Pyris1TGA操作规范.docx

1、Pyris1TGA操作规范1.0 目的 PURPOSE 1.1 本规范描述了PE Pyris 1热失重分析仪的操作，校正和维护方法。This document contains instructions used to provide a uniform method of operating, calibrating, and maintaining the Perkin Elmer Pyris 1 Thermogravimetric Analyzer. 2.0 范围 SCOPE2.1 本规范包括Perkin Elmer Pyris 1 TGA的校验，操作，维护程序。This documen

2、t covers the calibration, operation, and maintenance procedures for the Perkin Elmer Pyris 1 TGA.3.0 职责 RESPONSIBILITIES3.1 所有的实验室分析人员必须遵守本规范。This instruction should be observed by all testing personnel.3.2 分析人员使用前应先检查设备的校验日期，如果过期，则应向实验室主管或QC校验人员汇报。Visually check to make sure the calibration date on

3、 the instrument is not expired. If the instrument is expired, report it to a supervisor or the quality control calibration staff. 3.3 当仪器出现异常时应向实验室主管或QC校验人员汇报。Malfunctioning instruments should be reported to both a supervisor and a QC calibration staff.4.0 安全防护 SAFETY PRECAUTION4.1 按管理要求穿戴合适的个人防护用品。

4、It is necessary to wear all Personal Protective Equipment assigned by your Supervisor.4.2 预防措施Instrumental Precaution注意：操作者在使用Pyris 1时必须遵守下面的预防措施：NOTE: The following precautions must be observed when using the Pyris 1 Thermogravimetric Analyzer.4.2.1 当Pyris软件出现异常时不要按下计算机的Reset键。如果要关闭异常的Pyris窗口时应同时按下

5、Ctrl+Alt+Del键，然后从任务管理其中关闭Pyris软件。Never press the Reset button on the computer if the Pyris software appears to malfunction. Press the Ctrl-Alt-Del keys simultaneously and select the Task Manager. From the Task Manager, close the Pyris software.4.2.2 在关闭PE Pyris 1设备和切断电源前，不要拆掉仪器上的任何面板。Never remove th

6、e outer instrument cover or side panels on the PE Pyris 1 without shutting the instrument down and disconnecting its power cord from the power source.4.2.3 PE Pyris 1所使用的气体纯度不应低于99.9%。Only high-quality purge gases should be used with the PE Pyris 1. Minimum purity of 99.9% is recommended. 4.2.4 遵守PE

7、 Pyris 1和相关设备的开启和关闭程序。Always observe the proper startup or shutdown procedures with the PE Pyris 1 and all related instruments.4.2.5 通过天平室的气流流速始终控制在40-60cc/min, 建议使用惰性气体来作为天平室的冲洗气，如：氮气、氩气。Always maintain a positive purge flow (40 60 cc/min) through the balance chamber at all times. An inert gas such

8、 as nitrogen or argon is recommended as a balance purge.4.2.6 当加热炉的外套管移掉时禁止将加热炉抬升，否则将严重损坏PE Pyris 1的加热炉和其他部件。Do not raise the furnace when the clear Pyrex furnace tube has been removed. This will cause severe damage to the furnace and other components of the PE Pyris 1 analyzer.4.2.7 当PE Pyris 1的加热炉

9、在升温时，将其前面的塑料保护面板放下，以避免意外接触高温的加热炉。When the PE Pyris 1 standard or high temperature furnace is heating, keep the protective plastic shield on the PE Pyris 1 in the down position. This will protect you from accidentally touching the furnace when it is hot.4.2.8 在切断电源和冷却风扇停止旋转前，不要移动PE Pyris 1。Do not att

10、empt to move the PE Pyris 1 while it is on. Wait until the power is off and the furnace cooling fan has stopped spinning before moving the instrument.4.2.9 在分析仪工作时禁止将其连接至PE Pyris 1的导线拔掉。Do not remove cables from the PE Pyris 1 when the analyzer is turned on.4.2.10 禁止触摸PE Pyris 1的加热炉开口，禁止向里面投入物体。Do n

