oC/minute)Protectiontemperaturelimit(toolow)CalibrationvaluesincorrectCJTboardbadorSW2isoffBadIFboardSampletemperatureisbelow-100oCorabove600oC(typical)TroubleshootingTemperatureSampleTemperaturedoesn’tfollowProgramTemperatureRatei.e.Programrate20oC/minuteandsampletemprateis15oCCJTboard,linearityofMAZ-02onCJTboardisbadIFboardbadFurnacebadCalibrationincorrect(T.gain)Sampletemperaturenonlinear(curves)CJTboardbadIFboardbadCPUboardbad“ControlTempHigh”/”ControlTempLow”BadCJTboardBadIFboardBadcontrolT/C“SampleTempHigh”/”SampleTempLow”BadCJTboardCN1onCJTislooseBadIFboardBadCPUboardBad15VPowerSupplyTroubleshootingHeatFlowSignalDSCSignaldoesn’tdisplayonCRTDisplayscaletoolarge(insensitive)Calibration-DSCSpanincorrectDeltaTboardBadCN1looseIFboardbadFurnaceDSCdetectorthermocouplebrokenSensordiscdirty/corrodedNoisegreaterthan10uWandnotcyclicalSilvercover(innercover)MissingWarpedPositionDeltaTboardbadSensorbadIFboardbadPurgegasratetoohighTroubleshootingHeatFlowSignalNoisecyclicalBadconnectionbetweencontrolTCandfurnaceheatsinkSampleandcontrolwirescrossedonCJTboardDSCsignalandheaterwiresaretoocloseSignalnoisehighatlowtemperaturesGasinletnotcappedFoilaroundTC’smissingNoKaoWoolatbottomofheatsinkPeaks~0oCGasinletnotcappedGassupply/tubeNotdryLooseIncorrecttube(permeabletoatmosphere)WatercondensationinthefurnaceTroubleshootingHeatFlowSignalUnusualpeaksinDSCSignalSamplespilledontosensordiscDebrisinheatsinkBadsensorUnusualshiftinthesignalSampleplatescrewslooseDebrisinheatsinkBadsensorTroubleshootingOther“NGAGC1or2”IFboardBadConnection“Down”CPUboardbadMeasureddatawillnotgointoRAMNotenoughdatapoints(greaterthan200)DatastoreintempprogramnotselectedMeasurementtimelessthan2minutesMeasurementwon’tstartKeyboardlockedRAMisfullASD-2,resetadefaultcalibrationbypressingthepowerswitchand[Grip]and[Adjust]buttonssimultaneously.Releasethebuttonsassoonastheybegintoflash.Continuingtoholdthebuttonscancauseamalfunctioninthesystem.TroubleshootingASD-2AutosamplerErrorLEDFlashes(Autosampler)CableonbackofautosamplernotconnectedDSCpowernotonTransportarmorgripmechanicalfailureMessagesdisplayedinS/WCommunicationserror…ASnotonCablenotconnectedMeasurementstopped“containerdropped”ArminwrongpositionSamplepanincorrectposition(notfound)DeformedpanMeasurementstopped“liddropped”LidnotincorrectpositionTransportpositionnotcorrectMeasurementstopped“mechanicalerror”MechanicalfailureBlockageTroubleshootingCJT60/MotherBoard

TestPoints

SampleTC

ControlTC

ProgramTemperature(℃)30100300ProgramTemperature(℃)30100300ControlTemperature(℃)---------------ControlTemperature(℃)29.999.5298.1SampleTemperature(℃)31.3101.1298.6SampleTemperature(℃)---------------CJT60BoardIN(Inputside)VoltagebetweenTP5andTP6(mV)0.200mV3.000mV