Pyris 1 TGA 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 SCOPE

2.1 本规范包括Perkin Elmer Pyris 1 TGA的校验，操作，维护程序。

This document covers the calibration, operation, and maintenance procedures for the Perkin Elmer Pyris 1 TGA.

3.0 职责 RESPONSIBILITIES

3.1 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 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 PRECAUTION

4.1 按管理要求穿戴合适的个人防护用品。

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 the 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%。

EOI-0142/R2, Version 1.0

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 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 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 attempt 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 not touch the opening on the furnace lift mechanism or insert objects into the

opening.

5.0 定义 DEFINITIONS

5.1 TGA：热失重分析仪

TGA : ThermoGravimetric Analyzer

6.0 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100°C后升温，如果热电偶校验正常，则显示的温度应非常接近100°C。

NOTE: Prior to performing any experiment or calibration 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 100°C and

checking the temperature displayed in the status panel. The temperature should be close to 100°C if the instrument is calibrated.

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

Analyzer

6.1.2 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 stabilized, 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: Always 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 requirement).

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, then 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 weight 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“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 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 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 specified

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, 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 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 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 temperature 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：

The PE Pyris 1’s calibration should remain unchanged for quite some time,

provided that there are no changes in the instrument's 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. Some 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 range 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 should 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.

6.3.2 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。

Select the Sample Info tab and fill in the Sample ID, Operator ID, Comment, and File Name.

切一段长度1~2mm的细alumel条，放入样品盘中。

Cut a small piece of alumel approximately 1 – 2 mm long and place it in the sample pan.

点击操作窗口中的Raise Furnace，升起加热炉。

Click on the Raise Furnace button in the control panel.

点击操作窗口中的Zero Weight，分析仪会读取样品的毛重。

Click on the Zero Weight button in the control panel. The analyzer reads the weight of the sample.

当读数稳定后，点击OK，读数会显示在Sample Info页中的Enter Sample Weight 一栏中。

After the weight reading has stabilized, click on the OK button. The weight is entered into the Zero field of the Enter Sample Weight area on the Sample Info page.

将磁铁放在支架上移近加热炉。

Place the magnet onto the sample loading platform and move the platform next to the furnace tube.

调整支架的高度至读数显示在3~6mg之间，此读数是由样品的磁性产生的，当样品失去磁性时，读书会变小。

Adjust the height of the sample loading platform so that you get a weight reading between 3 and 6 mg. The apparent weight reading is a result of the magnetism of the sample. As the sample loses magnetism, the apparent weight reading decreases.

当读数稳定后，点击控制窗中的Sample Weight，读数会显示在Sample Info页中的Enter Sample Weight一栏中。

After the weight reading has stabilized, click on the Sample Weight button on the control panel. The weight is entered into the Weight field of the Enter Sample Weight area of the Sample Info page.

点击控制窗中的Start Method，开始测试。

Click on the Start Method button on the control panel.

实验结束后，从“alumel”中打开实验结果文件，将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“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）。

In Data Analysis, open the data file from alumel run. 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 Weight (change by selecting Weight from the Curves menu; you may have to use Swap Y Axes from the Rescale Tools bar to place Weight on the left-hand

axis).

从“Math”菜单中选择“Derivative”，图中会显示出导数曲线，通过设定转折点来精确设定onset计算的左限。

Select Derivative from the Math menu. The first derivative of the curve is displayed.

Use the inflection point to accurately determine what the left limit should be for the onset calculation.

点击初始曲线。

Click on the sample curve to make it the focused or active curve.

从“Calc”菜单中选择“Onset”。

Select Onset from the Calc menu.

移动位于曲线上的两个红X标记，将左侧的标记移至一阶导数的转折点，将右侧的标记移至曲线过转折点平坦部分。

Move the two red X marks on the curve. Position the left limit marker at the

inflection point of the first derivative curve and place the right limit marker past the inflection point on a level portion of the curve.

点击Onset对话框中的Calculate键，屏幕会弹出Adjust Tangents对话框。

Click on the Calculate button in the Onset dialog box. The Adjust Tangents dialog

box is seen.

调节各点的切线直到它们相交。

Adjust the tangents of each point until they cross.

点击Adjust Tangents对话框中的Calculate键，系统会计算出样品的onset温度值（Onset X）并显示在屏幕上。

Click on the Calculate button in the Adjust Tangents dialog box. The onset

temperature is calculated for the sample and displayed on the screen (Onset X).

在Method Editor栏中，从View菜单中选择Calibrate。

In the Method Editor, select Calibrate from the View menu.

