DSC.docx
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DSC
DSC操作说明
目 录
•关于样品
•特别提示
•样品准备
•开机准备
•程序设置
•程序运行
•数据分析
•数据导出
•整理
关于样品
•样品预先按照正确方法处理好,如:
–去除不需要的水分
–玻璃化温度测定前,稳定24小时
–形态尽量为粉末状
•样品有无爆炸性需特别注意!
–不做爆炸性物,及含能粒子物,如ClO4-
–不清楚时需预先检验,如少量样品烧灼或锤击
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.
∙Ifthelimitisreachedatthebeginningofasegment,thenthatsegmentisskippedandmethodexecutioncontinueswiththenextsegment.
∙Ifthelimitisreachedduringtheexecutionofasegment,thentheremainingportionofthesegmentisskipped.
Example(DMA):
1.Equilibrateat100°C
2.AbortnextsegmentifStorageModulus<1000Mpa
3.Ramp5°C/minto200°C
4.Isothermalfor10min
5.Ramp5°C/minto100°C
AirCool
AvailableforDSCOnly:
TheAirCoolsegmentcontrolstheinternalcoolingsolenoidvalveconnectedtocompressedair(aircoolfeature).Aircoolactivateswhenthefurnaceisbelow600°C.
Example:
AirCool:
On
Datastorage
TheDatastoragesegmentcontrolsdatacollectionduringtheexperiment.IfaDataStoragesegmentisnotused,datastoragewillbeautomaticallyinitiatedbythefirstRamp,Isothermal,orStepsegmentthatappearsinthemethod.
Example:
DataStorage:
On
Equilibrate
Backtotop
TheEquilibratesegmentheatsorcoolsthefurnacetothedefinedtemperature,stabilizesthefurnaceatthattemperature,thencontinuestothenextsegment.Thissegmentdoesnotautomaticallystartdatacollection.
Example:
Equilibrateat200°C
ExternalEvent
TheEventsegmentcontrolstheexternaleventrelaythroughtheeventjackonthebackoftheinstrument.Thisisusedtosynchronizecontrolofadditionalhardwarethroughthemethod.
Example:
ExternalEvent:
On
FillCooler
AvailableforDMAandDSCOnly:
ThissegmentisusedtocontrolthefillingoftheGasCoolingAccessory(GCA)orLiquidNitrogenCoolingSystem(LNCS)whenitfallsbelowanenteredpercentageduringanexperiment.
Example:
FillCoolerifbelow50%
FlowRate
AvailableforMFCOnly:
TheFlowRatesegmentisusedtoaltertherateofflowoftheselectedgaswhenaninstrumentisequippedwithaMassFlowController.
Example:
Flowrate50mL/min
Force
AvailableforDMAOnly:
TheForcesegmentappliesaconstantstaticforcetothesample,thenexecutesthenextsegment.ThissegmentisonlyvalidforexperimentsdoneintheControlledForceandStrainRatemodes.
TheForcesegmentintheStrainRatemodeshutsoffdisplacement(strain)controlwhenthissegmentisexecuted.ExecutingasubsequentSetStrainorRampStrainsegmentshutsoffforcecontrolandresumesdisplacement(strain)control.
Example:
Force0.5N
FrequencySweep
AvailableforDMAOnly:
TheFrequencySweepsegmentisusedinmultiplefrequencyexperimentstocollectdataateachfrequencyintheselectedfrequencytableataconstanttemperature.ThissegmentisonlyvalidforDMAMultifrequencymode.
Thissegmentturnsondatastoragewhenitbegins,andturnsitoffwhenitends.
GasSelection
Backtotop
AvailablewiththeMFCOnly:
TheGassegmentcontrolstheswitchingofgas,betweenGas1andGas2foraninstrumentwithaMassFlowController(MFC)installed.Thissegmentisusedtosynchronizegasswitchingataspecifictimeortemperatureinanexperiment.
