Pyris Software Guide

Pyris Software Guide

THERMAL ANALYSIS

Release History

Released Date Software Version January 2016 Release 13

Any comments about the documentation for this product should be addressed to:

User Assistance PerkinElmer, Inc. 710 Bridgeport Avenue Shelton, Connecticut 06484-4794 U.S.A.

Or emailed to: [email protected]

Notices

The information contained in this help file is subject to change without notice.

Except as specifically set forth in its terms and conditions of sale, PerkinElmer makes no warranty of any kind with regard to this help file, including, but not limited to, the implied warranties of merchantability and fitness for a particular purpose.

PerkinElmer shall not be liable for errors contained herein for incidental consequential damages in connection with furnishing, performance or use of this material.

Copyright Information

This help file contains proprietary information that is protected by copyright.

All rights are reserved. No part of this file may be reproduced in any form whatsoever or translated into any language without the prior, written permission of PerkinElmer, Inc.

Copyright © 2016 PerkinElmer, Inc.

Trademarks

Registered names, trademarks, etc. used in this help file, even when not specifically marked as such, are protected by law.

PerkinElmer is a registered trademark of PerkinElmer, Inc. Pyris is a trademark of PerkinElmer, Inc.

Microsoft and Windows are registered trademarks of Microsoft Corporation in the United States and other countries.

mailto:[email protected]

Table of Contents 3

Table of Contents Getting Started ....................................................................................................... 2 Getting Started with Pyris ................................................................................................ 3

Pyris Advanced Software ........................................................................................... 3 Pyris Help................................................................................................................. 3 Pyris User Manuals ................................................................................................... 3 Pyris Configuration ................................................................................................... 3 Data Analysis ........................................................................................................... 3 Pyris Manager .......................................................................................................... 3 Pyris ReadMe ........................................................................................................... 3

Access to Pyris Functions ................................................................................................. 4 Functions available without a USB key ....................................................................... 4 Functions requiring an Instrument Control or Advanced Instrument Control key ........... 4 Functions only available with an Advanced Instrument Control key .............................. 4

Using the Pyris Manager .................................................................................................. 5 To open the Pyris Manager........................................................................................ 5 Displaying the Pyris Manager ..................................................................................... 5 Features of the Pyris Manager ................................................................................... 6

Navigating in Pyris .......................................................................................................... 8 Customizing Pyris ............................................................................................................ 9

Dockable Toolbars, Status Panel, and Control Panel .................................................... 9 Customizing the Status Panel .................................................................................. 10 Customizing the Curves Display ............................................................................... 10

Using Pyris Enhanced Security ....................................................................................... 11 Pyris Enhanced Security .......................................................................................... 11

Security Settings ........................................................................................................... 13 Users ..................................................................................................................... 13 Groups ................................................................................................................... 15 Locking out users ................................................................................................... 18 Passwords .............................................................................................................. 19 Administration Audit Trail ........................................................................................ 20 Login History .......................................................................................................... 21 Database Report ..................................................................................................... 22 Audit Trail Viewer ................................................................................................... 23 Electronic Signatures .............................................................................................. 26 File Versioning ........................................................................................................ 27

Save Preferences Page .................................................................................................. 28 Tools for Support of Validation and Compliance ........................................................ 29

Pyris Software Compliance ............................................................................................. 30 Troubleshooting ............................................................................................................ 31 Setting Up your Analyzer ...................................................................................... 33 Pyris Configuration ........................................................................................................ 34

Analyzers/Ports Lists ............................................................................................... 34 Add Analyzer .......................................................................................................... 34 Edit........................................................................................................................ 35 Remove ................................................................................................................. 35

4 Pyris Software Guide

Add or Remove an Analyzer ........................................................................................... 36 Adding an Analyzer ................................................................................................. 36 Removing an Analyzer ............................................................................................. 36

Configure your Analyzer ................................................................................................. 37 Instrument Configuration......................................................................................... 37

