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DSC Kinetic Analysis

DSC Kinetic Analysis

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0% found this document useful (0 votes)
54 views83 pages

DSC Kinetic Analysis

DSC Kinetic Analysis

Uploaded by

Hari Mudzah
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
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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. E)SHIMADZU CORPORATION KYOTO JAPAN ANALYTICAL & MEASURING INSTRUMENTS DIVISION 346-69840C Copyright® Shimadzu Corporation 2002-2010. All rights reserved, ineluding those to reproduce this publication or parts thereof in any from without emission 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 petiod of aveilability 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-6OWS, 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. Donat disassemble or modify the unit without our approval 5. Forrepair ofthe product inside, centact 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, ifnot 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 & 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 basie summary of the DS 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 ary 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 § 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, Analysis Measurement Sum Contents 1 Summary i 1.1 The DSC Kinetic Analysis Program... 1.2 Data to be used for DSC Kinetic Analysis. 13 The DSC Kinetic Analysis Result File. 2 Parts List 2.1 DSC Kinetic Analysis Program Parts Summary... 3 Installation .. 3.1 Before installation .. 3.2 Installation. 2.2.1 'TAGOWS Software Setup . 322 Registration of DSC Kinetie Analysis Program.. 3.2.3 DSC Kinetic Analysis Program Setup. 4 DSC Kinetic Analysis Program operation procedures 4.1 Flow of DSC Kinetic Analysis Program (Ozawa method)...... 4.1.1 Open of TA-GOWS format (Extension: tad) data 4.2 Operation procedures Starting of <>.. Selecting data for DSC Kinetic Analysis. Setting the display range (Changing theldsplay postticn tee DSC Kinetic Analysis. Isothermal Analysis, Report output... : i Storing results of Kinetic Analysis. u Closing the <> uu 4.3 DSC Kinetic Analysis operation procedures 1 Kinetic Analysis... 4.3.2 Kinetie Analysis - By data 4.3.3 Kinetic Analysis - Select peak 4.34 — Kinetic Analysis Options .. 4.4 Isothermal Analysis operation procedures... 4.4.1 Isothermal Analysis. : 4.4.2 Isothermal Analysis options 4.5 DSC Kinetic Analysis Configuration. 4.5.1 Options... 5 DSC Kinetic ‘Analysis Program Functions us 5.1 <> menu item: 5.1 [File] menu 5.12 [Display] menu... 5.1.3 [Scale] menu 5.14 — [Analysis menu.. 5.1.5 [Display Position] 5.16 — [Report] menu. Contents, 5.1.7 [Window] menu. 5.2 menu items. 2.1 [Display] menu 5.2.2 [Report] menu. sessed 5.3 menu items ....ssssssssnensesessses 5.3.1 [Display] menu 5.8.2 [Scale] men 5.3.3 [Report] menu. 5.4 menu items 54.1 [Pile] menu. 5.4.2 [Pont] menu 5.4.3 [Item] menu 5.4.4 — [Option] menu... 5.4.5 Operations on Print pre 5.5 ASCII Conversion Program. 5.5.1 Starting the <> 5.5.2 <> Configuration, <> Operation..... <> menu Operation . 6 DSC Kinetic Analysis Measurement Summary .. 6.1 Cautions in Measurement... 7 DSC Kinetic Analysis Summary... 7.1 DSC Kinetic Analysis... 7.2 Isothermal Analysi 8 DSC Kinetic Analysis Configuration 81 Analysis configuration file. 8.2 Items which can changed from analysis configuration file... 8.3 Analysis configuration file patl evesaese 5 . 66 sesso 66 68 8.4 Composition of the analysis configuration fil 85 Analysis configuration file contents summary DSC Kinetic Analysis Program (Ozawa method) for TA-6OWS, 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 ean 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 [KJmol],[Keal/mol] + Reaction order © Frequency factor min!) © Analysis temperature [K],(°C] Hsothermal Analysis] «Kinetic Energy {[Ki/mot} {Keal/mot] * Reaction order Frequency factor (min!) + Analysis temperature [K},[*C] + Rate constant [min"!] * 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. » 2) 3) 4) The data files for Kinet 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, Analysis processing are to have been measured using the DSC-60 or After conducting a DSC Kinetie Analysis, the analysis results and plot information is stored in @ Kinetic Analysis result file (file extension: .KDO). Old data file when Shimadzu Thermal Analyzer System TA-SOWSI is used. (with file extensions: .D20,.R2?) (Old data file when Shimadzu Thermal Analyzer System TA-SOl is used. (files in which file name begins with @, and having the file extension ,000) DSC Kinetic Analysis Program (Ozawa method) for TA-GOWS, 1.3 The DSC Kinetic Analysis Result File The Kinetic Analysis result files generated by this program have the file extension -KDO, 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 <> and re-analyzed. In addition, this file can be converted to ASCII format in the <> for further data processing in Microsoft” Exel”, Lotus!-2-3" of other third-party software. Also note that Kinetic Analysis result files cannot be opened in programs other than the DSC Kinetic Analysis program. 