DSCWord格式.docx

1、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TA Instrument Explorer，等出现仪器界面后，再点击其图标，出现操作界面仪器图标仪器启动后界面操作界面程序设置 将压好的样品埚置样品平台上（靠自己一方

2、） 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： Procedure summary 中选择standard; custom Sample中输入样品名称; 质量 Data file name中建立个人数据的位置点Summary 点Procedure点Notes Procedure的填写: Procedure information中 选custom；其它 Method 1： 编写方法：点击Editor，删除原有语句，双击右侧 segment list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

3、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 TA universal analysis，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

4、当位置 在空白区右击鼠标，选择accept limits，得结果数据导出 打开一个数据文件 菜单 file 中，找到 export data file，选择需要的数据如 file signals only 在弹出的界面里，选择文件格式与字符类型，如 spreadsheet text file、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segment list.（2）选用预先编好的程序，即

5、下拉菜单中除custom以外的方法，使用时一定要参照附件segment list。（3） 实验中一些具体的细节听熟悉的人指导。附segment listA segment is a preprogrammed series of instructions used in a method. Several segments can be linked together to create the desired method. The available segment list will vary depending on the instrument and optional access

6、ories installed.For details on a specific segment see the table below:SegmentDescriptionAbort next segment on limitAvailable for DSC,TGA, and SDT Only: The Abort next segment on limit segment allows you to skip over or terminate other method segments when specified limit conditions are met. Then the

7、 experiment proceeds to the next segment. If the limit is reached at the beginning of a segment, then that segment is skipped and method execution continues with the next segment. If the limit is reached during the execution of a segment, then the remaining portion of the segment is skipped.NOTE: Th

8、e Abort segment is generally followed by a Ramp, or Isothermal segment.Example （DSC）:1. Equilibrate at 200C2. Abort next segment if mW13. Isothermal for 100 minAbort next segment on signalAvailable for DMA and TMA Only:The Abort next segment on signal segment allows you to skip over or terminate oth

9、er method segments when specified limit conditions are met. Then the experiment proceeds to the next segment. The signal specified for limit checking can be any signal that is being saved into the datafile.Example （DMA）:1. Equilibrate at 1002. Abort next segment if Storage Modulus 1000 Mpa3. Ramp 5C

10、/min to 2004. Isothermal for 10 min5. Ramp 5C/min to 100Air CoolAvailable for DSC Only:The Air Cool segment controls the internal cooling solenoid valve connected to compressed air （air cool feature）. Air cool activates when the furnace is below 600C.Example:Air Cool: OnData storageThe Data storage

11、segment controls data collection during the experiment. If a Data Storage segment is not used, data storage will be automatically initiated by the first Ramp, Isothermal, or Step segment that appears in the method. Data Storage:EquilibrateBack to topThe Equilibrate segment heats or cools the furnace

12、 to the defined temperature, stabilizes the furnace at that temperature, then continues to the next segment. This segment does not automatically start data collection. Equilibrate at 200External EventThe Event segment controls the external event relay through the event jack on the back of the instru

13、ment. This is used to synchronize control of additional hardware through the method. External Event:Fill CoolerAvailable for DMA and DSC Only:This segment is used to control the filling of the Gas Cooling Accessory （GCA） or Liquid Nitrogen Cooling System （LNCS） when it falls below an entered percent

14、age during an experiment.Fill Cooler if below 50% Flow RateAvailable for MFC Only:The Flow Rate segment is used to alter the rate of flow of the selected gas when an instrument is equipped with a Mass Flow Controller.Flow rate 50 mL/minForceAvailable for DMA Only:The Force segment applies a constant

15、 static force to the sample, then executes the next segment. This segment is only valid for experiments done in the Controlled Force and Strain Rate modes.The Force segment in the Strain Rate mode shuts off displacement （strain） control when this segment is executed. Executing a subsequent Set Strai

16、n or Ramp Strain segment shuts off force control and resumes displacement （strain） control.Force 0.5 NFrequency SweepThe Frequency Sweep segment is used in multiple frequency experiments to collect data at each frequency in the selected frequency table at a constant temperature. This segment is only

17、 valid for DMA Multifrequency mode.This segment turns on data storage when it begins, and turns it off when it ends.Gas SelectionAvailable with the MFC Only:The Gas segment controls the switching of gas, between Gas 1 and Gas 2 for an instrument with a Mass Flow Controller （MFC） installed. This segm

18、ent is used to synchronize gas switching at a specific time or temperature in an experiment. Select Gas1Heater PIDThe Heater PID segment is used to change the performance of the instrument furnace during the execution of a thermal method. PID stands for Proportional, Integral, and Derivative, the th

19、ree modes of traditional temperature control. The Heater PID segment specifies the control coefficients for each mode of temperature control.For more detailed information, click here more. P= 35 I= 70 D=2High Resolution rampAvailable for TGA High Resolution instruments only. The High Resolution ramp

20、 segment varies the heating/cooling rate of the furnace in response to changes in the rate of decomposition of the sample to improve weight change resolution. Ramp 50.00C/min res 4.0 to 800.00High Resolution sensitivityAvailable for TGA High Resolution instruments only. The High Resolution sensitivi

21、ty segment sets an additional parameter associated with the High Resolution ramp segments, which can be used to adjust the response of the High Resolution temperature control algorithm. This is sometimes necessary due to the wide variation in decomposition mechanisms of typical sample materials. The

22、 sensitivity setting is a unitless number ranging from 1.0 （lowest sensitivity） to 8.0 （highest sensitivity）. Increasing sensitivity tends to increase experiment time. High resolution sensitivity 2.0Increment ForceThe Increment Force segment raises or lowers the static force in a step, then executes

23、 the next segment. This segment is only valid for experiments done in controlled force mode.1. Equilibrate to 502. Isothermal for 5 min.3. Increment force 0.05 N4. Repeat segment 2 for 3 times Increment TemperatureThe Increment Temperature segment raises or lowers the temperature in a controlled ste

24、p, lets the temperature equilibrate, then begins the next segment. Increment by 5Initial temperatureThe Initial Temperature segment heats or cools the furnace to the defined temperature, stabilizes the furnace at that temperature, then holds the temperature until the experiment is continued by selec

25、ting Resume on the Tool Bar or menu, or pressing START on the instrument keypad. The instrument status will display ready when the temperature is stabilized. This segment does not automatically start data collection. Initial Temp 200IsostrainThe Isostrain segment applies an instantaneous strain to t

26、he sample and the force required to maintain the strain at a constant value is monitored.1. Equilibrate 302. Isostrain at 1%3. Ramp 3IsothermalThe Isothermal segment holds the sample at the current temperature （as programmed by the previous segment） for a defined period of time. This segment automat

27、ically turns on data collection, except when preceded by a Data Storage OFF segment. Isothermal for 10 minJumpThe Jump segment instantly changes the set point temperature, causing ballistic changes in the sample temperature. This segment then allows the immediate execution of the next segment （which

28、 is usually the Isothermal segment）. Note that large temperature overshoots may result from the use of this segment. This segment does not automatically start data collection. Jump to 200Mark end of cycleThe Mark end of cycle segment places a marker in the data for use by the data analysis programs.

29、 In general markers provide quick parsing of data to separate experimental segments （i.e., the heat-cool cycle）. A cycle mark number of 0 will automatically increment the mark number each time it is used, providing a running cycle count. Mark end of cycle 0Modulate temperatureAvailable for Modulated Instruments Only: This segment allows you to ent