Download - Manual DSC Kinetic Analysis

346-69840B

Thermal Analysis System TA-60WS

DSC Kinetic Analysis Program (Ozawa method)

Instruction Manual (Instruction, Operation)

READ AND UNDERSTAND THIS MANUAL BEFORE OPERATION. SAVE THIS MANUAL.

Copyright© Shimadzu Corporation 2002-2008. All rights reserved, including those to reproduce this publication or parts thereof in any from without permission in writing from Shimadzu Corporation. Information in this publication is subject to change without notice and does not represent a commitment on the part of the vendor. Any errors or omissions which may have occurred in this publication despite the utmost care taken in its production will be corrected as soon as possible, but not necessarily immediately upon detection. Shimadzu Corporation will continue to supply original Shimadzu maintenance parts associated with a given product for a period up to 7 years from the cessation of production of that product. Please be informed that after this period of time, Shimadzu Corporation cannot guarantee supply of such original maintenance parts. However, following discontinuation of a product, the period of availability of maintenance parts which have been produced on a subcontract basis is up to the discretion of the concerned sub-contracting company. Microsoft, Microsoft Excel, Microsoft Word, Windows are registered trademarks or trademarks of Microsoft Corporation in the United States. Pentium is registered trademarks of Intel Corporation in the United States.

Precautions for Safety Operation

Thank you for adopting the DSC Kinetic Analysis program for SHIMADZU Thermal Analysis Workstation TA-60WS. This program will determine reaction rate parameters using data generated for kinetic analysis using the DSC-60 or DSC-50 Differential Scanning Calorimeter. This Instruction Manual describes the functions and use of this program. Functions and operations common to the TA-60WS, such as the data collection, etc. , are not included. For these operations, refer to the instruction manual for the TA-60WS program. In order to make full use of the instrument with sufficient knowledge for safety operation, please observe strictly the following points. 1. Do not use the unit for the purpose other than the above-mentioned analysis. 2. Follow the procedures described in this instruction manual. 3. Observe all warnings and cautions. 4. Do not disassemble or modify the unit without our approval. 5. For repair of the product inside, contact our sales office or agent.

MEANING OF CAUTION SIGNS WARNING indicates a potentially hazardous situation which, if not avoided, could result in death, serious injury or moderate injury. CAUTION indicates a potentially hazardous situation which, if not avoided, may result in minor injury, or may result in machine damage. NOTE is used to emphasize essential information.

How to use this manual

This manual consists of 8 chapters. First, verify that all of the parts mentioned in Chapter 2 Parts List are included in your shipment, and then install the program according to Chapter 3 Installation. After completing the installation, read Chapter 1 Summary. This chapter gives a basic summary of the DSC Kinetic Analysis program and the files generated by this software. To generate data files for Kinetic Analysis, conduct the measurements according to Chapter 6 DSC Kinetic Analysis Measurement Summary. Next, review Chapter 4 DSC Kinetic Analysis Program operation procedures. This chapter outlines the general Kinetic Analysis procedures from analysis to report output. For operational and function descriptions of the menu commands used in this software, refer to Chapter 5 DSC Kinetic Analysis Program Functions. Certain functions featured in the analysis configuration of the DSC Kinetic Analysis program may be modified, such as the number of decimal places displayed in the analysis result. For details, refer to Chapter 8 DSC Kinetic Analysis Configuration.

Contents

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1 Summary.......................................................................................... 1 1.1 The DSC Kinetic Analysis Program ....................................................................... 1

1.2 Data to be used for DSC Kinetic Analysis.............................................................. 1

1.3 The DSC Kinetic Analysis Result File ................................................................... 2

2 Parts List ......................................................................................... 3 2.1 DSC Kinetic Analysis Program Parts Summary ................................................... 3

3 Installation....................................................................................... 4 3.1 Before installation................................................................................................... 4

3.2 Installation .............................................................................................................. 5 3.2.1 TA-60WS Software Setup ................................................................................................ 5 3.2.2 Registration of DSC Kinetic Analysis Program ............................................................. 6 3.2.3 DSC Kinetic Analysis Program Setup ............................................................................ 7

4 DSC Kinetic Analysis Program operation procedures.................... 8 4.1 Flow of DSC Kinetic Analysis Program (Ozawa method)...................................... 8

4.1.1 Open of TA-60WS format (Extension: .tad) data ........................................................... 9

4.2 Operation procedures............................................................................................ 11 4.2.1 Starting of <<DSC Kinetic Analysis Program (Ozawa method) window>>................11 4.2.2 Selecting data for DSC Kinetic Analysis .......................................................................11 4.2.3 Setting the display range ...............................................................................................11 4.2.4 Changing the display position....................................................................................... 12 4.2.5 DSC Kinetic Analysis..................................................................................................... 13 4.2.6 Isothermal Analysis ....................................................................................................... 13 4.2.7 Report output ................................................................................................................. 13 4.2.8 Storing results of Kinetic Analysis ............................................................................... 14 4.2.9 Closing the <<DSC Kinetic Analysis Program (Ozawa method) window>>.............. 14

4.3 DSC Kinetic Analysis operation procedures ........................................................ 15 4.3.1 Kinetic Analysis ............................................................................................................. 15 4.3.2 Kinetic Analysis - By data ............................................................................................. 17 4.3.3 Kinetic Analysis - Select peak ....................................................................................... 19 4.3.4 Kinetic Analysis Options ............................................................................................... 21

4.4 Isothermal Analysis operation procedures........................................................... 22 4.4.1 Isothermal Analysis ....................................................................................................... 22 4.4.2 Isothermal Analysis options .......................................................................................... 24

4.5 DSC Kinetic Analysis Configuration .................................................................... 25 4.5.1 Options............................................................................................................................ 25

5 DSC Kinetic Analysis Program Functions.................................... 26 5.1 <<DSC Kinetic Analysis Program (Ozawa method) window>> menu items ...... 26

5.1.1 [File] menu ..................................................................................................................... 26 5.1.2 [Display] menu ............................................................................................................... 30 5.1.3 [Scale] menu ................................................................................................................... 32 5.1.4 [Analysis] menu.............................................................................................................. 33 5.1.5 [Display Position] menu ................................................................................................ 37 5.1.6 [Report] menu................................................................................................................. 40

Contents

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5.1.7 [Window] menu............................................................................................................... 43

5.2 <Ozawa Plot window> menu items ...................................................................... 44 5.2.1 [Display] menu ............................................................................................................... 44 5.2.2 [Report] menu................................................................................................................. 44

5.3 <Isothermal Analysis window> menu items ........................................................ 45 5.3.1 [Display] menu ............................................................................................................... 45 5.3.2 [Scale] menu ................................................................................................................... 46 5.3.3 [Report] menu................................................................................................................. 47

5.4 <Report window> menu items .............................................................................. 48 5.4.1 [File] menu...................................................................................................................... 48 5.4.2 [Font] menu .................................................................................................................... 51 5.4.3 [Item] menu .................................................................................................................... 52 5.4.4 [Option] menu................................................................................................................. 57 5.4.5 Operations on Print preview ......................................................................................... 58

5.5 ASCII Conversion Program .................................................................................. 59 5.5.1 Starting the <<ASCII Conversion Window>>.............................................................. 59 5.5.2 <<ASCII Conversion Window>> Configuration ........................................................... 59 5.5.3 <<ASCII Conversion Window>> Operation ................................................................. 60 5.5.4 <<ASCII Conversion window>> menu.......................................................................... 61 5.5.5 <Data Window> Operation ............................................................................................ 64

6 DSC Kinetic Analysis Measurement Summary............................ 65 6.1 Cautions in Measurement..................................................................................... 65

7 DSC Kinetic Analysis Summary.................................................... 66 7.1 DSC Kinetic Analysis ............................................................................................ 66

7.2 Isothermal Analysis .............................................................................................. 68

8 DSC Kinetic Analysis Configuration............................................. 69 8.1 Analysis configuration file .................................................................................... 69

8.2 Items which can changed from analysis configuration file ................................. 69

8.3 Analysis configuration file path............................................................................ 69

8.4 Composition of the analysis configuration file..................................................... 70

8.5 Analysis configuration file contents summary..................................................... 72

DSC Kinetic Analysis Program (Ozawa method) for TA-60WS

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1 Summary

1.1 The DSC Kinetic Analysis Program This program will determine reaction rate parameters based on the Ozawa Method using data generated for kinetic analysis with the Differential Scanning Calorimeter (DSC-60 or DSC-50). Isothermal analysis can also be performed. The analysis results can then be saved in an analysis result file or output in a report. For the various functions and operational procedures refer to the appropriate sections of this documentation. The analysis units used in the calculations conducted by this program are as follows. [Kinetic Analysis]

• Kinetic Energy [KJ/mol],[Kcal/mol] • Reaction order • Frequency factor [min-1] • Analysis temperature [K],[ºC]

[Isothermal Analysis] • Kinetic Energy [KJ/mol],[Kcal/mol] • Reaction order • Frequency factor [min-1] • Analysis temperature [K],[ºC] • Rate constant [min-1] • Reaction time [hour] • Reduced time [hour]

1.2 Data to be used for DSC Kinetic Analysis The DSC Kinetic Analysis Program is based on the Ozawa Method, so the data used by this program must conform to the following conditions. 1) The data files for Kinetic Analysis processing are to have been measured using the DSC-60 or

DSC-50 Differential Scanning Calorimeter having file extensions: . tad . Up to 12 analysis files may be selected for processing. In addition, all of the data to be analyzed is to have been acquired using the same measurement parameters, except for different heating rates. The sample weight must also be entered.

2) After conducting a DSC Kinetic Analysis, the analysis results and plot information is stored in a

Kinetic Analysis result file (file extension: .KD0). 3) Old data file when Shimadzu Thermal Analyzer System TA-50WSI is used. (with file

extensions: .D?0, .R??) 4) Old data file when Shimadzu Thermal Analyzer System TA-50I is used. (files in which file name

begins with @, and having the file extension .000)


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1.3 The DSC Kinetic Analysis Result File The Kinetic Analysis result files generated by this program have the file extension .KD0. This analysis result file includes the Ozawa Plot and the results of isothermal analysis. The stored Kinetic Analysis result file can be loaded in the <<DSC Kinetic Analysis window>> and re-analyzed. In addition, this file can be converted to ASCII format in the <<ASCII Convert window>> for further data processing in Microsoft® Excel®, Lotus1-2-3® or other third-party software. Also note that Kinetic Analysis result files cannot be opened in programs other than the DSC Kinetic Analysis program.


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2 Parts List

2.1 DSC Kinetic Analysis Program Parts Summary The DSC Kinetic Analysis Program consists of the items listed below. Before installing the software, verify that all of the disks are included in your shipment. 1．DSC Kinetic Analysis Program (Ozawa method) P/N 347-65168-92 Item No. Part No. Description Qty

1 222-11539-91 DSC Kinetic Analysis program for TA-60WS (CD-ROM) 1 2 346-67586-91 TA-60WS Program (CD-ROM ) 1 3 346-69840 DSC Kinetic Analysis program for TA-60WS Instruction

Manual (this document) 1


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3 Installation

3.1 Before installation Prior to running the installation program, it is necessary that Microsoft® Windows® are installed on your PC. Note, however, that Microsoft® Windows® are not included with this software. In addition, before installing this program, install the TA-60WS program included with this software. If this program is not installed, the DSC Kinetic Analysis program may not run properly. PC OS Windows® XP Professional

Windows Vista™ Business Display SVGA(800*600 pixel) or higher Mouse/Keyboard CD-ROM Drive Use for install Printer A thing corresponding to the above OS.

CAUTION

If you have a later version of the TA-60WS program, there is no need to install the version provided with this software.


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3.2 Installation

3.2.1 TA-60WS Software Setup When you insert CD-ROM in the PC supporting "autorun" function, the setup program will automatically start.

