DSCWord格式.docx
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特别提示
•样品台及温度探头勿受金属等硬物刮擦!
•温度高限不能超过仪器限制，如500℃！
•除非十分必要，不做分解温度测试。
•仪器运行中须经常检视
•热物件放置右侧黑色平台上
耐热平台
样品准备
•准确称量3-10mg，放置坩埚底部使成薄层
•放上埚盖，以镊子轻压，再转移至压盖器
•分多次轻轻试压，将埚盖压紧至最低位置
•最终坩埚底部不变形、呈平面！
坩埚
坩埚盖
压盖器
开机准备
•打开稳压器及仪器电源开关
•开启气体钢瓶总阀，调出口压0.05MPa
•点击TAInstrumentExplorer，等出现仪器界面后，再点击其图标，出现操作界面
①仪器图标
②仪器启动后界面
③操作界面
程序设置
•将压好的样品埚置样品平台上（靠自己一方）
•按由里到外顺序盖好三个盖子
•在软件界面实验视窗中，输入有关信息：
•Summary的填写：
–Proceduresummary中→选择standard;
custom
–Sample中→输入样品名称;
质量
–Datafilename中→建立个人数据的位置
点Summary
点Procedure
点Notes
•Procedure的填写:
–Procedureinformation中→选custom；
其它
–Method[1]：
•编写方法：
点击Editor，删除原有语句，双击右侧segmentlist中合适命令组织方法，点击各命令的数字，激活后填写预定数据，如实验开始温度、稳定时间、加热速率及实验结束温度等，核查无误。
•选择现成的方法（除Custom外的其它方法）
Notes的填写：
氮气流量20（-50）ml/min
典型的升温程序
程序运行
•点击左上侧图标，开始运行。
•程序运行中，右下侧视窗实时显示热流变化。
•设定程序完成后，运行自动终止，停止升温
•点击左上侧图标，可随时终止运行。
•程序结束后，在菜单栏control中，点击stop。
数据分析
•点击图标TAuniversalanalysis，打开数据分析界面。
•点击界面上方的分析模式，进行分析。
–可先用鼠标画框，选定相关区域，放大后进行
•峰面积计算
–要根据相关知识，选择合适的基线种类再积分，如线形、曲线等。
–调整积分前后两个端点到适当位置
–在空白区右击鼠标，选择acceptlimits，得结果
数据导出
•打开一个数据文件
–菜单file中，找到exportdatafile，选择需要的数据如filesignalsonly
–在弹出的界面里，选择文件格式与字符类型，如spreadsheettextfile、OEM。
–点击finish完成最终导出
整理
•将天平、压盖器、镊子、样品勺等物品清理干净。
•将坩埚收好
•等温度降至室温，可关闭电源及气体，结束实验。
附录
•关于加热程序编写方法的说明
（1）自己编写即custom的方法，需要熟悉各种命令的意义，请参见附件segmentlist.
（2）选用预先编好的程序，即下拉菜单中除custom以外的方法，使用时一定要参照附件segmentlist。
（3）实验中一些具体的细节听熟悉的人指导。
附segmentlist
Asegmentisapreprogrammedseriesofinstructionsusedinamethod.Severalsegmentscanbelinkedtogethertocreatethedesiredmethod.Theavailablesegmentlistwillvarydependingontheinstrumentandoptionalaccessoriesinstalled.
Fordetailsonaspecificsegmentseethetablebelow:
Segment
Description
Abortnextsegmentonlimit
AvailableforDSC,TGA,andSDTOnly:
TheAbortnextsegmentonlimitsegmentallowsyoutoskipoverorterminateothermethodsegmentswhenspecifiedlimitconditionsaremet.Thentheexperimentproceedstothenextsegment.
∙Ifthelimitisreachedatthebeginningofasegment,thenthatsegmentisskippedandmethodexecutioncontinueswiththenextsegment.
∙Ifthelimitisreachedduringtheexecutionofasegment,thentheremainingportionofthesegmentisskipped.
NOTE:
TheAbortsegmentisgenerallyfollowedbyaRamp,orIsothermalsegment.
Example（DSC）:
1.Equilibrateat200°
C
2.AbortnextsegmentifmW>
1
3.Isothermalfor100min
Abortnextsegmentonsignal
AvailableforDMAandTMAOnly:
TheAbortnextsegmentonsignalsegmentallowsyoutoskipoverorterminateothermethodsegmentswhenspecifiedlimitconditionsaremet.Thentheexperimentproceedstothenextsegment.Thesignalspecifiedforlimitcheckingcanbeanysignalthatisbeingsavedintothedatafile.
Example（DMA）:
1.Equilibrateat100°
2.AbortnextsegmentifStorageModulus<
1000Mpa
3.Ramp5°
C/minto200°
4.Isothermalfor10min
5.Ramp5°
C/minto100°
AirCool
AvailableforDSCOnly:
TheAirCoolsegmentcontrolstheinternalcoolingsolenoidvalveconnectedtocompressedair（aircoolfeature）.Aircoolactivateswhenthefurnaceisbelow600°
C.
Example:
AirCool:
On
Datastorage
TheDatastoragesegmentcontrolsdatacollectionduringtheexperiment.IfaDataStoragesegmentisnotused,datastoragewillbeautomaticallyinitiatedbythefirstRamp,Isothermal,orStepsegmentthatappearsinthemethod.
DataStorage:
Equilibrate
Backtotop
TheEquilibratesegmentheatsorcoolsthefurnacetothedefinedtemperature,stabilizesthefurnaceatthattemperature,thencontinuestothenextsegment.Thissegmentdoesnotautomaticallystartdatacollection.
