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1、1,SynchronousThermalAnalyzer同步热分析仪(STA),2,Introduction,Contents,1,Principle,2,Structure,3,Operation&Maintenance,4,Application,5,3,Introduction,ThermalAnalysis(TA)STAisbasedonthermalanalysis1915Japan本多光太郎thermo-balance(热天平)Recentyearscontrolledbycomputer、highautomationandmorepreciseCombinationwithoth
2、erinstrumentsTG-MS、TG-GC、TG-FTIRetc.,4,Introduction,MassThermogravimetry(TG)DifferentialThermogravimetry(DTG)TemperatureHeating-curveDetermination(HCD)DifferentialThermalAnalysis(DTA)EnthalpyDifferentialScanningCalorimetry(DCS),5,Principle,TGAtacertaintemperature,theweightofthematerialwillchangebeca
3、usesomeingredientsofthesubstancewillbedecomposedorremoved.TGisusedtomeasuretherelationshipbetweentheweightofmaterialandtemperaturechangesunderprogram-controlledtemperaturechange.Thermogravimetriccurveisrecorded,qualityastheordinateandtemperatureasabscissa.m=f(T或t)DTGDifferentialthermogravimetriccurv
4、e(DTGcurve)isobtainedbydifferentialprocessingofTGcurve.dm/dt=f(T或t),6,ThermalbalanceThermalbalanceisthemostimportantpartoftheSTAinstrument.Theprincipleofthermalbalanceissimilarwithwhichofbalance.Itcanmeasuretheweighofsamplecontinuouslyintheconditionofheatingandrecordtherelationshipbetweenchangesofsa
5、mpleweightandtemperaturecontinuously.,Principle,7,Structure,STA同步热分析仪,Heatingfurnace,Controlsystemoftemperature,Thermalbalance,Massflowmeter,Signaldetectionandrecordsystem,8,Operation,Weighingsamples,Program,1Specialcrucible2100.1mg3ZerosampleWeighsample,1Initialstate2Purgegas3Temperatureprogramwith
6、gasswitch,OnandOFF,1Turnon/Offallinstruments2Open/Closethegascylinder3Connect/Disconnectthecomputer,9,attention,Maintenance1.Useethanoloracetonetowipetheinsidesurfaceofthefurnace.2.Runtheheatingprogramto900withnosampleanduseairasthepurgegas.3.Washthecylindersusingultrasoniccleaner,theheatthemat900.4
7、.Replacetheglasscottonpiece.,No.1Keeptheoutersurfaceofthecrucibleclean.No.2Dontsprinklethesampleontheoutside.No.3Dontturnofftheinstrumentwhenthesampletemperatureishigherthan100.No.4etc.,Maintenance,10,Application,TG,1.Processandmechanismofthermaldecompositionreaction.2.Crystalwater,absorbedwaterandw
8、aterremoval.3.Reactionsbetweensolidandgas.4.Analysisofcompositionofsubstances.Andsoon.,DTG,ThedifferencebetweenTGandDTGisthatsignalsarehandleddifferently.DTGcurveispeakycurveandthepointatthepeakmaximumiscorrespondingtotheinflectionpointofTGcurve.Therateofthereaction.,11,Questions&answers,1.使用这台仪器时是否
9、需要参比物?答:不需要。仪器中只有一个天平,只需将样品放入其中即可。2.升温速率范围是多少,不同升温速率对TG有什么影响?答:升温速率5-100/min。不同的升温速率对样品的传热有影响,升温速率越快,样品温度与设定温度之间的延迟越大,在某一温度段的停留时间越短。通常升温速率在10-30/min比较合适。3.这台仪器可否测热量变化,与DSC的区别是什么?答:可以,在数据中选择热量即可。数据与DSC基本相同,可以得到物质的吸、放热数据。4.热重谱图如何分析?答:热重谱图应包括TG、DTG和热量曲线。TG曲线是阶梯式的,应按阶段分析;DTG曲线是峰形曲线,可以观察最大峰值;热量曲线可以分析样品的吸、放热性质。这三条曲线应该配合起来一起分析。,12,Thankyouforyourattention!,谢谢,