CAUTION

When the version number written on your CD-ROM containing a TA-60WS program is higher than the one written on the CD-ROM containing the TA-60WS program accompanying this program, you do not need to install the latter. Proceed to the next paragraph.

The setup program starts. And, either of the following screen is displayed.

New installation screen

Maintenance screen

When you newly install it. Or, when the software Ver.1.50 or earlier is installed.

When the software Ver.1.51 or later is installed.

When the displayed screen is a new installation screen For the subsequent operation, follow the instructions in the window.

When the displayed screen is a maintenance screen Select the [Repair] item with the mouse. And select the [Next] button.


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3.2.2 Registration of DSC Kinetic Analysis Program The majority of the DSC Kinetic Analysis program is in CD-ROM of TA-60WS. However, it is necessary to register first of all for the installation by the following setup work. 1. When you insert CD-ROM in the PC supporting "autorun" function, the setup program will

automatically start.


Maintenance screen

When the displayed screen is a new installation screen 2. For the subsequent operation, follow the instructions in the window.

When the displayed screen is a maintenance screen 2. Select the [Repair] item with the mouse. And select the [Next] button. 3. Select the [Finish] button. Permission to install will be obtained by this.


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3.2.3 DSC Kinetic Analysis Program Setup When registration is completed, it is possible to set it up.

CAUTION

When the version number written on your CD-ROM containing a TA-60WS program is higher than the one written on the CD-ROM containing the TA-60WS program accompanying this program, you do not need to install the latter. Proceed to the next paragraph.

CAUTION

First of all, please end the setup program when the setup program of TA-60WS starts by auto run. 1. Select the Setup.exe file which exists in the following folder in CD-ROM in the Explorer etc.,

and it starts. ?: \KDSC\Disk1\Setup.exe ( ? is drive name)

2. The setup program starts. And, either of the following screen is displayed.


Maintenance screen

When you newly install it When it has already been installed

When the displayed screen is a new installation screen For the subsequent operation, follow the instructions in the window.

When the displayed screen is a maintenance screen Select the [Repair] item with the mouse. And select the [Next] button.


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4 DSC Kinetic Analysis Program operation procedures

4.1 Flow of DSC Kinetic Analysis Program (Ozawa method)

Operation Procedure Reference Section

Starting of <<DSC Kinetic Analysis Program (Ozawa method) window>> ↓

4.2.1

Configuration of <<DSC Kinetic Analysis Program (Ozawa method) window>>↓

4.5

Select data for DSC Kinetic Analysis ↓

4.2.2

Set display range ↓

4.2.3

Change display position ↓

4.2.4

DSC Kinetic Analysis ↓

4.3

Isothermal Analysis ↓

4.4

Report output ↓

5.1.6

Save Kinetic Analysis results

↓

5.1.1.2 5.1.1.3

Close <<DSC Kinetic Analysis Program (Ozawa method) window>> 4.2.9


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4.1.1 Open of TA-60WS format (Extension: .tad) data The following procedure is used to open the TA-60WS format data files (extension .tad) acquired on the Shimadzu Differential Scanning Calorimeter (DSC-60 and DSC-50).

CAUTION

The analysis result file (extension .KD0) is not available in this procedure. You can open this file from the [Open] item of the [File] menu of the <<DSC Kinetic Analysis Program (Ozawa method) window>>. For opening the <<DSC Kinetic Analysis Program (Ozawa method) window>> directly, the following methods are available. 1. Select the [Execution of program] item in the [DSC Kinetic Analysis] item in the [Analysis]

pull-down menu on the <<TA-60WS Acquisition: Status window>>. 2. Select the [Execution of program] item in the [DSC Kinetic Analysis] item in the [Application]

pull-down menu on the <<TA60 window>>. <Operation>

1. Select the [Select data file] item in the [DSC Kinetic Analysis] item in the [Analysis] pull-down menu on the <<TA-60WS Acquisition: Status window>>. Or select the [Select data file] item in the [DSC Kinetic Analysis] item in the [Application] pull-down menu on the <<TA60 window>>. The <Open File for Kinetic Analysis DSC window> is displayed.

2. Select the [Select File] button. The <Open window> is displayed. Select the data file name and select the [Open] button.

①

②

③

④

⑤

⑥ ⑦


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CAUTION

All data need to be acquired using the same measurement parameters except the heating rate, and have to include the sample weight.

NOTE

You can select the multiple files how to select the file while holding down the [Shift] key or [Ctrl] key in the <Open window>.

3. The selected file name is displayed in the <Open File for Kinetic Analysis DSC window>.

4. Push the [Analyze] button. The <<DSC Kinetic Analysis Program (Ozawa method) window>> is displayed with the all files on the [Files] list box.

5. Select the [Exit] button. The <Open File for Kinetic Analysis DSC window> is closed.

<Item>

① [Select File] button Display the <Open window> for selecting the data file.

② [Remove] button

Remove a selected file shown by the highlight from the [Files] list box.

③ [All Remove] button Remove all of the files in the [Files] list box.

④ [Help] button

Display help messages related to this window.

⑤ [Files] list box The selected file names are displayed.

⑥ [Analyze] button

Open the <<DSC Kinetic Analysis Program (Ozawa method) window>>, the all selected files in the [Files] list box are read.

⑦ [Exit] button

Close the <Open File for Kinetic Analysis DSC window>.


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4.2 Operation procedures

4.2.1 Starting of <<DSC Kinetic Analysis Program (Ozawa method) window>>

A DSC Kinetic Analysis Program (Ozawa method) is performed from the Explorer of Microsoft® Windows® etc. The <<DSC Kinetic Analysis Program (Ozawa method) window>> opens, and at the same time, a window is displayed for selecting a file to be loaded.

4.2.2 Selecting data for DSC Kinetic Analysis In the <Open File window>, select the data which is to be used for DSC Kinetic Analysis. 1) The data files for Kinetic Analysis processing are to have been measured using the DSC-60 or

DSC-50 Differential Scanning Calorimeter having file extensions: . tad . Up to 12 analysis files may be selected for processing. In addition, all of the data to be analyzed is to have been acquired using the same measurement parameters, except for different heating rates. The sample weight must also be entered.

2) After conducting a DSC Kinetic Analysis, the analysis results and plot information is stored in a

Kinetic Analysis result file (file extension: .KD0). 3) Old data file when Shimadzu Thermal Analyzer System TA-50WSI is used. (with file

extensions: .D?0, .R??) 4) Old data file when Shimadzu Thermal Analyzer System TA-50I is used. (files in which file name

begins with @, and having the file extension .000)

CAUTION

All of the data to be analyzed is to have been acquired using the same measurement parameters, except for different heating rates. The sample weight must also be entered.

4.2.3 Setting the display range The data display range may be set before performing an analysis. The following two methods are available for setting the display range.

1) Setting display range while data is overlaid Select [Range] from the [Display] menu. A dialog box having an [OK] button is displayed. Click on the screen, and then set the display range. Select the [OK] button.

NOTE

If a check mark is placed in the [Select Analysis Range] check box of the Options dialog box, selected [Options] from the [File] menu, this mode is established automatically. Refer to 5.1.2 2) Range


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2) Setting display range for each set of data independently Select [Range - By data] from the [Display] menu. The <Range window>, for inputting the range, will be displayed with 2 vertical lines at each side of the screen. The DSC data file selected first will be displayed. The range may be set using either the mouse or by key input, followed by selection of the [OK] button. Then the next DSC data file will be displayed. When all of the selected data files are displayed and ranges set independently, the data are then displayed together on the overlay screen. If you wish to cancel any of the range settings, select [Range Cancel] in the [Display] menu.

4.2.4 Changing the display position This is used for changing the display position. By changing this, analysis can be performed easily. The following methods are available.

CAUTION

Setting the display range prior to changing the display facilitates the position change procedure.

1) Aligning the start point for each set of data Select [Auto Start Point Arrangement] from the [Display Position] menu. The start point for each set of data will be aligned and displayed on the screen.

2) Staggering the start points at fixed intervals for each set of data Select [Auto Slide] from the [Display Position] menu. The <Auto Slide window> will open, allowing you to set the number of points by which the start points will be staggered. After making the setting, select the [OK] button. The data will be drawn on the screen sequentially, staggered according to the value entered.

NOTE

The sequence in which the data will be loaded for display can be verified in the <Display Parameters window>. Refer to 5.1.2.1 Display Parameters.

3) Positioning each set of data independently for display Select [Manual Slide] from the [Display Position] menu. The <Manual Slide window> with its [Test] button will be displayed. At the same time, a square mark will be displayed at the start point of the displayed data. The mouse can be used to drag the data by the square mark to the desired location on the Y-axis. After positioning the data, select the [OK] button. The <Manual Slide window> will close, and the data will be redrawn on the screen, repositioned to where the square mark was set.


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4.2.5 DSC Kinetic Analysis After setting the analysis range, the kinetic analysis is conducted on the basis of that range, and the results are displayed on the screen. The methods available for performing the kinetic analysis using this scenario are as follows.

• Performing kinetic analysis by selecting the analysis range from the overlaid data [Kinetic Analysis] in the [Analysis] menu

• Performing kinetic analysis by selecting the analysis range for each set of data independently [Kinetic Analysis - By data] in the [Analysis] menu

• Performing kinetic analysis by selecting the range and peak point for each set of data [Kinetic Analysis - Select peak] in the [Analysis] menu

After setting the analysis range, select the [Analyze] button in each of the Analysis windows.

• Except for the [Kinetic Analysis] item in the [Analysis] menu, calculation is automatically performed following the range setting.

The analysis results based on the set analysis range are displayed in the <<DSC Kinetic Analysis Program (Ozawa method) window>> along with all of the employed DSC data, and at the same time, the <Ozawa Plot window> is opened, displaying the relationship between the log of the heating rates and the inverse of the peak temperatures.

NOTE

For details on each of the analysis procedures, refer to 4.3 DSC Kinetic Analysis operation procedures.

4.2.6 Isothermal Analysis Select [Isothermal Analysis] from the [Analysis] menu. When the <Isothermal Analysis - Input Temperature window> opens, select the kinetic energy to be used in the analysis from the combo box, set the temperature you wish to use for analysis, and press the [Analyze] button. The relation between the reaction rate and reaction time based on the analysis temperature is determined, and the result is displayed in the <Isothermal Analysis window>.

NOTE

For details on each of the analysis procedures, refer to 4.4 Isothermal Analysis operation procedures.

4.2.7 Report output In the [Report] menu, the various analysis items to be included in the report are selected. The items which may be output include the DSC data overlay plot, the Ozawa plot, isothermal analysis result and analysis parameters. By selecting [Print Preview] from the [File] menu in the <Report window>, you may view an image of the report prior to the actual printout.

NOTE

For details on setting up a report, refer to 5.1.6 [Report] menu.


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4.2.8 Storing results of Kinetic Analysis The analysis results of DSC Kinetic Analysis are stored in a kinetic analysis result file. The file extension of this stored file is .KD0.

• Select [Save] from the [File] menu. This saves an existing kinetic analysis result file to the same name, overwriting the previous results.

• Select [Save As] from the [File] menu.

This opens the <Save Analyzed File As window>, allowing you to specify a new name for the kinetic analysis result file to be saved. Press the [Save] button to store the results under the newly named file. If the indicated file name already exists, a warning message to that effect is displayed.

4.2.9 Closing the <<DSC Kinetic Analysis Program (Ozawa method) window>> Select [Exit] from the [File] menu. If the analysis results have not yet been saved, the box for saving the data is displayed which allows you to save the file before closing the window.


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4.3 DSC Kinetic Analysis operation procedures The following items may be analyzed in the kinetic analysis program.

• Kinetic energy (kJ/mol, kcal/mol) • Reaction order • Frequency factor (min-1) • Ozawa plot (LOG A - 1/T) • Analysis start point, end point, peak temperature (K or °C)

CAUTION

If the kinetic energy has not been determined, isothermal analysis cannot be performed.