Example:
SelectGas1
HeaterPID
TheHeaterPIDsegmentisusedtochangetheperformanceoftheinstrumentfurnaceduringtheexecutionofathermalmethod.PIDstandsforProportional,Integral,andDerivative,thethreemodesoftraditionaltemperaturecontrol.TheHeaterPIDsegmentspecifiesthecontrolcoefficientsforeachmodeoftemperaturecontrol.
Formoredetailedinformation,clickhere
more.
Example:
P=35 I=70D=2
HighResolutionramp
AvailableforTGAHighResolutioninstrumentsonly.TheHighResolutionrampsegmentvariestheheating/coolingrateofthefurnaceinresponsetochangesintherateofdecompositionofthesampletoimproveweightchangeresolution.
Example:
Ramp50.00°C/minres4.0to800.00°C
HighResolutionsensitivity
AvailableforTGAHighResolutioninstrumentsonly.TheHighResolutionsensitivitysegmentsetsanadditionalparameterassociatedwiththeHighResolutionrampsegments,whichcanbeusedtoadjusttheresponseoftheHighResolutiontemperaturecontrolalgorithm.Thisissometimesnecessaryduetothewidevariationindecompositionmechanismsoftypicalsamplematerials.Thesensitivitysettingisaunitlessnumberrangingfrom1.0(lowestsensitivity)to8.0(highestsensitivity).Increasingsensitivitytendstoincreaseexperimenttime.
Example:
Highresolutionsensitivity2.0
IncrementForce
AvailableforDMAOnly:
TheIncrementForcesegmentraisesorlowersthestaticforceinastep,thenexecutesthenextsegment.Thissegmentisonlyvalidforexperimentsdoneincontrolledforcemode.
Example:
1.Equilibrateto50°C
2.Isothermalfor5min.
3.Incrementforce0.05N
4.Repeatsegment2for3times
IncrementTemperature
TheIncrementTemperaturesegmentraisesorlowersthetemperatureinacontrolledstep,letsthetemperatureequilibrate,thenbeginsthenextsegment.
Example:
Incrementby5°C
Initialtemperature
Backtotop
TheInitialTemperaturesegmentheatsorcoolsthefurnacetothedefinedtemperature,stabilizesthefurnaceatthattemperature,thenholdsthetemperatureuntiltheexperimentiscontinuedbyselectingResumeontheToolBarormenu,orpressingSTARTontheinstrumentkeypad.Theinstrumentstatuswilldisplay"ready"whenthetemperatureisstabilized.Thissegmentdoesnotautomaticallystartdatacollection.
Example:
InitialTemp200°C
Isostrain
AvailableforDMAOnly:
TheIsostrainsegmentappliesaninstantaneousstraintothesampleandtheforcerequiredtomaintainthestrainataconstantvalueismonitored.
Example:
1.Equilibrate30°C
2.Isostrainat1%
3.Ramp3°C/minto200°C
Isothermal
TheIsothermalsegmentholdsthesampleatthecurrenttemperature(asprogrammedbytheprevioussegment)foradefinedperiodoftime.Thissegmentautomaticallyturnsondatacollection,exceptwhenprecededbyaDataStorageOFFsegment.
Example:
Isothermalfor10min
Jump
TheJumpsegmentinstantlychangesthesetpointtemperature,causingballisticchangesinthesampletemperature.Thissegmentthenallowstheimmediateexecutionofthenextsegment(whichisusuallytheIsothermalsegment).Notethatlargetemperatureovershootsmayresultfromtheuseofthissegment.Thissegmentdoesnotautomaticallystartdatacollection.
Example:
Jumpto200°C
Markendofcycle
TheMarkendofcyclesegmentplacesamarkerinthedataforusebythedataanalysisprograms.Ingeneralmarkersprovidequickparsingofdatatoseparateexperimentalsegments(i.e.,theheat-coolcycle).Acyclemarknumberof0willautomaticallyincrementthemarknumbereachtimeitisused,providingarunningcyclecount.
Example:
Markendofcycle0
Modulatetemperature
AvailableforModulatedInstrumentsOnly:
Thissegmentallowsyoutoent