2 Parts List 2.1 DSC Kinetic Analysis Program Parts Summary DSC Kinetic Anal Program (Ozawa method) for TA-60WS ‘The DSC Kinetic Analysis Program consists of the items listed below. Before installing the software, ‘verify that all ofthe disks are included in your shipment. 1, DSC Kinetic Analysis Program (Ozawa method) P/N 347-65168-92 tem No,| Part Ne. Description Qt 1__|23-11539-91_| DSC Kinetic Analysis program for TA-60WS (CD-ROM) 1 2 | 3a6-67586.91_| TA-GOWS Program (CD-ROM ) 1 3 |346-69840 | DSC Kinetic Analysis program for TA-60WS Instruction 1 Manual (this document) Prograi (Ozawa method) for TA-6OWS 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 Windows" 7 Professional 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. Program (Ozawa method) for TA-60WS 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 ION ‘When the version number written on your CD-ROM containing a TA-6OWS 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 sereen is displayed. New installation sereen ‘Maintenance screen © When you newly install it. Or, when the @ When the software Ver.1.S1 or later is software Ver. 1.50 or earlier is installed, installed. When the displayed sercen is a new installation sereen For the subsequent operation, follow the instructions in the window. When the displayed sereen is a maintenance screen Select the [Repair] item with the mouse. And select the [Next] button, etic Anal Program (Ozawa yethod) for TA-6OWS 3.2.2. Registration of DSC etic Analysis Program ‘The majority of the DSC Kinetic Analysis program is in CD-ROM of TA-6OWS, However, it is necessary to register first of all forthe installation by the following setup work 1, When you insert CD-ROM in the PC supporting "autorun" funetion, the setup program will automatically star New installation sereen 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. DSC Kinetic Analysis Program (Ozawa method) for TA-60WS 3.2.3. DSC Kinetic Analysis Program Setup ‘When rexistration is completed, itis possible to set it up. [CAUTION ‘When the version number written on your CD-ROM containing a TA-6OWS program is higher than the one written on the CD-ROM containing the TA-GOWS program accompanying this program, you ddo not need to install the latter. Procced to the next paragraph, CAUTION First ofall, 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 ete., and it stats. 2: AKDSC\Disk\Setup.exe (? is drive name) ‘The setup program starts. And, either ofthe following sereen is displayed. New installation screen Maintenance sereen © When you newly instal it © When it has already been installed When the displayed screen is a new installation sereen For the subsequent operation, follow the instructions in the window. When the displayed sereen is a maintenance screen Select the {Repar] item withthe mouse. And select the [Next] button. DSC ki Analysis Program (Ozawa method) for TA-60WS 4 DSC Kinetic Analysis Program operation procedures 4.1 Flow_of DSC Kinetic Analy method) Program (Ozawa Operation Procedure Reference Section Starting of <> 42 4 Configuration of <> 4s J Select data for DSC Kinetie Analysis 422 4 Set display range 423 J Change display position 424 4 DSC Kinetic Analysis, 43 4 Isothermal Analysis 44 J Report output 5.1.6 J Save Kinetic Analysis results S112 i 5.1.13 Close < 429 DSC Kinetic Analysis Program (Ozawa method) for TA-60WS 4.1.1 | Open of TA-60WS format (Extension: .tad) data ‘The following procedure is used to open the TA-6OWS format data files (extension ,tad) acquired on the Shimadzu Differential Scanning Calorimeter (DSC-60 and DSC-50). ‘CAUTION ‘The analysis result file (extension .KDO) is not available in this procedure, You can open this file from the [Open] item of the [File] menu of the <>, For opening the <> 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 <>, Select the [Execution of program] item in the [DSC Kinetic Analysis] item in the [Application] pull-down menu on the <>. 1. Select the [Select data file] item in the [DSC Kinetic Analysis] item in the [Analysis] pull- down menu on the <>. Or select the [Select data file] item in the [DSC Kinetic Analysis] item in the [Application] pull-down menu on the <>. ‘The is displayed, Eames i © S : @ cS ¢ 2. Select the [Select File] button. The is displayed. Select the data file name and select the [Open] button, DSC Kinetic Analysis Program (Ozawa method) for TA-GOWS, Alll data need to be acquired using the same measurement parameters except the heating rate, and hhave to include the sample weight. ‘You can select the multiple files how to select the file while holding down the [Shift] key or [Ctrl] key in the . 