4.3.1 Kinetic Analysis The start and end points are set while the DSC data is overlaid on the screen. The analysis can then be performed. Before carrying out this step, analysis can be conducted simply by displaying only the analysis range according to 4.2.3 Setting the display range, and aligning the start points according to 4.2.4 Changing the display position.

CAUTION

Since the range is set while the DSC data is overlaid on the screen, if the analysis range is different for each set of data, refer to section 4.3.2 Kinetic Analysis - By data.

1. Select [Kinetic Analysis] in the [Analysis] menu. The < Kinetic Analysis window> with an

[Analyze] button, will be displayed. 2. Select the [Options] button to specify the various analysis items. Enter any comments as

necessary.

NOTE

Refer to 4.3.4 Kinetic Analysis Options 3. Click on the screen to set the analysis start point (the point where the peak starts to rise) and the

analysis end point (where the signal curve returns to baseline).


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NOTE

When setting the analysis range, be sure to select stable portions of the curve at either end of the peak.

4. To move the vertical lines for setting the start and end points, move the mouse cursor to one of

the lines so that the cursor shape is changed. Press the left mouse button and drag the line to the desired location. Release the mouse button to set the line.

5. Click the [Analyze] button. Analysis is performed and the analysis result (kinetic energy, etc.) is

displayed at the upper right portion of the screen. If display of the Ozawa Plot was specified in the <Kinetic Analysis Options window>, the <Ozawa Plot window> is opened at the same time, displaying the log of the heating rates and the inverse of the peak temperatures used to determine the kinetic energy.

6. If Set Group Position was selected as one of the kinetic analysis options, the <Set Group

Position window> will be opened, displaying an auxiliary box at the site where the analysis results will be displayed. Click the mouse at the site you wish to display this, or use the mouse to drag it to the desired location, and select [OK]. The analysis results will be displayed at the desired location.

NOTE

If there are 2 or more kinetic analyses, the most recent kinetic analysis result will be displayed in the <Ozawa Plot window>.

CAUTION

The kinetic energy is calculated from the area included between the boundaries of the DSC curve and a straight line connecting the analysis start and end points.


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4.3.2 Kinetic Analysis - By data This is used to set the analysis start point and end point for each set of data independently. 1. Select [Kinetic Analysis - By data] from the [Analysis] menu. The <Range window>, for the

analysis range, will be displayed with 2 vertical lines at each side of the screen. 2. In the <Range window>, either the mouse or keyboard is used to set the analysis start and end

point, and the [OK] button is selected. The X-axis range is set as temperature. The DSC data which was selected first will be displayed.

Mouse Using the mouse, drag the vertical lines to the desired analysis start and end points, respectively.

Keyboard Use the keyboard to directly input the analysis start and end points.

3. The DSC data file which was selected next will then be displayed with the vertical lines

positioned at the locations set for the previous data.

NOTE

[Exit] button : Cancels setting of analysis range and analysis. [Back] button : Returns to the analysis range setting screen of the data displayed just previous to the

currently displayed data. 4. Repeat steps 2 and 3 until the analysis ranges have been set for all the data. 5. When all of the data ranges are set, the <Range window> disappears and all of the DSC data are

then displayed together in overlay fashion in the <<DSC Kinetic Analysis Program (Ozawa method) window>>. In addition, the analysis results (kinetic energy, etc.) are displayed at the upper right portion of the screen. If display of the Ozawa Plot was specified in the <Kinetic Analysis Options window>, the <Ozawa Plot window> is opened at the same time, displaying the log of the heating rates and the inverse of the peak temperatures (Ozawa Plot) used to determine the kinetic energy.


Position window> will be opened, displaying an auxiliary box at the site where the analysis results will be displayed. Click the mouse at the site where you wish to display the results, or use the mouse to drag it to the desired location, and select [OK]. The analysis results will be displayed at the indicated position.


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7. The <Kinetic Analysis - [Key Input] window> will then open.

[Next Analysis] .... This resets the analysis range and executes analysis. [Exit] .... This exits the analysis. [Options] .... This is used for setting the various analysis items and units. You may also

enter a comment as necessary.

NOTE

Refer to 4.3.4 Kinetic Analysis Options.

NOTE



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4.3.3 Kinetic Analysis - Select peak For each set of data, the analysis range (analysis start and end points) and the peak point are specified, and analysis is conducted. This function is used when the peak is smooth, or when you wish to specify the peak based on literature, etc. 1. Select [Kinetic Analysis - Select peak] from the [Analysis] menu. The <Range - Select peak

window> will open, enabling you to set the analysis range. At each side in the window, two vertical cursors will also be displayed.

2. In the <Range - Select peak window>, either the mouse or keyboard is used to set the analysis

start point and the analysis end point, as well as the peak point, and the [OK] button is then selected. The X-axis is set as temperature. The DSC data which was selected first will be displayed.

Mouse Using standard mouse operation, drag the vertical lines to the desired analysis start, end and the peak points.

Keyboard

Use the keyboard to directly input the analysis start, end and the peak points.

3. The DSC data file which was selected next will then be displayed, with the vertical lines positioned at the locations set for the previous data.

NOTE

The peak point-indicating cursor automatically searches the peak point for that set of data, and is displayed at that position. [Exit] button : Cancels setting of analysis range and analysis. [Back] button : Returns to the analysis range setting screen of the data displayed just

previous to the currently displayed data. 4. Repeat steps 2 and 3 until the analysis ranges and peak points have been set for all the data. 5. After all the ranges and peak points are set, the <Range - Select peak window> disappears and

all of the DSC data are then displayed together in overlay fashion in the <<DSC Kinetic Analysis Program (Ozawa method) window>>. The analysis results (kinetic energy, etc.) are displayed at the upper right portion of the screen.


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If display of the Ozawa Plot was specified in the <Kinetic Analysis Options window>, the <Ozawa Plot window> is opened at the same time, displaying the log of the heating rates and the inverse of the peak temperatures used to determine the kinetic energy.


Position window> will open, displaying an analysis results positioning box at the site where the analysis results will be displayed. Click the mouse at the site where the results are to be displayed, or use the mouse to drag it to the desired location, and select [OK]. The analysis results will be displayed at the desired position.

7. The <Kinetic Analysis - [Key Input] window> will then open.

[Next Analysis] .... This resets the analysis range and executes analysis. [Exit] .... This exits the analysis. [Options] .... This is used for setting the various analysis items and units. You may also

enter a comment as necessary.

NOTE

Refer to 4.3.4 Kinetic Analysis Options.

NOTE



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4.3.4 Kinetic Analysis Options Selecting the [Options] button in the <Kinetic Analysis window> or <Kinetic Analysis-[Key Input] window> will open the <Select - DSC Kinetic Analysis window>. Arranged in the <Select - DSC Kinetic Analysis window> are all of the items which may be designated for analysis, in addition to the analysis units which may be used. Clicking on a unit to be used for an analysis will place an check mark in the checkbox preceding the unit selected. Analysis is performed on the basis of items or units with a selected checkbox.

Here you may set whether or not the Kinetic Energy, Reaction order, Frequency factor and the Ozawa Plot will be displayed, as well as the analysis units to be used. In addition, you may also enter an annotation to be used for each of the analysis results. (A maximum of 32 characters may be entered.) To display the analysis results at a specific location on the screen, select the Group Mode option. In addition, selecting the “Temperature” checkbox will cause the temperature to be displayed at the analysis start and end points and the peak point for each set of data.

CAUTION

These option settings are applied to all the Kinetic Analysis modes in common. The set items are retained, so it is not necessary to set them each time.


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4.4 Isothermal Analysis operation procedures Before performing the Isothermal Analysis, it is necessary to first determine the kinetic energy by conducting the kinetic analysis. Also, verify that the data to be analyzed has the target reaction rate before performing the analysis. (Note that if the reaction rate cannot be determined, accurate isothermal analysis results cannot be obtained.) In Isothermal Analysis, the relation between reaction percent and time at a constant temperature, in addition to the following items, can be analyzed or displayed.

• Kinetic Energy (kJ/mol, kcal/mol) : Average of kinetic energies obtained from kinetic analysis. • Reaction order • Frequency factor (min-1) : Frequency factor determined from kinetic analysis. • Analysis temperature (K or °C) : Temperature at which analysis was conducted. • Rate constant (min-1) : Rate constant determined by Arrhenius formula. • Reaction time (hour) : Isothermal analysis X-axis values • Reduced time (hour)

4.4.1 Isothermal Analysis 1. Select [Isothermal Analysis] from the [Analysis] menu. The <Isothermal Analysis - Input

Temperature window> with its [Analyze] button will be displayed.

CAUTION

If Isothermal analysis is conducted prior to selecting this, and the <Isothermal Analysis window> is displayed, a message will be displayed inquiring as to whether or not you wish to save the analysis results.

2. Select the [Options] button to specify the various analysis items as well as annotations.

NOTE

Refer to 4.3.2 Isothermal Analysis options. 3. Next, enter the temperatures to be used in Isothermal Analysis (maximum 6 temperatures). The

temperature values will be sorted and recorded in sequence from lower to higher temperature.


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NOTE

• To perform a 0°C analysis, enter 0.0 between setting values. • The temperature unit refers to the unit used for the X-axis in the DSC data display. If you wish to

change the unit, select [Display Parameters] from the [Display] menu, and change the X-axis unit appropriately. Refer to 5.1.2.1 Display Parameters

4. Select the [Analyze] button.

The relation between the reaction percent and time will be obtained with respect to the temperatures set in the table, and the result will be displayed in the <Isothermal Analysis window>. In addition, the designated analysis items will also be displayed with the Isothermal Analysis results.

5. If Group Mode was selected as one of the Thermal Analysis options, the <Set Group Position

window> will be opened. An analysis result positioning box is displayed at the site where the analysis results will be displayed. Click the mouse at the site where you wish to display the results, or use the mouse to drag it to the desired location, and select [OK]. The analysis results will be displayed at the desired position.

CAUTION

If a wide temperature range was used, the data may be overlapped in the display.


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4.4.2 Isothermal Analysis options When the [Options] button is selected in the <Isothermal Analysis - Input Temperature window>, the <Setting - Isothermal Analysis window> is opened. The <Setting - Isothermal Analysis window> enables the selection of the unit to be used for the Kinetic Energy, and whether or not Reaction order, Frequency factor, Reduced time, Analysis temperature, Rate constant and Reaction time are displayed. You may also enter an annotation to be used for each of the analysis results. (A maximum of 32 characters may be entered.) To display the analysis result at a desired location, select the Group Mode checkbox.

Clicking on a unit to be used for the Kinetic Energy or on one of the other items to be used, will place an × mark in the checkbox preceding the item selected. The items selected will be displayed in the <Isothermal Analysis window>.

CAUTION

• If the analysis results are not displayed on the screen, change the font size or separate the thermal analyses into smaller groups.

• The set items are retained so it is not necessary to set them each time.


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4.5 DSC Kinetic Analysis Configuration This is for setting the default environment to be valid when the DSC Kinetic Analysis program is first initialized. The configuration settings made here are valid only in the <<DSC Kinetic Analysis Program (Ozawa method) window>>.

4.5.1 Options 1. Select [Options] from the [File] menu. 2. The window for setting the environment of the <<DSC Kinetic Analysis Program (Ozawa

method) window>> will open.

• Load Data Folder

This sets the name of the default folder to be used for selecting files. Selecting the [Folders] button will display a list of folders from which the appropriate folder may be selected.

• Select Analysis Range

This specifies whether or not the analysis range (display range) is to be selected when data is loaded. To enable selection of the analysis range, click on the “Select Analysis Range” check box to place a check mark in it. The range selection will be performed on the overlaid DSC data.