11、ot touch the opening on the furnace lift mechanism or insert objects into the opening.5.0 定义 DEFINITIONS5.1 TGA：热失重分析仪TGA : ThermoGravimetric Analyzer6.0 工作程序 INSTRUCTIONS注意：在使用PE Pyris 1进行实验或者校正前，应先对热电偶进行检查。将温度设定至100C后升温，如果热电偶校验正常，则显示的温度应非常接近100C。NOTE: Prior to performing any experiment or calibrat

12、ion procedure, be sure that the thermocouple currently installed on the PE Pyris 1 is functioning properly. The thermocouple can be checked by programming the PE Pyris 1 to 100C and checking the temperature displayed in the status panel. The temperature should be close to 100C if the instrument is c

13、alibrated.6.1 设备的启动和测量Start up and measurement注意：在开机前确保动力气，天平气，参比气都已打开并调节到要求的流速。 NOTE: Make sure the Pneumatic gas, Balance gas and Reference gas are all open and adjusted to the requirement before the Analyzer turn on. 6.1.1 按下面的顺序打开系统：Turn the system on following order:计算机Computer 分析仪Analyzer6.1.2

14、 运行Pyris软件，然后按下相关设备的按钮。Execute the Pyris manager, then click on each instrument button.6.1.3 等待每个设备的绿灯都亮起。Wait until the green light comes to each instrument button (instrument window opens automatically).6.1.4 将加热炉升起，待重量读数稳定后，按下“Zero”键去除样品盘的皮重。Raise the furnace, after the sample weight reading is s

15、tabilized, then tare the sample pan by pressing the Zero weight button.6.1.5 降下加热炉，在支架的保护下取下样品盘，放入样品，再将样品盘放回原处。Lower the furnace; remove and fill the sample pan with the specimen while supporting the sample pan with platform.注意：当取下或放回样品盘时，必须使用支架对样品盘进行保护。由于Pyris 1的天平非常敏感易损，禁止再没有支架的保护下取下或放回样品盘。NOTE: A

16、lways use the platform to work on sample pan. The weight balance is extremely sensitive, so do not change sample pan without platform support.6.1.6 从“File”中打开适当的操作程序（每个程序可以根据特殊的要求进行修改）。Open the appropriate method from the File menu (each method can be modified according to specific condition require

17、ment).6.1.7 打开“Sample Info”栏，填写Sample ID, Operator ID, Comment, File Name，同时检查初始状态栏并输入正确的系统参数。Select the Sample Info tab and fill in the Sample ID, Operator ID, Comment, and File Name. Also check initial state tab and program tab for proper parameter set up.6.1.8 装入样品盘，升起加热炉。Load the sample pan, the

18、n raise the furnace.6.1.9 输入初始温度，然后点击“Go to temperature”键。当温度升至设定的初始温度后，点击“Sample weight”键称量样品重量，再点击“Start/stop”键，系统进入自动运行状态。Enter the initial temperature and press the Go to temperature button. When the temperature reaches to initial temperature, measure the sample weight by pressing the Sample wei

19、ght button, and run the analysis by clicking the Start/stop button once.6.1.10等待系统完成全部的测试。Wait until the system finishes scanning.6.1.11激活运行窗口。Make the last run an active window. 失重百分比：Percent Weight Loss:计算样品的失重百分比时，将图中的x轴设为温度（或者可以从“Display”菜单中选”Rescale X”，再设定温度值来改变x轴的单位）y轴设为重量百分比（从“Curves”中选择“Weig

20、ht”，有时需要使用Rescale Tools中的Swap Y Axes功能将重量显示在左侧的x轴上）。To calculate the percent weight loss of the specimen, be sure that the curve is displayed with the x axis as Temperature (change by selecting Rescale X from the Display menu and selecting Temperature for the Set Axis Units value) and the y axis as

21、Weight percent (change by selecting Weight from the Curves menu; it maybe required to use Swap Y Axes from the Rescale Tools bar to place Weight on the left-hand axis).从“Calc”菜单中选择“delta Y”，输入工作单上所要求的温度，点击“Calculate”，将结果记录在工作单上。Select delta Y from Calc menu, then enter the temperature parameter spec