Equilibrateat200°
ExternalEvent
TheEventsegmentcontrolstheexternaleventrelaythroughtheeventjackonthebackoftheinstrument.Thisisusedtosynchronizecontrolofadditionalhardwarethroughthemethod.
ExternalEvent:
FillCooler
AvailableforDMAandDSCOnly:
ThissegmentisusedtocontrolthefillingoftheGasCoolingAccessory（GCA）orLiquidNitrogenCoolingSystem（LNCS）whenitfallsbelowanenteredpercentageduringanexperiment.
FillCoolerifbelow50%
FlowRate
AvailableforMFCOnly:
TheFlowRatesegmentisusedtoaltertherateofflowoftheselectedgaswhenaninstrumentisequippedwithaMassFlowController.
Flowrate50mL/min
Force
AvailableforDMAOnly:
TheForcesegmentappliesaconstantstaticforcetothesample,thenexecutesthenextsegment.ThissegmentisonlyvalidforexperimentsdoneintheControlledForceandStrainRatemodes.
TheForcesegmentintheStrainRatemodeshutsoffdisplacement（strain）controlwhenthissegmentisexecuted.ExecutingasubsequentSetStrainorRampStrainsegmentshutsoffforcecontrolandresumesdisplacement（strain）control.
Force0.5N
FrequencySweep
TheFrequencySweepsegmentisusedinmultiplefrequencyexperimentstocollectdataateachfrequencyintheselectedfrequencytableataconstanttemperature.ThissegmentisonlyvalidforDMAMultifrequencymode.
Thissegmentturnsondatastoragewhenitbegins,andturnsitoffwhenitends.
GasSelection
AvailablewiththeMFCOnly:
TheGassegmentcontrolstheswitchingofgas,betweenGas1andGas2foraninstrumentwithaMassFlowController（MFC）installed.Thissegmentisusedtosynchronizegasswitchingataspecifictimeortemperatureinanexperiment.
SelectGas1
HeaterPID
TheHeaterPIDsegmentisusedtochangetheperformanceoftheinstrumentfurnaceduringtheexecutionofathermalmethod.PIDstandsforProportional,Integral,andDerivative,thethreemodesoftraditionaltemperaturecontrol.TheHeaterPIDsegmentspecifiesthecontrolcoefficientsforeachmodeoftemperaturecontrol.
Formoredetailedinformation,clickhere
more.
P=35
I=70D=2
HighResolutionramp
AvailableforTGAHighResolutioninstrumentsonly.TheHighResolutionrampsegmentvariestheheating/coolingrateofthefurnaceinresponsetochangesintherateofdecompositionofthesampletoimproveweightchangeresolution.
Ramp50.00°
C/minres4.0to800.00°
HighResolutionsensitivity
AvailableforTGAHighResolutioninstrumentsonly.TheHighResolutionsensitivitysegmentsetsanadditionalparameterassociatedwiththeHighResolutionrampsegments,whichcanbeusedtoadjusttheresponseoftheHighResolutiontemperaturecontrolalgorithm.Thisissometimesnecessaryduetothewidevariationindecompositionmechanismsoftypicalsamplematerials.Thesensitivitysettingisaunitlessnumberrangingfrom1.0（lowestsensitivity）to8.0（highestsensitivity）.Increasingsensitivitytendstoincreaseexperimenttime.
Highresolutionsensitivity2.0
IncrementForce
TheIncrementForcesegmentraisesorlowersthestaticforceinastep,thenexecutesthenextsegment.Thissegmentisonlyvalidforexperimentsdoneincontrolledforcemode.
1.Equilibrateto50°
2.Isothermalfor5min.
3.Incrementforce0.05N
4.Repeatsegment2for3times
IncrementTemperature
TheIncrementTemperaturesegmentraisesorlowersthetemperatureinacontrolledstep,letsthetemperatureequilibrate,thenbeginsthenextsegment.
Incrementby5°
Initialtemperature
TheInitialTemperaturesegmentheatsorcoolsthefurnacetothedefinedtemperature,stabilizesthefurnaceatthattemperature,thenholdsthetemperatureuntiltheexperimentiscontinuedbyselectingResumeontheToolBarormenu,orpressingSTARTontheinstrumentkeypad.Theinstrumentstatuswilldisplay"
ready"
whenthetemperatureisstabilized.Thissegmentdoesnotautomaticallystartdatacollection.
InitialTemp200°
Isostrain
TheIsostrainsegmentappliesaninstantaneousstraintothesampleandtheforcerequiredtomaintainthestrainataconstantvalueismonitored.
1.Equilibrate30°
2.Isostrainat1%
3.Ramp3°
Isothermal
TheIsothermalsegmentholdsthesampleatthecurrenttemperature（asprogrammedbytheprevioussegment）foradefinedperiodoftime.Thissegmentautomaticallyturnsondatacollection,exceptwhenprecededbyaDataStorageOFFsegment.
Isothermalfor10min
Jump
TheJumpsegmentinstantlychangesthesetpointtemperature,causingballisticchangesinthesampletemperature.Thissegmentthenallowstheimmediateexecutionofthenextsegment（whichisusuallytheIsothermalsegment）.Notethatlargetemperatureovershootsmayresultfromtheuseofthissegment.Thissegmentdoesnotautomaticallystartdatacollection.
Jumpto200°
Markendofcycle
TheMarkendofcyclesegmentplacesamarkerinthedataforusebythedataanalysisprograms.Ingeneralmarkersprovidequickparsingofdatatoseparateexperimentalsegments（i.e.,theheat-coolcycle）.Acyclemarknumberof0willautomaticallyincrementthemarknumbereachtimeitisused,providingarunningcyclecount.
Markendofcycle0
Modulatetemperature
AvailableforModulatedInstrumentsOnly:
Thissegmentallowsyoutoent
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