3. Select the [OK] button. The configuration settings will then become valid.


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5 DSC Kinetic Analysis Program Functions

5.1 <<DSC Kinetic Analysis Program (Ozawa method) window>> menu items

5.1.1 [File] menu

5.1.1.1 Open This is used when you wish to open a data file for DSC Kinetic Analysis. The following files may be opened for use with DSC Kinetic Analysis. 1) Kinetic Analysis with this software may be conducted using raw data acquired with the

Shimadzu Differential Scanning Calorimeter (DSC-60 or DSC-50), corrected data files (files with extension .D?0... vary according to the type of correction), or previously analyzed analysis result files (file extension .R??). However, when loading analysis result files for analysis, the analysis results in those files cannot be displayed. (Only the data in the analysis results file can be used.)

2) After conducting DSC Kinetic Analysis, the analysis result and plot information are stored

in a Kinetic Analysis result file (file extension: .KD0).

CAUTION

All of the data to be analyzed is to have been acquired using the same measurement parameters, except for different heating rates. The sample weight must also be entered.

<Operation>

In the <Open File window>, the data files in the folder specified as the Load Data Folder using the DSC Kinetic Analysis Defaults are displayed.

①

②

③

④

⑦⑥

⑧

⑨⑤


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If required, a folder name will be changed and a file will be chosen. The file of the folder set up as the [option] of DSC Kinetic Analysis is displayed on a <Open File window>.

Item ① Folder

Displays the folder in which the file is stored.

② Folder list box This displays the current folder (drive).

③ File name text box

This displays the file name of the file selected in the File list box. To directly specify the name of the file to be loaded, enter the file name here.

④ File list box

This is the list box from which the file name is selected. The files in the displayed folder corresponding to the file type selected in the [Type] menu are listed.

⑤ Selected file list box

This displays the files which have been selected in the File list box.

⑥ [Select] button This selects the file. The file you selected will be displayed in the Selected file list box. Double clicking on a file in the File list box performs the same function as this button.

⑦ [Remove] button

This removes a selected file from the Selected list box.

⑧ [Open] button This loads a selected file in the Selected file list box, and closes the <Open File window>.

⑨ [Cancel] button

This cancels loading of files, and closes the <Open File window>.

Menu [Preview] : Displays information about the file. [Type] : Sets the type of files and data to be displayed in the File list box. [Sort] : Sorts the listing of files in ascending or descending order of file

name, Acquisition Date and Time, etc. [Help] : Displays help messages related to the <Open File window>


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Selecting data files for Kinetic Analysis

CAUTION

Since the DSC Kinetic Analysis Program is based on the Ozawa Method, three or more data files (file extension .D?0, .R??, maximum 12 files), having the same measurement parameters with different heating rates only may be selected.

1. In the upper level list box, highlight an appropriate file name of data to be used for kinetic

analysis, and click the [Select] button. Double clicking with the mouse on the file name will also select it. The selected file name will be displayed in the lower level list box. In the same way, select three or more files (maximum 12 files) of the same sample. If a desired file is not in the currently displayed folder, change folders in order to select that file.

2. After selecting all of the data files to be analyzed, select the [Open] button.

3. All of the selected DSC data will be displayed on the screen.

CAUTION

All of the data to be analyzed is to have been acquired using the same measurement parameters, except for different heating rates. The sample weight must also be entered. If an analysis result file (.R??) is loaded for analysis, only the data in the result file is loaded, and the analysis results cannot be displayed on the screen.

Selecting Kinetic Analysis result file 1. In the upper level list box, highlight the kinetic analysis result file (file extension .KD0), and

click the [Select] button or, double click on the file name with the mouse. The selected file name will be displayed in the lower level list box.

2. Select the [Open] button.

3. The kinetic analysis result file will be displayed on the screen.

CAUTION

When a kinetic analysis result file is selected, another file cannot be selected at the same time. Select only one kinetic analysis result file and press the [Open] button. (Only one kinetic analysis file can be displayed in the lower list box.)

NOTE

If you wish to remove a selected file name from the lower list box, click on that file name and select the [Remove] button. The file name will be deleted from those displayed in the lower list box.


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5.1.1.2 Save This is selected to store the results of a kinetic analysis to disk using the DSC Kinetic Analysis software. Stored along with the kinetic analysis result are the isothermal analysis results, data and data display information, and scale information, etc. When a stored analysis result file is opened, the analysis results are restored as they were when the file was saved. The kinetic analysis result file has the extension .KD0. When creating multiple files from the same data, change the base file name. If a file with the same name exists on the disk, a warning message will be displayed. Change the file name of the analysis results and save it under a different name, as described in the next section (Sec. 5.1.1.3).

5.1.1.3 Save As This is used to specify a new name for a kinetic analysis result file, and to save that file under the new name. The base file name is the portion of the file name which is newly specified. If a file with the same name already exists on the disk, a warning message will be displayed. <Operation>

Select [Save As] from the [File] menu. The window for entering the file name will open. If necessary, change the folder, enter a file name, and then select the [Save] button.

The kinetic analysis result file will be saved using the newly entered file name using the .KD0 extension.

5.1.1.4 Options This item is used to set the configuration which will be valid when the DSC Kinetic Analysis software is first started up. The configuration items which may be set are as follows.

• Default folder to be used when the <Open File window> opens. • Mode which determines whether or not selection of the analysis range (display) is

performed when the data is loaded. <Operation>

Refer to 4.5 DSC Kinetic Analysis Configuration

5.1.1.5 Exit This is used to close the <<DSC Kinetic Analysis Program (Ozawa method) window>>. <Operation>

Select [Exit] from the [File] menu.


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5.1.2 [Display] menu

5.1.2.1 Display Parameters This is used to change the unit for the X-axis (temperature) and Y-axis (DSC signal), and the color and type of curve. <Operation>

Select [Display Parameters] from the [Display] menu. The <Display Parameters window> will open.

The X-axis unit, file name, Y-axis unit, display lines used and Display ON/OFF status are displayed. The X-axis unit is changed via the combo box above the table. To change the Y-axis unit and the type and color of line used, move the table cursor (black border) to the row which you wish to change, and select the [Setting] menu, or double click on the row you wish to change. The <Display Parameters setting window> will open.

After making the appropriate settings, select the [OK] button. The <Display Parameters window> will return. After the settings have been made for all of the data, select the [OK] button. The screen will be redrawn based on the new Display Parameters settings.

CAUTION

If the [Off] option is selected for the Display On/Off item, kinetic analysis cannot be performed. Be sure to select the Display [On] option if kinetic analysis is to be performed.


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5.1.2.2 Range This is used to set the display range when it is appropriate to cut off unnecessary portions of the data. This item sets the range while the DSC data is overlaid. However, when there are analysis results, please note that they will all be deleted. <Operation>

Select [Range] from the [Display] menu. The <Display Range Setting button> will be displayed at the top of the window.

Clicking the mouse while the cursor is positioned over the graph will cause 2 blue auxiliary lines to appear. Use the mouse to move the auxiliary lines to limit the curve to the desired range. Press the [OK] button to set the display range and redraw the screen.

5.1.2.3 Range - By data In kinetic analysis, since at least 3 sets of data are overlaid at the same time, it may be difficult to set the range. This item allows you to set the display range for each set of data separately, eliminating all but the portions that you wish to analyze. <Operation>

Select [Range - By data] from the [Display] menu. The data file first selected will be displayed in the window, with the <Range window> displayed at the top.

At this time, two auxiliary lines will appear at each end of the window. Use the mouse to move the auxiliary lines to limit the curve to the desired range. You may also enter the range values directly from the keyboard. Press the [OK] button. The next DSC data file will be displayed. When all of the ranges have been set, the curves will automatically be redrawn on the screen.

5.1.2.4 Range Cancel This is used to undo the display range operation performed in Section 5.1.2.2 and 5.1.2.3. The set range is canceled and the entire range of data is redisplayed on the screen. <Operation>

Select [Range Cancel] from the [Display] menu.

5.1.2.5 Cross Cursor This is used to toggle the on/off display of a cross-shaped cursor, which allows you to read the values of the cursor position at the vertical and horizontal axes when they are displayed. <Operation>

Select [Cross Cursor] from the [Display] menu. If the axis cursor is displayed, a check mark is placed in front of this item. Selecting this item again will remove the axis cross cursor.


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5.1.3 [Scale] menu

5.1.3.1 Key Input This is used the change the display scale of the X-axis (temperature) and Y-axis (DSC signal) by entering the values from the keyboard. <Operation>

Select [Key Input] from the [Scale] menu. The <Scale (Key Input) window> will appear, allowing you to change the scale.

Enter appropriate values for the X-axis and Y-axis scale, and press the [OK] button. The auxiliary lines displayed on the graph (black for X-axis, curve color for Y-axis) will move to the locations of the respective entered values. It is also possible to change the scale by dragging an auxiliary line using the mouse.

5.1.3.2 Zoom This is selected when you wish to use the mouse to zoom in on a portion of the graph. <Operation>

Select [Zoom] from the [Scale] menu. The <Zoom window> will appear at the top of the screen.

Press the left mouse button at one corner of the area of interest to be zoomed, and drag the mouse to the opposite corner of the area of interest. (A rectangular frame will be displayed on the graph, indicating the area to be zoomed.) When you release the mouse button, only the specified area will be displayed. You may continue the zooming procedure as many times as desired, until the [Exit] button is pressed to close the window. Checking the "Adjust the factions" check box allows you to perform "fraction processing". Fraction processing ends the maximum and minimum values or omits them so that the scale span is balanced.

5.1.3.3 Undo Scale This is used to restore the current scale to the previous scale. <Operation>

Select [Undo Scale] from the [Scale] menu. Selecting [Undo Scale] again will toggle the scale back to the previous scale setting.

5.1.3.4 Default Scale This restores the scale to the original scale. The original scale refers to the entire range of the DSC data which was loaded from the file. <Operation>

Select [Default Scale] from the [Scale] menu.


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5.1.4 [Analysis] menu

5.1.4.1 Annotation This is used to position annotations as desired on the DSC Kinetic Analysis graph. <Operation>

Select [Annotation] from the [Analysis] menu. The <Annotation window> will open.

To close this window, press the [Exit] button. By entering a character string in the edit box and pressing the [Annotate] button, the entered text is displayed on the graph. (Up to 32 characters may be used for one annotation.) In addition, clicking the mouse on the graph will move that annotation to the location where you choose. The entered annotation is displayed in a rectangle. (The size of the rectangle depends on the number of characters comprising the annotation.)

5.1.4.2 Move This is used to reposition analysis result values or annotations at a desired location on the DSC Kinetic Analysis graph. <Operation>

Select [Move] from the [Analysis] menu. The <Move window> will open.

To move the result values or annotations, move the cursor to that object so that the cursor becomes cross-shaped. Pressing down the mouse button will cause the frame around that object to be displayed. Drag the object to the desired location, and release the mouse button to set the result or annotation at its new position. To close this window, press the [Exit] button.

5.1.4.3 Delete This is used to delete an analysis result or annotation currently on the DSC Kinetic Analysis graph. <Operation>

Select [Delete] from the [Analysis] menu. The <Delete window> will open. To close this window, press the [Exit] button.

To delete a result or annotation, move the cursor to that object so that the cursor becomes cross-shaped. Pressing down the left mouse button will cause the frame around that object to be displayed. Releasing the mouse button will delete that result or annotation.


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5.1.4.4 Reset Group The position of the displayed results of the kinetic analysis can be repositioned as a group. The function does not allow changing the actual contents of the character strings. <Operation>

Select [Reset Group] from the [Analysis] menu. The <Group Position window> will open.

The result to be repositioned is selected from a combo box. (The analysis result character string will be displayed in a red frame.) Click the mouse at the desired position, or drag the frame using the mouse. Select the [Reset] button to move the framed character string. To close this window, select the [Exit] button.

5.1.4.5 Delete Group This is used to delete the results of kinetic analysis in groups. Note that if all the results are deleted, the <Ozawa Plot window> will also be deleted. <Operation>

Select [Delete Group] from the [Analysis] menu. The <Group Delete window> will open.