3. The selected file name is displayed in the , lepr4Cel4 DSO conatCekrZ 00 Csteracnvosooeanatcoh N50 4. Push the [Analyze] button, ‘The <> is displayed with the all files on the [Files] list box. Select dhe [Enid] bution, The “Open File for Kinetic Analysis DSC window” is closed. [Select File] button Display the for selecting the data file @® [Remove] button Remove a selected file shown by the highlight from the [Files] list box. @ [AM Remove] button Remove all ofthe files in the [Files] list box. e ® [Help} button Display help messages related to this window © [Files] list box The selected fle names are displayed. © [Analyze] button Open the <>, the all selected files in the [Files] list box are read. ® [Exit] button Close the . ~10- Ds inetic Anal Program (Ozawa method) for TA-60WS 4.2 Operation procedures 4.2.1 Starting of <> A DSC Kinetic Analysis Program (Ozawa method) is performed from the Explorer of Microsoft” Windows” et. ‘The <> opens, and at the same time, window is displayed for selecting a file o be loaded. 4.2.2 Selecting data for DSC Kinetic Analysis In the , 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 (o 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 Kinetie Analysis, the analysis results and plot information is stored in a Kinetic Analysis result file ile extension: -KDO). 3) Old data file when Shimadzu Thermal Analyzer System TA-SOWSI is used. (with file extensions: .D20, .R??) 4) Old data file when Shimadzu Thermal Analyzer System TA-SO1 is used. (files in which file name begins with @, and having the file extension ,000) 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 ae 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. Seleet 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 $.1.2 2) Range Program (Ozawa yethod) for TA-6OWS 2) Setting display range for each set of data independently Select [Range - By data] from the [Display] menu, The , 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. It 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. Selting 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 . Refer to 5.1.2.1 Display Parameters. 3) Pos Select [Manual Slide] from the (Display Position] menu, The 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, ‘Afer positioning the data, select the [OK] button, ‘The will close, and the data will be redrawn on the sereen, repositioned to where the square mark was set ioning each set of data independently for display Program (Ozawa method) for TA-6OWS 4.2.5 After setting the analysis range, the kinetic analysis is conducted on the basis of that range, and the results are displayed on the sereen, The methods available for performing the kinetic analysis using this scenario are as follows. © Performing kinetic analysis by selecting the analy' [Kinetic Analysis} in the [Analysis] menu © Performing kinet [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 range from the overlaid data, analysis by selecting the analysis range for each set of data independently Alter 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. we analysis results based on the set analysis range are displayed in the < is opened, displaying the relationship between the log of the heating rates and the inverse of the peak temperatures NOTE For details on cach 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 , For details on cach of the analysis procedures, refer (0 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 , you may view an image ‘of the report prior to the actual printout For details on setting up a report, refer to $.1.6 [Report] menu. 1B Anal} Program (Ozawa yethod) for TA-6OWS 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 .KDO. ‘* 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 > 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 Program (Ozawa method) for TA-60WS 4.3 DSC Kinetic Analysis operation procedures ‘The following items may be analyzed in the kinetic analysis program © Kinetic energy (kd/mol, keal/mol) * Reaction order Frequency factor (min-1) © Ozawa plot (LOG A- 1/T) * Analysis start point, end point, peak temperature (K or °C) LUTION Ifthe 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, Bofore 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. 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 to4.34 Kinetic Analysis Options 3. Click om the sereen 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), DSC Kinetic Analysis Program (Ozawa method) for TA-GOWS, 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, ete.) is displayed at the upper right portion of the screen. If display of the Ozawa Plot was specified in the , 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 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 Ifthere are 2 or more kinetic analyses, the most recent kinetic analysis result will be displayed in the , ‘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, ~16- DSC Kinetic Analysis Program (Ozawa method) for TA-60WS 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 , for the analysis range, will be displayed with 2 vertical lines at each side of the screen. In the disappears and all of the DSC data are then displayed together in overlay fashion in the <>. In addition, the analysis results (kinetic energy, ete.) are displayed at the "upper right portion of the screen. If display of the Ozawa Plot was specified in the , the 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 If Set Group Position was selected as one of the kinetic analysis options, the 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, ae DSC Kinetic Analysis Program (Ozawa method) for TA-GOWS, ae Pere 7. The 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 center a comment as necessary. Refer to 4.3.4 Kinetic Analysis Options. IFthere are 2 or more kinetic analyses, the most recent kinetic analysis result will be displayed in the . ~18— DSC Kinetic Analysis Program (Ozawa method) for TA-60WS 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, ete. 