22、ified on a traveler. Press Calculate and report Delta Y value on a traveler.固含量分析：Filler Content Analysis:当计算样品的固含量时，将图中的x轴设为时间（或者可以从“Display”菜单中选”Rescale X”，再设定时间值来改变x轴的单位），y轴设为重量百分比（从“Curves”中选择“Weight”，有时需要使用Rescale Tools中的Swap Y Axes功能将重量显示在左侧的x轴上）。To calculate the filler content of the specimen

23、, be sure that the curve is displayed with the x axis as Time (change by selecting Rescale X from the Display menu and selecting Time for the Set Axis Units value) and the y axis as Weight percent (change by selecting Weight from the Curves menu; it maybe required to use Swap Y Axes from the Rescale

24、 Tools bar to place Weight on the left-hand axis).从“Calc”菜单中选择“delta Y”，输入时间参数（时间应该包括右侧平直曲线部分对应的时间），点击“Calculate”，将结果（100%-计算值）记录在工作单上。Select delta Y from Calc menu, then enter the time parameter (the time parameter should include flat region of the right hand side graph). Press Calculate and report

25、 100% - Delta Y value on a traveler.6.1.12 将分析结果打印出来附在工作单后面。Print the analysis report and attach it to the traveler.6.2 维护要求 Maintenance Requirements为了延长PE Pyris 1的加热炉的使用寿命，应定期对加热炉进行清洗，例如每5-10次测试后运行一次自动清洗程序，用棉棒和溶剂彻底清洗加热炉的内部，待其彻底干燥后再继续使用。To prolong the life of the PE Pyris 1 standard and high tempera

26、ture furnaces, it is recommended that the automatic furnace cleaning procedure be performed routinely, such as every 5 10 runs. Thoroughly clean the inner surface of the furnace using Q-tips and proper solvent, and let it completely dry before use.6.3 校验要求 Calibration Requirements 注意：PE Pyris 1的校验包含

27、三项内容，为了确保测量的精确性，必须定期对设备进行校验。NOTE: There are three calibration routines for the PE Pyris 1. Periodic calibration checks will be necessary to verify accurate calibration.6.3.1 如果在一段时期内PE Pyris 1的操作环境没有改变，则其校验数据在此期间内有效。即使当系统关闭后，前面的校验数据仍储存在电脑里，再次开机后校验依然有效。某些条件会改变PE Pyris 1的温度校验或者称量校验结果，此时需要按下面的要求进行重新校验：

28、The PE Pyris 1s calibration should remain unchanged for quite some time, provided that there are no changes in the instruments operating conditions. Even when the system is shut off, the calibration values are stored so that the next time the instrument is turned on, it will still be calibrated. Som

29、e of the conditions that could change either the temperature or weight calibration of the PE Pyris 1 and require recalibration are as follows:如果实验的温度范围改变，则需要重新校验。If the operating temperature range of your experiments changes, recalibration may be necessary. Check the temperature calibration in the r

30、ange of interest to determine if the current calibration is still valid.如果气体种类或者气体流速改变，则需要重新校验以保证结果的精确性。If the purge gas type or purge gas flow rate is changed, the calibration should be checked for highest accuracy.如果更换新的加热炉，应重新进行温度校验。If a new furnace is installed, the temperature calibration shoul

31、d be checked.如果更换新的热电偶或者热电偶的位置有所改变，则应再次进行温度校验。If a new thermocouple is installed or if the position of the thermocouple changes, you should perform the temperature calibration again.如果分析仪的位置（水平或者垂直）有所改变，则应进行称量校验。If the analyzer is moved or releveled, you should perform the weight calibration again.6

32、.3.2 PE Pyris 1的温度校验：The temperature calibration routines for the PE Pyris 1 are:打开Method Editor窗口，从File栏中选择Open Method，双击Method目录中的Alumel.tgm文件，系统会显示出nickel校验操作窗口。From the Method Editor, select Open Method from the File menu. Double click on the Alumel.tgm method file which is in the Method directory. The nickel calibration method is displayed on the screen.打开Sample Info栏，输入Sample ID, Operator ID, Comment, ， File Name信息。Selec