The result to be deleted is selected from a combo box. (The analysis result character string is displayed in a red frame.) When the [Delete] button is pressed, the character string which is framed will be deleted. To close this window, select the [Exit] button.

NOTE

If there are 2 or more kinetic analyses, the result of the most recent kinetic analysis is displayed in the <Ozawa Plot window>. Each time a kinetic analysis result is deleted, the result from the kinetic analysis performed previously in sequence is displayed in the <Ozawa Plot window>.

5.1.4.6 Delete Isothermal Analysis This deletes the <Isothermal Analysis window> (Isothermal Analysis result) if Isothermal Analysis has been performed. <Operation>

Select [Delete Isothermal Analysis] from the [Analysis] menu. The <Isothermal Analysis window> will be deleted.


－ 35 －

5.1.4.7 Clear This is used to delete all analysis results currently displayed on the graph, including any annotations. The Ozawa Plot and Isothermal Analysis windows will be deleted at the same time. <Operation>

Select [Clear] from the [Analysis] menu. All analysis results and annotations will be deleted from the graph.

5.1.4.8 Kinetic Analysis This is used to determine the reaction rate based on the analysis range which is set while the DSC data is overlaid on the screen. At the same time, the <Ozawa Plot window> is opened, displaying the heating rate log and the inverse of the peak temperature (Ozawa plot) used in determining the kinetic energy. The horizontal axis is (1/T) [/K], and the vertical axis is LOG A. The range is set while the DSC data is overlaid on the screen. If different analysis ranges are to be used, follow the procedure described in Section 5.1.4.9 Kinetic Analysis - By data. <Operation>

Refer to Section 4.3.1 Kinetic Analysis

5.1.4.9 Kinetic Analysis - By data This is used to determine the reaction rate based on the analysis range which is specified for each set of DSC data independently. At the same time, the <Ozawa Plot window> is opened, displaying the heating rate log and the inverse of the peak temperature (Ozawa plot) used in determining the kinetic energy. The horizontal axis is (1/T) [/K], and the vertical axis is LOG A. This analysis function is used when you wish to use a different analysis range for each set of data. <Operation>

Refer to Section 4.3.2 Kinetic Analysis - By data

5.1.4.10 Kinetic Analysis - Select peak This is used to determine the reaction rate based on the analysis range and peak which are specified for each set of DSC data separately. At this time, the <Ozawa Plot window> is opened, displaying the heating rate log and the inverse of the peak temperature (Ozawa plot) used in determining the kinetic energy. The horizontal axis is (1/T) [/K], and the vertical axis is LOG A. This analysis function is used when the peak is smooth, or when you wish to specify the peak based on literature, etc. <Operation>

Refer to Section 4.3.3 Kinetic Analysis - Select peak


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5.1.4.11 Isothermal Analysis The kinetic energy obtained from the kinetic analysis is used to calculate the reaction percent and reaction time with respect to a constant temperature, and display these results in the <Isothermal Analysis window>. The X-axis is time in hours, and the Y-axis is Reaction Percent. However, before performing the calculation, verify target reaction percent and reaction rate of the data to be analyzed. <Operation>

Refer to Section 4.4.1 Isothermal Analysis


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5.1.5 [Display Position] menu

5.1.5.1 Default display This is used to automatically adjust the scale of the vertical and horizontal axis so that all of the data, from the smallest to the largest value, will be displayed on the screen. The Y-axis value will be common to each set of data values. <Operation>

Select [Default Display] from the [Display Position] menu. The data will be moved so that all of the data is displayed on the screen.

5.1.5.2 Auto Start Point Arrangement This is used to automatically shift (slide) each set of data along the Y-axis so that the respective start points of all the data are aligned.

CAUTION

The Y-axis values and the data values will no longer correspond. <Operation>

Select [Auto Start Point Arrangement] from the [Display Position] menu. The data will move so that all of the start points are aligned.

→

5.1.5.3 Auto Slide This is used to automatically shift the data so that the start point of each set of data is offset in the Y-axis direction by a specified fixed value.

CAUTION


Select [Auto Slide] from the [Display Position] menu. The <Auto Slide window> will open.


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Enter a value from -50 to 50 in the Slide Offset text box, and then select the [OK] button. The data will be drawn in the <<DSC Kinetic Analysis Program (Ozawa method) window>> at the specified fixed starting point intervals in the order that is loaded into the window.

NOTE

The entered value causes the data to move an amount based on the Y-axis scale normalized to 100. If a positive value is entered, the first set of data which is loaded slides downward. If a negative value is entered, the data slides upward.

→

5.1.5.4 Manual Slide This is used to allow you to reposition the data as desired using the mouse.

CAUTION


Select [Manual Slide] from the [Display Position] menu. The <Manual Slide window> with its [Test] button will be displayed. At the same time, a square mark will be displayed at the start point of the displayed data. The mouse can be used to drag the data by the square mark to the desired location on the Y-axis. After positioning the data, select the [OK] button. The <Manual Slide window> will close, and the data will be redrawn on the screen, repositioned at the position where the square mark was set. [Test] button : The data is temporarily drawn with the start point at the position of the

square mark. [Cancel] button : Cancels the manual slide operation.

→


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CAUTION

If the [Cancel] button is selected, the slide which was performed using the [Test] button will be invalidated, and the data will return to its original display position.


－ 40 －

5.1.6 [Report] menu

5.1.6.1 All Analysis Result This is used to output a report of all the analysis results (overlaid DSC data, Ozawa plot and Isothermal Analysis window) performed in the <<DSC Kinetic Analysis Program (Ozawa method) window>>. In addition to the plots, the file information and the measurement program, etc., may also be output.

<Operation>

Select [All Analysis Result] from the [Report] menu. The <Report window> used for formatting all of the kinetic analysis results will be opened. From the <Report window> [Item] menu, select the following items.

[Multiview Graph] [Kinetic Graph] [Isothermal Graph]

Only the items currently displayed as analysis results will be available for selection. After setting up the report format, select the [Print] button to print out all of the kinetic analysis results.

NOTE

By selecting the [Print Preview] item in the [File] menu of the <Report window>, you may preview the report as it will appear when printed.

NOTE

For a detailed description of the <Report window>, refer to Section 5.4 <Report window> menu item


－ 41 －

5.1.6.2 Kinetic Analysis This is used to output the results of kinetic analysis (overlay DSC data, Ozawa plot) in report format. In addition to graphed screens, file information and analysis programs may also be reported.

<Operation>

Select [Kinetic Analysis] from the [Report] menu. The <Report window> used for formatting the kinetic analysis results will be opened. From the <Report window> [Item] menu, select the following items.

[Multiview Graph] [Kinetic Graph]

After setting up the report format, select the [Print] button to print out the kinetic analysis results.

NOTE


NOTE



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5.1.6.3 Isothermal Analysis This is used to output the Isothermal Analysis results in report format. In addition to graphed screens, information stored in files and analysis programs may also be reported.

<Operation>

Select [Isothermal Analysis] from the [Report] menu. The <Report window> used for formatting the Isothermal Analysis results will be opened. Select [Isothermal Graph] from the [Item] menu in the <Report window>. After setting up the report format, select the [Print] button to print out Isothermal Analysis results.

NOTE


NOTE



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5.1.7 [Window] menu

5.1.7.1 Ozawa Plot The analysis result displayed in <Ozawa Plot window> is always present as an icon in the <<DSC Kinetic Analysis Program (Ozawa method) window>>, available whenever processing is necessary. This menu item is used for reopening the window whenever necessary. <Operation>

Select [Ozawa Plot] from the [Window] menu. The <Ozawa Plot window> will be reopened to its original size and location on the screen.

5.1.7.2 Isothermal Analysis The analysis result displayed in the <Isothermal Analysis window> is always present as an icon in the <<DSC Kinetic Analysis Program (Ozawa method) window>>, available whenever processing is necessary. This menu item is used for reopening the window whenever necessary. <Operation>

Select [Isothermal Analysis] from the [Window] menu. The <Isothermal Analysis window> will be reopened to its original size and location on the screen.


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5.2 <Ozawa Plot window> menu items


5.2.1.1 Display Parameters This is used to change the color and style of lines and marks in the Ozawa plot. <Operation>

Select [Display Parameters] from the [Display] menu in the <Ozawa Plot window>. The <Style Setting window> will open.

After completing the settings, select the [OK] button. These settings will then be used in the display of the <Ozawa Plot window>.

5.2.1.2 Cross Cursor This is used to toggle the on/off display of the cross cursor, which enables you to read the vertical and horizontal axis values corresponding to the cross cursor location on the Ozawa Plot. <Operation>

Select [Cross Cursor] from the [Display] menu in the <Ozawa Plot window>. When the axis cross cursor is displayed, a check mark will be placed in front of this item. Selecting this item again will remove the check mark, and the axis cross cursor will be removed.

5.2.2 [Report] menu This is used to output the Ozawa Plot as a report. When the <Report window> opens for setting the kinetic analysis report format, make the appropriate settings, and click the [Print] button. The kinetic analysis results will be output in a report. <Operation>

Refer to 5.1.6.2 Kinetic Analysis


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5.3 <Isothermal Analysis window> menu items


5.3.1.1 Reset Group This is for repositioning the displayed Isothermal Analysis results to a desired location. This function cannot be used to change the written contents of the group. <Operation>

Select [Reset Group] from the [Display] menu of the <Isothermal Analysis window>. The <Set Group Position window> will open.

At the same time, an auxiliary frame will be displayed around the analysis result character string. Click the mouse at the site in the window where you wish to reposition the results, or drag the frame to that position. Select the [OK] button to move the framed results to the indicated position. When the repositioning is completed, select the [OK] button. Press the [Cancel] button to cancel.

5.3.1.2 Display Parameters This is used to change the color and style of lines and marks of the graph in the <Isothermal Analysis window>. <Operation>

Select [Display Parameters] from the [Display] menu in the <Isothermal Analysis window>. The <Display Parameters window> will open, with the line names, displayed lines and mark settings indicated.

To change a displayed line or mark, move the cursor (black frame) to the row in the table where you wish to make a change, and select [Setting] menu, or simply move the cursor to the appropriate row and double-click. The <Style Setting window> will open.


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After completing the settings, select the [OK] button. The <Display Parameters window> will return. When all of the settings have been completed, select the [OK] button. These settings will then be used in the display of the <Isothermal Analysis window>.

5.3.1.3 Cross Cursor This is used to toggle the on/off display of the cross cursor, which enables you to read the vertical and horizontal axis values corresponding to the cross cursor location on the Isothermal Analysis graph. <Operation>

Select [Cross Cursor] from the [Display] menu in the <Isothermal Analysis window>. When the axis cursor is displayed, a check mark will be placed in front of this item. Selecting this item again will remove the check mark, and the axis cross cursor will be removed.

5.3.2 [Scale] menu

5.3.2.1 Key Input This is used to enter values from the keyboard to change the X-axis (hour) and Y-axis (C) display scale. <Operation>

Select [Key Input] from the [Scale] menu in the <Isothermal Analysis window>. The <Scale (Key Input) window> will appear, allowing you to change the scale.

Enter appropriate values for the X-axis and Y-axis scale, and press the [OK] button. The auxiliary lines displayed on the graph (black for-X axis, curve color for Y-axis) will move to the locations of the respective entered values. In addition, it is also possible to change the scale by dragging an auxiliary line directly using the mouse.

5.3.2.2 Zoom This is selected when you wish to use the mouse to zoom in on a portion of the graph. <Operation>

Select [Zoom] from the [Scale] menu in the <Isothermal Analysis window>. The <Zoom window> will appear at the top of the screen.