点击Calibration窗口中的Temperature栏，输入所测得的alumel的Onset值，点

击Use栏中的Check。

Click on the Temperature tab in the Calibration window. Enter the Measured Onset values for alumel and click in the check box in the Use column for reference

material.

点击Save and Apply键，将校验数据传至分析仪，保存校验文件。

Click on the Save and Apply button to send the calibration values to the analyzer

and save the current calibration file.

点击Close键退出校验窗口。

Select the Close button to exit the Calibration window.

6.3.3 PE Pyris 1的重量校验

The weight calibration routines for the PE Pyris 1 are

打开Pyris软件中的Instrument Viewer 或Method Editor，选择View菜单中的Calibrate。

While in the Instrument Viewer or the Method Editor in the Pyris software, select Calibrate from the View menu.

选择Calibration窗口中的Weight栏。

Select the Weight tab in the Calibration window.

在Reference Weight编辑栏内输入参照物的重量(100mg)。

Enter the weight of your reference material (100 mg) in the Reference Weight edit box.

注意：应使用NIST砝码，操作时需要戴上手套并且使用镊子。

NOTE: NIST traceable weights should be used. When handling the weights, always wear gloves and use forceps to hold.

点击Begin Calibration。

Select the Begin Calibration button.

如果垂线上有样品盘，则将盘中的样品清除；如果垂线下无样品盘，则在托盘上放置一空盘，随后装至垂线上。将托盘从样品盘下方移走，点击对话框内的OK。

If there is a sample pan already on the hang down wire, remove any sample from the pan. If there is no sample pan already in place, then place an empty sample pan on the sample loading tray and load the pan onto the hang down wire. Move the sample loading tray away from the sample pan. Click on OK in the dialog box. 当Read Zero栏中的0读数稳定后，点击对话框中的OK。

When the zero weight reading is stable in the Read Zero field, click on OK in the dialog box.

将校验参照物放进样品盘中，点击OK。

Place the reference weight in the sample pan. Move the sample loading tray away from the sample pan. Click on OK.

当Read Value栏中的读数稳定后，点击OK，校验完成。

When the weight reading is stable in the Read Value field, click on OK. The calibration is complete.

点击Calibration窗口中的Save and Apply，保存校验数据。

Select the Save and Apply button in the Calibration window to send the new calibration values to the analyzer and save the calibration file.

进入下一个校验程序，或者点击Close关闭校验窗口并对参照物进行2次以上复测，检验校验结果正确与否。

Go to the next calibration procedure or select Close to close the Calibration window and begin using the new calibration values to check at least two more reference weights.

如果复测的结果正确(误差± 2%)，则校验数据可以使用，反之，则应重新进行称量校验。

If the reading is correct (± 2%), begin using the calibration value. If not, repeat the weight calibration steps.

6.3.4 加热炉的日常校验：

The furnace calibration routines for the PE Pyris 1 are:

注意：在对加热炉进行校验前，应检查热电偶是否正常，样品盘内是否留有样品。

检查热电偶的方法是：升起加热炉，将程序设定到100°C(在Go To Temp栏中输入100，然后点击Go To Temp)，然后检查Status Panel中测得的温度值是否处于或

低于校验范围的下限。完成检查工作最简单的方法是点击控制面板中的“Go To

Load”键，当提示选择校验的最低和最高温度时，选择一个包含操作范围的温度

值。当进行加热炉校验时，加热炉必须处于升起位置，手动抬升和夹紧是不够的，

必须选择控制面板中的“Raise Furnace”键。

NOTE: Before performing the furnace calibration of the PE Pyris 1, make sure that the thermocouple is functioning properly and that the sample pan is empty. To

verify thermocouple operation, raise the PE Pyris 1 furnace and program the

temperature to 100°C. Enter 100 in the Go To Temp entry field of the Control

Panel and click on the Go To Temp button. Check that the current sample

temperature displayed in the Status Panel is at or below the intended minimum

calibration temperature. The easiest way to accomplish this is to click on the Go To Load button on the Control Panel. When selecting minimum and maximum

temperatures for the furnace calibration, select the limits so that they encompass

the temperature range in which you plan to operate. The furnace must be in the

raised position to perform a furnace calibration. Lifting and clamping by hand is not sufficient. You must select the Raise Furnace button on the Control Panel.

注意：加热炉的校验必须在温度校验完成后进行。

NOTE: Furnace calibration must be performed after Temperature calibration.

在Instrument Viewer 或Method Editor中，从View栏中选择Calibrate。

While in the Instrument Viewer or the Method Editor, select Calibrate from the View menu.

如果温度校验的数据有效，则跳过温度校验。

If applicable, complete the Temperature calibration.

将样品盘清空。

Remove any sample from the sample pan in the stirrup.