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. Inthe , either the mouse or keyboard is used to sct 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 direetly 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 atthe locations set fr the previous data NOTE ‘The peak point-indicating cursor automatically searches the peak point for that sot of data, and is displayed at that position [Exiq bution: Cancels seting of analysis range and analysis. [Back] button Returns to the analysis range setting sereen 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 al the data. 5. Affer all the ranges and peak points are set, the disappears and all of the DSC data are then displayed together in overlay fashion in the <>, The analysis results (kinetic energy, ete.) are displayed at the upper right portion of the screen, ne DSC Kinetic Analysis Program (Ozawa method) for TA-GOWS, If display of the Ozawa Plot was specified in the , the is opened at the same time, displaying the log of the heating rates and the inverse ofthe peak temperatures used to determine the kinetic energy, 6. If Set Group Position was selected as one of the kinetic analysis options, the 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 will then open. [Next Analysis]... This resets the analysis range and executes analysis, [exit] con This exits the analysis [Options] __... This is used for setting the various analysis items and units. You may also enter a comment as necessary, Refer to 4.3.4 Kinetic Analysis Options. Irthore are 2 or more kinetic analyses, the most recent kinetic analysis result will be displayed in the . —2- DSC Kinetic Analysis Program (Ozawa method) for TA-60WS 4.3.4 Kinetic Analysis Options Selecting the [Options] button in the or will open the 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 ata specific location on the sereen, 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 settings are applied to all the Kinetic Analysis modes in common, The set items are retained, so itis not necessary to set them each time. ae DSC Kinetic Analysis Program (Ozawa method) for TA-GOWS, 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, keal/mol) : Average of kinetic energies obtained from kine 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-I) Rate constant determined by Atthenius 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 with its [Analyze] button will be displayed. Tep- (Cf Tt _ x.00] 2] aim =| ton. aD 5]. ot a.m ‘CAUTION If Isothermal analysis is conducted prior to selecting this, and the 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. Refer to 4.3.2 Isothermal Analysis options. 3. Next, enter the temperatures to be used in Isothermal Analysis (maximum 6 temperatures). The emperature values will be sorted and recorded in sequence from lower to higher temperature. 2 DSC Kinetic Analysis Program (Ozawa method) for TA-6OWS, ‘© 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 Seleet 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 . Im addition, the designated analysis items will also be displayed with the Isothermal Analysis results If Group Mode was selected as one of the Thermal Analysis options, the will be opened. [An analysis result positioning box is displayed at the site where the analysis results will be displayed, Click the mouse atthe site where you wish fo 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 Ifa wide temperature range was used, the data may be overlapped in the display ae DSC Kinetic Analysis Program (Ozawa method) for TA-GOWS, 4.4.2 Isothermal Analysis options When the [Options] button is selected in the , the is opened. The ‘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 resulta a desired location, select the Group Mode checkbox kinetic Eneray fReaction order frequency factor ffedicodime fans fonoorshr> te constant sesmfite constant © tesco te Moe Clicking on a unit to be used for the Kinetic Energy or on one ofthe other items to be used, will place ‘an % mark in the checkbox preceding the item selected. The items selected will be displayed in the -lsothermal Analysis window> ‘CAUTION Ifthe 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 itis not necessary to set them each time. —4— DSC Kinetic Anal Program (Ozawa method) for TA-6OWS 4.5 DSC Kinetic Analysis Configuration This is for setting the default environment to be valid when the DSC Kinetic Analy init is program is first ized. The configuration settings made here are valid only in the <> 4.5.1 Options |. Select [Options] from the [File] menu. 2. The window for setting the environment of the <> 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 he 