Press the left mouse button at one corner of the area of interest to be zoomed, and drag the mouse to the opposite corner of that area. (A rectangular frame will be displayed on the


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graph, indicating the area you wish to zoom.) When you release the mouse button, the specified area of interest will be displayed. You may continue the zooming procedure as many times as desired, until the [Exit] button is pressed to close the window. Checking the "Adjust the factions" check box allows you to perform "fraction processing". Fraction processing ends the maximum and minimum scale values or omits them so that the scale span is balanced.

5.3.2.3 Undo Scale This is used to restore the current scale to the previous scale. <Operation>

Select [Undo Scale] from the [Scale] menu in the <Isothermal Analysis window>. Selecting [Undo Scale] again will toggle the scale back to the previous scale.

5.3.2.4 Default Scale This restores the scale to the original scale. The original scale refers to the entire range of all the data which were loaded from the files. <Operation>

Select [Default Scale] from the [Scale] menu in the <Isothermal Analysis window>.

5.3.3 [Report] menu This is used to output the Isothermal Analysis results as a report. When the <Report window> opens for setting the Isothermal Analysis report format, make the appropriate settings, and click the [Print] button. The Isothermal Analysis results will be output in a report. <Operation>

Refer to 5.1.6.3 Isothermal Analysis


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5.4 <Report window> menu items It is used when outputting DSC Kinetic Analysis data and Isothermal Analysis data in report format The information stored in the file, and the measurement program as well can be output except for the drawing screen. <Operation>

A [Report] menu corresponding to each purpose is chosen. <Report window> opens.

5.4.1 [File] menu

5.4.1.1 Format Open Report format created in the <Report window> may be stored as files, and these may be loaded back into memory. <Operation>

Select the [Format Open] item in the [File] menu. A dialogue box will open for selecting a file. Change the directory if necessary, enter in the text box the filename that you want to load and then select the [Open] button.

CAUTION

Only report format files can be loaded.


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5.4.1.2 Format Save This will save the currently displayed report format. <Operation>

Select the [Format Save] command in the [File] menu. If there is no filename, the same dialogue box as that which appears when [Format Save As] is selected will open, enter the filename and select the [OK] button. If you wish to change the filename, select [Format Save As].

CAUTION

The format will be saved under the filename used when the file was loaded.

5.4.1.3 Format Save As This will saves the currently displayed report format to disk for the first time. A format which has already been saved may also be saved under a different filename. <Operation>

Select the [Format Save As] command in the [File] menu. A dialogue box will open for entering the filename. Change the directory if necessary, enter the filename and then select the [OK] button.

CAUTION

You do not need to enter an extension as one will be automatically added. The extension will be [.RFM].

5.4.1.4 Print Preview This window preview a report format. <Operation>

Select the [Print Preview] command in the [File] menu, or click the right mouse button. Opening <Print Preview> window.


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5.4.1.5 Print This will print a report. <Operation>

Select the [Print] command in the [File] menu. Or click on the [Print] button in the [Report] window.

5.4.1.6 Printer Set Select the printer on which the report will be printed. <Operation>

Select the [Printer Set] command in the [File] menu.

Select the printer to be set from the drop-down list box. Select the [Set up] button, and a dialogue box will open for setting a printer. After selecting the [OK] button, the screen will return to the printer selection screen. Select the [OK] button.

CAUTION

If the printer that you wish to set is not available, select the [Run Control] command in the [File] menu and install the printer driver.

5.4.1.7 Run Control This is for activating the Windows® Control Panel. When printing a report, if a printer driver has not been installed, you may install the printer driver from the [Control Panel] window. <Operation>

Select the [Run Control] command in the [File] menu. Control Panel will open. Select the printer.

CAUTION

See Control Panel Help for instructions on using Control Panel.

5.4.1.8 Exit Close the [Report] window.


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5.4.2 [Font] menu

5.4.2.1 Graph-Axis This will change the font used for the graph axis. <Operation>

Select the [Graph-Axis] command in the [Font] menu. A dialogue box will open for selecting fonts. Select the typeface name, height and width and then select the [OK] button.

If you clear the text box (no entries), the default values will be set. If the analysis results include a sub window as well as purity determination, the graph-axis font is changed at the same time.

CAUTION

If you select typeface name, the height and width will be automatically selected. To change these, either select the respective values in the list box or directly enter the values into the text box. The displayed numerical values refer to the number of dots in the character height.

CAUTION

Although any value may be entered for font height and width, the output font height and width will be closest to those of the actual printer.

5.4.2.2 Graph-Annotation This will change the font for the comments in a graph. <Operation>

Select the [Graph-Annotation] command in the [Font] menu. A dialogue box will open for selecting fonts. Select the typeface name, height and width and then select the [OK] button. Refer to 5.4.2.1 Graph-Axis for the change method of a font.


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5.4.2.3 Title This will change the font for the title. <Operation>

Select the [Title] command in the [Font] menu. A dialogue box will open for selecting fonts. Select the typeface name, height and width and then select the [OK] button. Refer to 5.4.2.1 Graph-Axis for the change method of a font.

5.4.2.4 Information/Program/Comments This will change the font used for the Information, programs and comments. <Operation>

Select the [Information/Program/Comments] command in the [Font] menu. A dialogue box will open for selecting fonts. Select the typeface name, height and width and then select the [OK] button. Refer to 5.4.2.1 Graph-Axis for the change method of a font.

5.4.3 [Item] menu

5.4.3.1 Multiview Graph, Kinetic Graph, Isothermal Graph This will set the each graph in a report. <Operation>

Select the each [Graph] command in the [Item] menu.

A dialogue box will open for setting the graph. Enter the line width (thickness) to be used to draw the data and then click the [OK] button.

• The line width that you can set is from 1 to 9.

• If you select [Auto String Size], the size of the text in the graph will be automatically set.

• If you wish to change a graph which has been set, select the [Graph] command in the

[Item] menu again, or double click inside the frame outline which opens the graph dialogue box. Make the desired changes and then click the [OK] button.


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• If you wish to delete a graph which has been set, select the [Graph] command in the [Item] menu again, or double click inside the frame outline which opens the graph dialogue box. Select the [Delete Item] button.

5.4.3.2 Title This will set the title in a report. <Operation>

Select the [Title] command in the [Item] menu.

A dialogue box will open for setting the title. Enter the title and then select the [OK] button. • Up to 80 characters may be entered.

• To return to the title prior to making changes, select the [Reset] button.

• If you wish to change a title which has been set, select the [Title] command in the [Item]

menu again, or double click inside the frame outline which shows the title. A dialogue box will open, make the changes and then select the [OK] button.

• If you wish to delete a title which has been set, select the [Title] command in the [Item]

menu again, or double click inside the frame outline which shows the title. A dialogue box will open. Select the [Delete Item] button.

5.4.3.3 Information 1, Information 2, Information 3,... This enables the user to write various Informations in a report. • Information can be displayed now for every multi-view file. The following items are available as Information.

• Filename • Sample name • Sample weight (DTA, DSC, TGA and DTG only) • Sample molecular weight (DTA, DSC,TGA and DTG only) • Sample length (TMA only) • Sample section area (TMA only) • Pan (Cell) type(DTA, DSC,TGA and DTG only) • Atmospheric gas • Gas flow rate • Operator name • Comments at time of measurement


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<Operation> Select the [Information] command in the [Item] menu. A dialogue box will open for setting the parameters.

Select the [Options] button, select the item that you want printed in the report and then select the [OK] button.

After setting the Information, select the [OK] button. A frame will be displayed showing the Information. • If you wish to copy the contents of Information, select the text that you wish to copy and

then select the [Copy] command in the [Edit] menu in the dialogue box. • If you wish to cut the contents of Information, select the text that you wish to cut, and

then select the [Cut] command in the [Edit] menu in the dialogue box. • If you wish to paste the contents of Information which has been copied, select the text

that you wish to paste, and then select the [Paste] command in the [Edit] menu in the dialogue box.

• To undo something that you have copied, cut, pasted, select the [Undo] command in the

[Edit] menu in the dialogue box. • If you wish to return a changed information to its condition prior to the changes, select

the [Reset] button. • If you wish to delete Information which has been set, either select [Information] in the

[Item] menu, or double click inside the frame showing the Information that you wish deleted. A dialogue box will then open. Select the [Delete Item] button in this box.

• If you wish to change Information which has been set, either select [Information] in the

[Item] menu, or double click inside the frame showing the Information that you wish to change. A dialogue box will then open. Reset the Information and then select the [OK] button in this box.


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5.4.3.4 Program 1, Program 2, Program 3... Various programs can be written in a report. • Program can be displayed now for every multi-view file. <Operation>

Select the [Program] command in the [Item] menu. A dialogue box will open for setting the program(s).

Select the [Options] button, select the item(s) and stage number(s) that you want to print in the report and then select the [OK] button.

After setting the program, select the [OK] button. A frame will be displayed showing the program.

CAUTION

Enter a "0" in the Step Number text box will cause all of the steps to be output.

• If you wish to return a changed program to its condition prior to the changes, select the [Reset] button.

• If you wish to copy the contents of a program, select the text that you wish to copy and

then select the [Copy] command in the [Edit] menu in the dialogue box. • If you wish to cut the contents of a program, select the text that you wish to cut, and then

select the [Cut] command in the [Edit] menu in the dialogue box. • If you wish to paste program contents which have been copied, select the text that you

wish to paste, and then select the [Paste] command in the [Edit] menu in the dialogue box.

• To undo something that you have copied, cut, pasted, select the [Undo] command in the

[Edit] menu in the dialogue box. • If you wish to delete a program which has been set, either select [Program] in the [Item]

menu, or double click inside the frame showing the program that you wish deleted. A dialogue box will then open. Select the [Delete Item] button in this box.

• If you wish to change a program which has been set, either select [Program] in the [Item]

menu, or double click inside the frame showing the program that you wish to change. A dialogue box will then open. Reset the program and then select the [OK] button in this box.


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5.4.3.5 Comment 1, Comment 2, Comment 3, Comment 4, Comment 5 Various comments can be written in a report. • The comment is numbered so that it can distinguish. Therefore, two or more comments can

be displayed now. <Operation>

Select the [Comment] command in the [Item] menu. A dialogue box will open for setting the comments.

A dialogue box will open for setting comments. Enter the comments and then select the [OK] button. A frame will be displayed showing the comment. • If you wish to return a changed comment to its condition prior to the changes, select the

[Reset] button. • If you wish to copy comments, select the text that you wish to copy and then select the

[Copy] command in the [Edit] menu in the dialogue box. • If you wish to cut comments, select the text that you wish to cut, and then select the [Cut]

command in the [Edit] menu in the dialogue box. • If you wish to paste comments which have been copied, select the text that you wish to

paste, and then select the [Paste] command in the [Edit] menu in the dialogue box. • To undo something that you have copied, cut, pasted, select the [Undo] command in the

[Edit] menu in the dialogue box. • If you wish to delete comments which have been set, either select [Comment] in the

[Item] menu, or double click inside the frame showing the comments that you wish deleted. A dialogue box will then open. Select the [Delete Item] button in this box.

• If you wish to change comments which have been set, either select [Comment] in the

[Item] menu, or double click inside the frame showing the comments that you wish to change. A dialogue box will then open. Reset the comments and then select the [OK] button in this box.


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5.4.4 [Option] menu

5.4.4.1 Landscape, Portrait The orientation of the paper in the [Report] window can be changed. However, a setup of the main part of a printer is not changed. <Operation>

From the [Option] menu, select [Portrait] to orient the paper vertically, or select [Landscape] to orient the paper horizontally. The area which shows the paper will be changed to the selected orientation.

5.4.4.2 Arrange Cursor This will display a help cursor for arranging items in a report. When moving the display position of comments or reports, etc., it is convenient to use a cross cursor. <Operation>

Select the [Arrange Cursor] command in the [Option] menu. • When the help cursor is selected, it will be displayed on the screen by clicking the

mouse.

This cursor can be eliminated by again selecting the [Arrange Cursor] command in the [Option] menu.