在Calibration窗口中打开Furnace栏。

Select the Furnace tab in the Calibration window.

在Minimum栏内输入一个最小温度作为校验的起始温度，其数值应低于日常测量范围的下限。

In the Minimum field, enter a minimum temperature where the calibration will begin.

This should be below your normal operating region.

在Maximum栏内输入一个最大温度作为校验的结束温度，其数值应高于日常测量范围的上限。

In the Maximum field, enter a maximum temperature where the calibration will end.

This should be above your normal operating region.

注意：最大温度值减去最小温度值的差值应高于100°C，否则加热炉校验将无法进行。

NOTE: Maximum temperature minus minimum temperature must be greater than

100°C or the furnace calibration will not be performed.

点击Begin Calibration键。

Select the Begin Calibration button.

校验开始后，系统会显示出加热炉校验所需的估计剩余时间。

The approximate time remaining in the furnace calibration is displayed.

校验结束后，在Calibration窗口中选择Select the Save and Apply，保存校验数

据。

Select the Save and Apply button in the Calibration window to send the new

calibration values to the analyzer and save the calibration file.

点击Close，关闭校验窗口，完成校验。

Select the Close button to close the Calibration window and begin using the new

calibration values.

6.3.5 TGA专用100毫克标准砝码的校验

Calibration of specific 100mg Standard Weight for TGA

仪器生产商提供的TGA专用100毫克标准砝码必须每六个月校验一次。

The specific 100 mg Standard Weight for TGA provided by Perkin Elmer shall be

calibrated every six months.

用一校验过的天平称标准砝码六次，每次重量差异不应超过0.1mg。将结果记录在EOI-0142/R2。

Weight the specific 100 g Standard Weight on a calibrated balance six times, the

difference shall not be more than 0.1mg each time. Record the results in EOI-

0142/R2.

6.3.6 校验参照物

Calibration Reference Materials

TGA所需的校验参照物要符合ISO9000的规范要求。ISO规范中的校验参照物有两个等级：参考级和鉴定级。参考级参照物符合仪器校验的ISO规范，它可以直接从Perkin Elmer公司获得。Perkin Elmer通过每批产品的批号来提供所需的ISO文档编号，这个批号应填入原材料的ISO控制文件中。ISO指引30中将RM(参考级参

照物)定义为：材料或物质的一个或多个性质与被测物充分的相似，可以很好的用于仪器的校验、测试方法的评估或者物质的定量分析。

Perkin Elmer Thermal Analysis calibration materials are ISO 9000 compatible.

They are called Reference Materials. ISO has two classifications for calibration

materials: Reference Materials and Certified Reference Materials. Reference

Materials (RMs) comply with ISO for instrumentation calibration. They are available from Perkin Elmer and Perkin Elmer provides documentation with each RM that

cross references the material’s lot code. This declaration should be filed with all

other material certificates and documents in your ISO file. ISO Guide 30 defines a RM as a “Material or substance one or more of whose property values are

sufficiently homogeneous and well established to be used for the calibration of an apparatus, the assessment of a measurement method, or for assigning values to

materials.”

鉴定级参照物(CRMs)可以通过连续的对比追溯至国家或国际标准，并不是所有的校验物都是鉴定级参照物。鉴定级参照物非常昂贵并且不是适用于所有的热分析技

术，如果不能确定应使用何种参照物，应将参考级参照物与鉴定级参照物进行对

比，与QA部门协商决定。如果最终决定使用鉴定级参照物，可以向全国标准技术

研究所订购。

Certified Reference Materials (CRMs) are traceable to national or international

standards through an unbroken chain of comparisons. Not every calibration

material is a CRM. CRMs can be very expensive and are not available for all

thermal analysis techniques. If you are not sure what material to use, then check

with Quality Assurance Department and discuss the differences between RMs and CRMs. If you find that you need CRMs, you may order them from the National

Institute of Standards and Technology (301 975-6776).

磁力校验参照物是用于对加热炉进行Curie温度校验，它可以从PEXPRESS处整套购得。建议每次进行校验时使用新的参照物，这样可以避免磁滞和氧化对校验结果

产生影响。每个参照物的附属文件中指出了其磁力标准的转移温度。

Magnetic Calibration Reference Materials are used to perform the Curie point

temperature calibration on the standard furnace. They are available from PE

XPRESS in kit form and separately. It is recommend that to use fresh reference

materials each time to calibrate instrument. This way one can avoid the effects of

hysteresis and oxidation on the Curie point of the reference materials. The

transition temperature for each of the magnetic standards is indicated in the

documentation included with the reference material.

7.0 参考文件 REFERENCE

8.0 记录 RECORD

9.0 附录 APPENDIX