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 ‘The range selection will be performed on the overlaid DSC data, it 3. Select the [OK] button. ‘The configuration settings will then become valid. DSC Kinetic Analysis Program (Ozawa method) for TA-GOWS, 5 DSC Kinetic Analysis Program Functions 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 .D70... vary according to the type of correction), or previously result files (file extension .R2?). However, when loading analysis result files for analysis, the analysis results in those files cannot be displayed. (Only the data in analyzed analys the analysis results file can be used.) 2) Affer conducting DSC Kinetic Analysis, the analysis result and plot information are stored in a Kinetic Analysis result file (file extension: .KD0), 5.1 < In the , the data files in the folder specified as the Load Data Folder using the DSC Kinetic Analysis Defaults are displayed. RY At RE, a me Jame as 26 DSC Kinetic Analysis Program (Ozawa method) for TA-60WS required, a folder name will be changed and a file will be chosen. ‘The file ofthe folder set up as the [option] of DSC Kinetic Analysis is displayed on a , Item ® Folder Displays the folder in which the file is stored. 8 Folder list box ‘This displays the current folder (drive). e File name text box ‘This displays the file name of the file selected in the File list box. ‘To ditectly specify the name of the file o be loaded, enter the file name here, File list box. ‘This isthe 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, e Selected file list box ‘This displays the files which have been selected in the File list box: e e [Select] button ‘This selects the file. The file you selected will be displayed in the Selected file list box, Double clicking on a file im the File list box performs the same function as this button, ® [Remove) button ‘This removes a selected file from the Selected list box. © (Open) buton This loads a selected file in the Selected file list box, and closes the . ® [Cancel] button ‘This cancels loading of files, and closes the 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 ae DSC Kinetic Analysis Program (Ozawa method) for TA-GOWS, 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, .R22, maximum 12 files), having the same measurement parameters with 4ifferent heating rates only may be sclected. 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 he displayed in the lower level list box. In the same way, select three or more files (maximum 12 files) of the same sample. Ifa desired file is notin the currently displayed folder, change folders in order to select that file. 2. Affer selecting all of the data files to be analyzed, select the [Open] button, 3. Allof the selected DSC data will be displayed on the sereen, ‘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. {fan analysis result file (82?) 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. Inthe upper level list box, highlight the kinetic analysis result file (fie extension KDO), and click the [Select] button or, double click on the file name with the mouse, The selected fle ‘name will be displayed inthe lower level ist box. 2. Select the [Open] button. 3. The kinetic analysis result file will be displayed on the sereen, ‘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 It 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. — 28 — DSC Kinetic Analysis Program (Ozawa method) for TA-6OWS, 5.1.1.2 Save This is selected to store the results ofa 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 .KDO. When creating multiple files from the same data, change the base file name. Ifa file with the same name exists on the disk, @ ‘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 (See. 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. 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. a hi a ————"wsaewy SR POF ‘The kinetic analysis result file will be saved using the newly entered file name using the KDO 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 opens. ‘© Mode which determines whether or not selection of the analysis range (display) is, performed when the data is loaded. Refer to 4.8 DSC Kinetic Analysis Configuration, 5.1.1.5 Exi This is used to close the SC Kinetic Analysis Program (Ozawa method) window>>. Select [Exit] from the [File] menu, DSC Kinetic Analysis Program (Ozawa method) for TA-60WS- 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. Select [Display Parameters] from the [Display] menu. The will open iltnbhonmeononontenenece nt ‘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 fon the row you wish to change. The will open. ‘After making the appropriate settings, select the [OK] button. The will return, After the settings have been made for all of the data, select the [OK] button ‘The sereen will be redrawn based on the new Display Parameters setings. ‘CAUTION If the [Of] 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. —30- DSC Kinetic Analysis Program (Ozawa method) for TA-6OWS, 5.1.2.2 Range ‘This is used to set the display range when itis 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 