CAUTION

The position of arrange cursor cannot be specified in the domain which writes in graph and a comment.


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5.4.5 Operations on Print preview

5.4.5.1 Moving items Items displayed on the print preview, such as graph, title, information, programs, comments, may be moved around freely using the mouse. <Operation>

Move the mouse cursor onto the item you wish to move. The mouse cursor will become cross-shaped.

Move the item to the desired location by dragging the mouse. The frame lines will move with the cursor.

• If the arrange cursor is set beforehand, it can be aligned with other items very smoothly.

5.4.5.2 Sizing Graph A graph displayed on the print preview may be changed to the desired size. <Operation>

Move the mouse cursor onto the graph frame line displayed on the print preview. The mouse cursor will become a double-pointed arrow.

Drag the mouse to change the frame to the appropriate size. The graph is the only item displayed on the print preview which may be sized. The sizes of the items are determined automatically by the number of characters and font.


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5.5 ASCII Conversion Program Data files and analysis result files created by this program are saved to disk as binary files, but these data must be converted into the ASCII format in order to load the data into commercially available spreadsheet programs. In the <<ASCII Conversion Window>>, data files and analysis result files can be converted into ASCII formatted files. Data can be converted into ASCII in the following formats in the <<ASCII Conversion Window>>.

• Microsoft Excel, Lotus1-2-3 [.DIF] format • Microsoft Excel [.TXT] format • Microsoft Excel [.CSV] format • Lotus1-2-3 [.PRN] format • Lotus1-2-3 [.ASC] format

In addition, the following items in files created by this program can also be converted into ASCII.

• File information at the time of data acquisition • Temperature programs • Load programs (TMA only) • Analysis results (Analysis result files only) • Data

5.5.1 Starting the <<ASCII Conversion Window>> Select the [ASCII Conversion] item of the [Analysis] menu in the <<TA-60WS Acquisition: Status window>>. Or select the [ASCII Conversion] item of the [Application] menu in the <<TA60 window>>. The << ASCII Conversion window>> opens, and at the same time, a window is displayed for selecting a file to be loaded.

5.5.2 <<ASCII Conversion Window>> Configuration

④ ⑤

①

②

③


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① Convert Item check boxes These are check boxes for selecting the items to be converted to ASCII.

② [Parameters] button

This will open the <Data Window> for setting the converted data type, significant figures and smoothing interval, etc. when converting data values into ASCII.

③ Format

This displays the file extension of the format selected in the [Format] menu.

④ [Clipboard] button This converts the items selected in ① into ASCII and sends them to the clipboard.

⑤ [File] button

This converts the items selected in ① into ASCII.

5.5.3 <<ASCII Conversion Window>> Operation 1. Select the file to be loaded into the <<ASCII Conversion Window>> from the <Open File

Window>.

2. Place check marks by those items listed in the Convert Item check box list that you wish to be converted. When there is a check mark next to [Data], the <Data Window> will open when you select the [Parameters] button, where you can set the data interval, converted data type and significant figures, etc. (Refer to 5.5.5 <Data Window> Operation)

3. Set the converted file format for the [Format] menu. (Refer to 5.5.4.2 [Format] menu)

4. Select the conversion destination for the [Convert] menu. Execute the ASCII conversion.

a. Send converted data to the clipboard.

Either select [Clipboard] item in the [Convert] menu, or click on the [Clipboard] button. After ASCII conversion has been executed, the data will be sent to the clipboard.

b. Save converted data to a file

Either select [File] in the [Convert] menu, or click on the [File] button. A dialogue box will be displayed showing the file name. If necessary, change the file name and then select the [Save] button. If you select the [Cancel] button, the conversion will not be executed. After the ASCII conversion has been executed, the data will be saved to the file.


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5.5.4 <<ASCII Conversion window>> menu

5.5.4.1 [File] menu

1) Open Data

This command opens the <Open File window> for loading files into the <<ASCII Conversion Window>>. <Procedure>

Select [Open] from the [File] menu on the <<ASCII Conversion Window>>. The <Open File Window> will open. Change the folder if necessary, enter in the text box the filename that you want to load and then select the [Open] button.

CAUTION

It is possible to convert it only by one file.

[File list to which ASCII conversion can be done] • Data file (Ext. .D?0) • Analysis result file (Ext. .R00) • Stress Strain Analysis result file (Ext. .S00) • Specific Heat Analysis result file (Ext. .H00) • DSC Kinetic Analysis result file (Ext. .KD0) • TG Kinetic Analysis result file (Ext. .KT0)

[File list to which ASCII conversion cannot be done]

• Multi view file (Ext. .M00) • Stress Strain Multi view file (Ext. .Y00)

2) Exit This command closes the <<ASCII Conversion Window>>. <Procedure>

Select [Exit] from the [File] menu on the <<ASCII Conversion Window>>. The <<ASCII Conversion Window>> is closed.


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5.5.4.2 [Format] menu In [Format] menu, the converted format is set. <Procedure>

Select the conversion format with the [Format] menu.

• Excel［.DIF］ This converts the data into the (*.DIF) format which can be loaded by .Microsoft® Excel® and Lotus 1-2-3®.

• Excel［.TXT］

This converts the data into the (*.TXT) format which can be loaded by Microsoft® Excel®.

• Excel［.CSV］

This converts the data into the (*.CSV) format which can be loaded by Microsoft® Excel®.

• Lotus1-2-3［.PRN］

This converts the data into the (*.PRN) format which can be loaded by Lotus 1-2-3®.

• Lotus1-2-3［.ASC］ This converts the data into the (*.ASC) format which can be loaded by Lotus 1-2-3®.

• Other formats

This will convert the data into formats with optional file extensions and delimiters.

When you select [Format Another], the following window will be displayed.

Enter the delimiter and file extension. When you select the [OK] button, the delimiter and extension will be set.


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5.5.4.3 [Convert] Menu

1) Clipboard

The content of the file is converted into ASCII character string on the set condition, and it sends it to the clipboard. <Procedure>

Select [Clipboard] from the [Convert] menu on the <<ASCII Conversion Window>>. The content of the file is converted into ASCII character string on the set condition, and it sends it to the clipboard.

NOTE

The same operation can be executed by clicking on the [Clipboard] button in the <<ASCII Conversion Window>> screen.

2) File

The content of the file is converted into ASCII character string on the set condition, and it preserves it in the file. <Procedure>

Select [File] from the [Convert] menu on the <<ASCII Conversion Window>>. The <Save As window> will open. Change the folder if necessary, enter in the text box the filename that you want to save and then select the [Save] button.

The content of the file is converted into ASCII character string on the set condition, and it preserves it in the file.

NOTE

The same operation can be executed by clicking on the [File] button in the <<ASCII Conversion Window>> screen.


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5.5.5 <Data Window> Operation

① Data point

This displays the total number of data points which have been loaded.

② Start point text box This is a text box for setting the data conversion start point.

③ End point text box

This is a text box for setting the data conversion end point.

④ Smooth point text box This is a text box for setting the data conversion interval.

⑤ Data Type check boxes

Select the data types to be converted.

⑥ Significant Figure input text boxes These are text boxes for setting the significant figures to be used in conversion. 1 to 6 digits can be entered as the significant figure.

⑦ [OK] button

This will save the parameters which have been set and close the <Data Window>.

⑧ [Cancel] button This will stop the setting operation and close the <Data Window>.

<Data Window> operation

1. When setting the data conversion range, enter values into the Start point text box and End point text box. The data between the start point and end point will be converted.

2. When smoothing the data, enter the number of smoothing points in the Smooth point

text box. Data will then be converted extracting and converting only those data at the specified interval.

NOTE

About the sampling interval of measured data and the number of data points. Acquired data are saved to disk at a sampling interval which was set at the time of acquisition. For instance, if the sampling interval was set to one (1) second, when data acquisition was performed over a 10 minute period, 1×60×10=600 points of data would have been obtained.

②

③

①

⑤

④

⑥

⑦ ⑧


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6 DSC Kinetic Analysis Measurement Summary In order to conduct DSC Kinetic Analysis, it is necessary to use data which was generated for Kinetic Analysis using the Differential Scanning Calorimeter (DSC-60 or DSC-50).

6.1 Cautions in Measurement Since the DSC Kinetic Analysis program applies the Ozawa method, analysis requires that:

• There should be no localization of temperature within the sample. The temperature distribution must be uniform

• There should be no localization of density within the sample. There should only be diffusion.

It is necessary to take due notice of these considerations. In addition, other cautions associated with measurement are listed below. (1) Since the Ozawa method is based on analyzing multiple data files in which different heating rates

were used, it is necessary that each data file was measured using a different heating rate.

(2) It is necessary that the measurement conditions for each analysis are kept as uniform as possible. Ensure that sample morphology, sample weight and gas flow rate are the same,

(3) To keep the heat capacity constant, it is strongly recommended that the sample vessels in which

the samples are placed should all be the same.

(4) Be sure to enter the sample weight for all analyzed data. (Data in which the sample weight has not been entered, cannot be selected for analysis.)

When performing measurements for kinetic analysis, be sure to pay careful consideration to the cautions and restrictions detailed above.


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7 DSC Kinetic Analysis Summary The DSC Kinetic Analysis program is based on the Ozawa Method, and as such, the reaction rate parameters (kinetic energy, reaction rate, frequency factor) are calculated, and followed by the isothermal analysis (rate constant, reaction time). The algorithms used to conduct these operations are described below.

7.1 DSC Kinetic Analysis The general equation expressing reaction rate is as follows:

( )nxRTEA

dtdx

−⎟⎠⎞

⎜⎝⎛ ∆−⋅= 1exp （1）

dtdx

: reaction rate

A : frequency factor E∆ : kinetic energy

1− x : incomplete reaction percent R : gas constant n : reaction order T : temperature

Now, when the temperature rises at the heating rate ⎟⎠⎞

⎜⎝⎛=

dtdT φ , the approximation calculation, etc.,

based on the P function can be used to express equation (1) as:

.14567.0log10 constTR

E+⋅

∆−=φ （2）

Where:

T : peak temperature In other words, if peak temperature measurements are performed with different heating rates, and a plot is made of the inverse of the peak temperature as the horizontal axis and the common logarithm of the heating rate as the vertical axis (Arrhenius's plot), equation (2) will yield a straight line, and the slope of the line is expressed as:

RESlope ∆

= 4567.0 （3）

R and T are known, so kinetic energy ∆E can be calculated from equation (3). Since the kinetic energy determined here is an approximate value, the error can be reduced via correction. (Refer to ASTM E698-79) Using the determined kinetic energy, reaction factor A can be determined from the following equation.


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0exp2 ≅⎟⎠⎞

⎜⎝⎛ ∆−−

∆RTEA

RTEφ

（4）

Further, the reaction percent ( )mC−1 at the peak apex becomes:

( )

( )⎪⎪⎩

⎪⎪⎨

⎧

≠

==−

− 1

1

1

1

11

n

n

n

eC

n

m （5）

Therefore, if the area from the peak start point to the peak apex is taken as a ratio ( )mC with respect

to the entire peak area, reaction order n can be deduced.


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7.2 Isothermal Analysis This refers to the determination of reaction percent and time in the case of heating being performed at a constant temperature. However, since it is necessary to use parameters determined via kinetic analysis (kinetic energy ∆E , reaction order n , frequency factor A ), kinetic analysis must be conducted prior to isothermal analysis. Rate constant k at fixed temperature T is expressed as:

⎟⎠⎞

⎜⎝⎛ ∆−=RTEAk exp （1）

Where:

A : frequency factor ∆E : kinetic energy R : gas constant T : absolute temperature

The equation can be solved using the parameters determined from the DSC Kinetic Analysis (kinetic energy ∆E , reaction order n , frequency factor A). Further, k can be used to calculate the relationship between reaction percent C at a fixed temperature and time t .

( )nCkdtdC

−= 1 （2）

If this is integrated with respect to time, reaction time t becomes:

( ) ( ){ }11 1

1 1 −−−

= −nCnk

t ( )1≠n

( )Ck

t −= 1ln1 ( )1=n （3）

thus enabling calculation of time t at various reaction percentages C .


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8 DSC Kinetic Analysis Configuration

8.1 Analysis configuration file In kinetic analysis, the analysis configuration file is created in order to store the analysis configuration settings. Analysis environment parameters which are often used may be changed in the analysis windows (and Options windows) of Kinetic Analysis and Isothermal Analysis - Input Temperature, and in the <Display Parameters window> under the [Display] menu of the analysis results windows. This chapter describes the method of changing the environment in ways that cannot be changed from within the analysis windows and Options windows, or from the <Display Parameters window>. Making these types of configuration modifications entails editing of the analysis configuration file.

8.2 Items which can changed from analysis configuration file

The configuration items listed below can be changed only by editing the analysis configuration file. • Number of data partitions used in Isothermal Analysis • Number of decimal places used in analysis results • Numerical value of the exponent when exponent is displayed in analysis results • Character display color in analysis results • Display color of auxiliary marks and lines

8.3 Analysis configuration file path An analysis environmental file is made by the next folder of the folder in which the DSC Kinetic Analysis (Ozawa method) program is installed.

CONFIG The DSC Kinetic Analysis configuration file name is DSCOZAWA.INI. This is a text file which can be edited using a text editor, such as <Notepad>, in the <Windows Accessories group>.


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8.4 Composition of the analysis configuration file The following two lines of text appear at the beginning of the file. This information is needed to identify the file, so do not edit them.

Calculation setup file Ver 1.00 (C) Copyright 1993 Shimadzu Corporation

Any text appearing in [ ] can be recognized as an analysis item. Every line following the analysis item in [ ], until an empty line is reached, indicates the associated analysis configuration. The following analysis items are contained in the file.

[Common] Common analysis configuration [Kinetic Analysis for DSC] Kinetic Analysis [Isothermal Analysis] Isothermal Analysis

The Analysis configuration setting formats are as follows.

Item=numerical value or character string

There should be no space between Item, numerical value, character string or = sign. Depending on the Item, the type of numerical value or character string varies. • Flag for performing/not performing analysis (character string)

YES : Analysis to be performed NO : Analysis not to be performed

• Number of decimal places in analysis result (numerical value)

ex) Setting "3" displays format 99.999 • Numerical value of the exponent when exponent is displayed in analysis results (numerical value)

When 0 is set, the exponent is not displayed. Analysis result is displayed in the following format when a numerical value is set.

ex) 99 x 10 (numerical value set)

• Flag indicating whether or not units will be displayed for rate constant, reduced time and reaction time in the results of isothermal analysis (character string)

YES : Unit is displayed at right of each result value NO : Unit is displayed at right of each comment (If there is no comment, nothing is displayed)

• Color of display of calculation result characters, auxiliary marks (character string)

BLACK RED BLUE GREEN YELLOW CYAN MAGENTA WHITE

• Type of lines used for Ozawa Plot and Isothermal Analysis data (Line Style)


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0 Normal line 1 Broken line 2 Dotted line 3 Broken line with one-dot intervals 4 Broken line with two-dot intervals

• Type of marks used for Ozawa Plot and Isothermal Analysis data (Mark Style)

0 none 1 Square 2 Triangle (pointed up) 3 Triangle (pointed down) 4 Circle 5 × (cross)

• Filling of marks used for Ozawa Plot and Isothermal Analysis data (Paint-Out)

0 Not filled 1 Filled

• The Isothermal Analysis data display parameters are formatted using the following display parameters. Set these referring to the items described above.

Display [data #]: Line style, line width, line color, mark style, mark color, mark paint-out


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8.5 Analysis configuration file contents summary

Item (with default value) Description Format (Range)

[Common] Common

TempDecimal=2 Number of decimal places used when displaying temperatures

0～12

TempUnit=｡C Unit used for temperature display °C or K

AnnotateColor=BLACK Color used for annotation display Color (characters)

AddLineColor=CYAN Color used for auxiliary lines Color (characters)

AddMarkColor=CYAN Color used for auxiliary marks Color (characters)DivisionPoint=50 Number of data partitions used in Isothermal

Analysis 10～100

[Kinetic Analysis for DSC] Kinetic Analysis

GroupFlag=YES Analysis results group display YES,NO

DisplayResultGraph=YES Ozawa Plot display YES,NO Comment(ReactionOrder)=Reaction order Reaction order analysis result comment Character string

ReactionOrderFlag=YES Whether or not to display Reaction order analysis result

YES, NO

ReactionOrderDec=1 Decimal places used in display of Reaction order analysis result

0 ～ 12

ReactionOrderColor=BLACK Reaction order analysis result display color Color (characters)

Comment(FrequencyFactor)=Frequency factor Frequency factor analysis result comment Character string

FrequencyFactorFlag=YES Whether or not to display Frequency factor analysis result

YES, NO

FrequencyFactorDec=2 Decimal places used in display of Frequency factor analysis result

0 ～ 12

FrequencyFactorColor=BLACK Frequency factor analysis result display color Color (Characters)

Comment(ActivationEnergy)=Kinetic Energy Kinetic Energy analysis result comment Character String

ActivationEnergyFlag(KJ/mol)=YES Whether or not to display Kinetic Energy (kJ/mol)

YES, NO

ActivationEnergyFlag(Kcal/mol)=YES Whether or not to display Kinetic Energy (kcal/mol)

YES, NO

ActivationEnergyDec(KJ/mol)=2 Decimal places used in display of Kinetic Energy (kJ/mol)

0 ～ 12

ActivationEnergyDec(Kcal/mol)=2 Decimal places used in display of Kinetic Energy (kcal/mol)

0 ～ 12

ActivationEnergyColor(KJ/mol)=BLACK Color used for display of Kinetic Energy (kJ/mol) Color (Characters)ActivationEnergyColor(Kcal/mol)=BLACK Color used for display of Kinetic Energy

(kcal/mol) Color (Characters)

OzawaPlotLineStyle=0 Ozawa Plot line style 0 ～ 4

OzawaPlotLineWidth=1 Ozawa Plot line width 1 ～ 9

OzawaPlotLineColor=BLUE Ozawa Plot line color Color (Characters)


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OzawaPlotMarkStyle=1 Ozawa Plot mark style 0 ～ 5

OzawaPlotMarkColor=BLUE Ozawa Plot mark color Color (Characters)

OzawaPlotMarkPaintOut=1 Ozawa Plot mark paint out (filling) 0, 1 TempDisplayFlag=NO Whether or not to display temperatures for

analysis start and end points and peak apex YES, NO

TempDisplayDec=2 Decimal places to be used in display of the various temperature values

0 ～ 12

TempColorDependData=YES Whether or not temperature display colors should match data color

YES, NO

TemperatureColor:=BLUE,GREEN,CYAN,… Designates color to be used for each temperature display when temperature display colors need not match data color (12 settings)

Color (characters)

[Isothermal Analysis] Isothermal Analysis

GroupFlag=YES Display of analysis results group YES, NO Comment(ActivationEnergy)=Kinetic Energy Kinetic Energy analysis results comment Character string

ActivationEnergyFlag(KJ/mol)=YES Whether or not to display Kinetic Energy (kJ/mol)

YES, NO

ActivationEnergyFlag(Kcal/mol)=YES Whether or not to display Kinetic Energy (kcal/mol)

YES, NO

ActivationEnergyDec(KJ/mol)=2 Decimal places for displayed Kinetic Energy (kJ/mol)

0 ～ 12

ActivationEnergyDec(Kcal/mol)=2 Decimal places for displayed Kinetic Energy (kcal/mol)

0 ～ 12

ActivationEnergyColor(KJ/mol)=BLACK Display color of Kinetic Energy (kJ/mol) Color (Characters)ActivationEnergyColor(Kcal/mol)=BLACK Display color of Kinetic Energy (kcal/mol) Color (Characters)

Comment(ReactionOrder)=Reaction order Reaction order analysis result comment Character string

ReactionOrderFlag=YES Whether or not to display Reaction order analysis result

YES, NO

ReactionOrderDec=2 Decimal places used in display of Reaction order analysis result

0 ～ 12

ReactionOrderColor=BLACK Display color of Reaction order analysis result Color (characters)Comment(FrequencyFactor)=Frequency factor Frequency factor analysis result comment Character string

FrequencyFactorFlag=YES Whether or not to display Frequency factor analysis result

YES, NO

FrequencyFactorDec=2 Decimal places used in display of Frequency factor analysis result

0 ～ 12

FrequencyFactorExp=30 Number of exponent digits used in display of Frequency factor analysis result

-30 ～ 30


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FrequencyFactorColor=BLACK Display color of Frequency factor analysis result Color (characters)

Comment(ReducedTime)=Redurced time Reduced time analysis result comment Character string

ReducedTimeFlag=YES Whether or not to display Reduced time analysis result

YES, NO

ReducedTimeDec=2 Decimal places used in display of Reduced time analysis result

0 ～ 12

ReducedTimeExp=30 Number of exponent digits used in display of Reduced time analysis result

-30 ～ 30

ReducedTimeColor=BLACK Display color of Reduced time analysis result Color (Characters)

ReducedTimeUnitDisplay=NO Whether or not unit is used in display of Reduced time analysis result

YES, NO

Comment(CalculateTemperature)=Analysis Temperature

Analysis temperature result comment Character string

CalculateTemperatureFlag=YES Whether or not to display Analysis temperature result

YES, NO

CalculateTemperatureDec=2 Decimal places used in display of Analysis temperature result

0 ～ 12

CalculateTemperatureColor=BLACK Display color of Analysis temperature result Color (characters)

Comment(RateConstant)=Rate constant Rate constant analysis result comment Character string RateConstantFlag=YES Whether or not to display Rate constant analysis

result YES, NO

RateConstantDec=2 Decimal places used in display of Rate constant analysis result

0 ～ 12

RateConstantExp=30 Number of exponent digits used in display of Rate constant analysis result

-30 ～30

RateConstantColor=BLACK Display color of Rate constant analysis result Color (characters)

RateConstantUnitDisplay=NO Whether or not unit is used with displayed Rate constant analysis result

YES, NO

Comment(ReactionTime)=Reaction time Reaction time analysis result comment Character string

ReactionTimeFlag=YES Whether or not to display Reaction time analysis result

YES, NO

ReactionTimeDec=2 Decimal places used in display of Reaction time analysis result

0 ～ 12

ReactionTimeExp=30 Number of exponent digits used in display of Reaction time analysis result

-30 ～ 30

ReactionTimeColor=BLACK Display color of Reaction time analysis result Color (characters)

ReactionTimeUnitDisplay=NO Whether or not unit is used with displayed Reaction time analysis result

YES, NO

TempTable(K)=0.00,0.00,0.00,0.00,0.00,0.00 Isothermal Analysis temperature [K] (6 values) Numerical value

TempTable(C)=0.00,0.00,0.00,0.00,0.00,0.00 Isothermal Analysis temperature [°C] (6 values) Numerical value


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Display[1]:0,1,BLUE,0,BLUE,1 Isothermal Analysis display parameters - 1st Value, color (characters)

Display[2]:0,1,GREEN,0,GREEN,1 Isothermal Analysis display parameters - 2nd Value, color (characters)

Display[3]:0,1,CYAN,0,CYAN,1 Isothermal Analysis display parameters - 3rd Value, color (characters)

Display[4]:0,1,RED,0,RED,1 Isothermal Analysis display parameters - 4th Value, color (characters)

Display[5]:0,1,MAGENTA,0,MAGENTA,1 Isothermal Analysis display parameters - 5th Value, color (characters)

Display[6]:0,1,YELLOW,0,YELLOW,1 Isothermal Analysis display parameters - 6th Value, color (characters)

Download - Manual DSC Kinetic Analysis

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