ll be deleted. Select [Range] from the [Display] menu. The will be displayed at the top of the window. Clicking the mouse while the cursor is positioned over the graph will eause 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 sereen, 5.1.2.3 Range - By data In kinetic analysis, since at least 3 sets of data are overlaid atthe 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, liminating all but the portions that you wish to analyze. Select [Range - By data] from the [Display] menu, The data file first selected will be isplayed in the window, with the Select [Range Cancel] from the [Display] menu. §.1.2.5 Cross Cursor ‘This is used to toggle the on/off display ofa cross-shaped cursor, which allows you to read the values of the cursor position at the vertical and horizontal axes when they are displayed, Select [Cross Cursor] from the [Display] menu. If the axis cursor is displayed, a check mark is placed in font ofthis item, Selecting ths item ausin will remove the axis cross cursor oe DSC Kinetic Analysis Program (Ozawa method) for TA-60WS 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 keybourd Select [Key Input] from the [Scale] menu. The will appear, allowing you to change the scale. (=P CHS se eetehe isa eon] Ke {oscinvingl 3ff-Us0n0 Coys cane 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 Itisalso 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, Select [Zoom] from the [Scale] menu. The will appear at the top of the Eset fcc (iat ie at | Press the left mouse button at one comer of the area of interest to be zoomed, and drag the Il be displayed con 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. mouse to the opposite corner of the area of interest. (A rectangular frame 5.1.3.3 Undo Seale ‘This is used to restore the current scale to the previous scale. Select [Undo Seale] from the [Scale] menu. Selecting [Undo Scale] ag: scale back to the previous scale setting, will toggle the 5.1.3.4 Default Scale ‘This restores the scale to the original scale ‘The original scale refers tothe entire range of the DSC data which was loaded from the file Select [Default Scale] from the [Scale] menu, -2- Ds 5.1.4 [Analysis] menu 5.1.4.1 Annotation This is used to position annotations as desired on the DSC Kinetic Analysis graph. Sclect [Annotation] from the [Analysis] menu, The 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 geaph. (Up to 32 chatacters 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 Select [Move] from the [Analysis] menu. The will open, To move the result values or annotations, move the cursor fo that object so that the cursor becomes eross-shaped Pressing down the mouse button will cause the frame around that object to be displayed. Drag the object to the desired location, and refease 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 raph, Select [Delete] from the [Analysis] menu, The 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, oe DSC Kinetic Analysis Program (Ozawa method) for TA-GOWS, 5. 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. Select [Reset Group] from the [Analysis] menu, The will open 11: Kinetic Analysis HefieReset of at {: ‘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 tha ial the results are deleted, the Select [Delete Group] from the [Analysis] menu, The will open. Sf 1: Kinetic Analls | ieee Bio} ‘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 Itthere are 2 or more kinetic analyses, the result of the most recent kinetic analysis is displayed in the . Each time a kinetic analysis result is deleted, the result from the kinetic analysis performed previously in sequence is displayed in the . 5.1.4.6 Delete Isothermal Analysis ‘This deletes the (Isothermal Analysis result) if Isothermal Analysis has been performed. Select [Delete Isothermal Analysis] from the [Analysis] menu, The will be deleted. —u— sis Program (Ozawa method) for TA-60WS 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. 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 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, 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 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, 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 xd for each set of DSC data separately. At this time, the is, the heating rate log and the inverse of the peak temperature (Ozawa plot) ig the kinetic energy, The horizontal axis is (I/T) [/K], and the vertical axis speci opened, displayi used in determ is LOGA This analysis function is used when the peak is smooth, or when you wish to specify the peak based on literature, ete Refer to Section 4.3.3 Kinetic Analysis Select peak 35 DSC Kinetic Analysis Program (Ozawa method) for TA-GOWS, 5. 11 Isothermal Analysis The kinetic energy obtained from the kinetic analysis is used to calculate the reaction percent and reaction time with respect (0 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. Refer to Section 4.4.1 Isothermal Analysis 36 DSC Kinetic Analysis Program (Ozawa method) for TA-6OW' 5.1.5 [Display Position] menu 5.1.5.1 Default display ‘his is used to automatically adjust the scale of the vertical and horizontal axis so that all of the data, from the smallest (othe largest value, will be displayed on the screen. The Y-axis value will be common to each set of data values Select [Default Display] from the [Display Position] menu, The data will be moved so that all ofthe data is displayed on the sereen, 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 al the data are aligned, CAUTION The Y-axis values and the data values will no longer correspond Select [Auto Start Point Arrangement] from the [Display Position] menu. The data will move so that all ofthe start points are aligned. seen tc ee 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. “The Y-axis values and the data values will no longer correspond, Select [Auto Slide] from the [Display Position] menu. The will open. oe DSC Kinetic Analysis Program (Ozawa method) for TA-GOWS, Enter @ value from -50 to 50 in the Slide Offset text box, and then seleet the [OK] button ‘The data willbe drawn in the <> atthe 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 “The Y-axis values and the data values will no longer comespond. Select [Manual Stide] from the [Display Position] menu, ‘The 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, seleet 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. ET NNT (see mayan —38— Program (Ozawa method) for TA-60WS 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, 39 DSC Kinetic Analysis Program (Ozawa method) for TA-6OWS 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 <>. {In addition to the plots, the file information and the measurement program, ete., may also be output. Select [All Analysis Result] from the [Report] menu, The used for formatting all of the kinetic analysis results will be opened. From the [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 By selecting the [Print Preview] item in the [File] menu of the , you may preview the report as it will appear when printed. For a detailed description of the , refer to Section 5.4 menu item —40- DSC Kinetic Analysis Program (Ozawa method) for TA-60WS 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. Select [Kinetic Analysis] from the (Report) menu, The used for formatting the kinetic analysis results will be opened. From the [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 By selecting the [Print Preview] item in the [File] menu of the , refer to Section 5.4 menu item ~a— DSC Kinetic Analysis Program (Ozawa method) for TA-60WS 5.1.6.3 Isothermal Analysis ‘This is used to output the tsothermal Analysis results in report format. In addition to graphed screens, information stored in files and analysis programs may also be reported. Select [Isothermal Analysis] from the [Report] menu, The used for formatting the Isothermal Analysis results will be opened, Select [Isothermal Graph] from the [Item] menu in the . ‘Afer setting up the report format, select the [Print] button to print out Isothermal Analysis results NOTE By selecting the [Print Preview] item in the [File] menu of the , you may preview te report as it will appear when printed, NOTE For a detailed description of the , refer to Section $4 menu item -~a- Program (Ozawa method) for TA-60WS 5.1.7. [Window] menu 5.1.7.1 Ozawa Plot The analysis result displayed in is always present as an icon in the <>, available whenever processing is necessary. This menu item is used for reopening the window whenever necessary. Select [Ozawa Plot] from the [Window] menu. The will be reopened to its original size and location on the screen. 1.7.2 Isothermal Analysis ‘The analysis result displayed in the is always present as an icon in the <>, available whenever processing is necessary. This menu item is used for reopening the window whenever Select [Isothermal Analysis] from the [Window] menu, The 4B DSC Kinetic Analysis Program (Ozawa method) for TA-60WS- 5.2 menu items 5.2.1 [Display] menu 5.2.1.1 Display Parameters ‘This is used to change the color and style of lines and marks in the Ozawa plot. Select [Display Parameters] from the [Display] menu in the . The will open. After completing the settings, select the [OK] button. These settings will then be used in the display of the . 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. Select [Cross Cursor] from the [Display] menu in the . 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. §.2.2. [Report] menu This is used to output the Ozawa Plot as a report. When the 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. Rofer to $.1.6.2. Kinetic Analysis —4— DSC Kinetic Analysis Program (Ozawa method) for TA-6OWS, 5.3 menu items 5.3.1 [Display] menu 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. Select (Reset Group] from the [Display] menu of the . ‘The will open. At the same time, an auxiliary frame will be displayed around the analysis result character string. Click the mouse atthe 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 [Cancef] 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 Select [Display Parameters] from the [Display] menu in the . ‘The 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