DSC 8500 Instrument Configuration ................................................................................ 38 DSC 8000 Instrument Configuration ................................................................................ 40 DSC 6000 Configuration ................................................................................................. 42 DSC 4000 Configuration ................................................................................................. 44 Pyris 1 TGA Configuration .............................................................................................. 46 TGA 4000 Configuration ................................................................................................. 48 TGA 8000 Configuration ................................................................................................. 50 Configuring Remote Control of the TGA 8000 with a Mobile Device ................................... 53

Using the Remote Control dialog to define which mobile devices can control the TGA 8000 ...................................................................................................................... 53

STA 8000 Configuration ................................................................................................. 55 STA 6000 Configuration ................................................................................................. 57 DMA 8000 Configuration ................................................................................................ 59 Diamond DSC Configuration ........................................................................................... 61 Jade DSC Configuration.................................................................................................. 63 Pyris 1 DSC Configuration .............................................................................................. 65 Setting Preferences ........................................................................................................ 67

Preferences ............................................................................................................ 67 General Preferences Page ........................................................................................ 70 Color Preferences Page............................................................................................ 72 Graph Preferences Page .......................................................................................... 72 Save Preferences Page ............................................................................................ 73 Real-Time Curves Preferences Page ......................................................................... 74 Remote Access Preferences Page ............................................................................. 75 Purge Gas Preferences Page .................................................................................... 75 Autosampler Preferences Page ................................................................................. 76 Environment Tab Page ............................................................................................ 76

DSC 8500 Instrument Page ............................................................................................ 79 DSC 8000 Instrument Page ............................................................................................ 81 DSC 6000 Instrument Page ............................................................................................ 83 DSC 4000 Instrument Page ............................................................................................ 85 Pyris 1 TGA Instrument Page .......................................................................................... 87 TGA 4000 Instrument Page ............................................................................................ 88 TGA 8000 Instrument Page ............................................................................................ 90

Analyzer Constants .................................................................................................. 90 Y Data .................................................................................................................... 91

STA 8000 Instrument Page ............................................................................................ 92 STA 6000 Instrument Page ............................................................................................ 93 DMA 8000 Instrument Page ........................................................................................... 94 Diamond DSC Instrument Preferences Page .................................................................... 97 Jade DSC Instrument Page ........................................................................................... 100 Pyris 1 DSC Instrument Page ........................................................................................ 102

Table of Contents 5

Calibration........................................................................................................... 105 Calibration .................................................................................................................. 106 DSC 8000 and DSC 8500 Calibration ............................................................................. 107

Baseline Optimization for the DSC 8000 and DSC 8500 ........................................... 108 DSC 8000 and DSC 8500 Sample Temperature Calibration ...................................... 111 DSC 8000 and DSC 8500 Furnace Calibration ......................................................... 116 DSC 8000 and DSC 8500 Heat Flow Calibration ...................................................... 117 DSC 8000 and DSC 8500 SmartScan ...................................................................... 131

DSC 6000 Calibration ................................................................................................... 132 Temperature Calibration ....................................................................................... 133 Heat Flow Calibration ............................................................................................ 134

DSC 4000 Calibration ................................................................................................... 135 Temperature Calibration ....................................................................................... 136 Heat Flow Calibration ............................................................................................ 137

Pyris 1 TGA Calibration ................................................................................................ 138 Temperature Calibration ....................................................................................... 138 Weight Calibration ................................................................................................ 139 Furnace Calibration ............................................................................................... 139

TGA 4000 Calibration ................................................................................................... 140 Furnace Calibration ............................................................................................... 140 Temperature Calibration ....................................................................................... 141 Weight Calibration ................................................................................................ 141

TGA 8000 Calibration ................................................................................................... 142 Weight Calibration ................................................................................................ 143 Temperature Calibration ....................................................................................... 145

Calculating the Onset Value ......................................................................................... 148 TG Drift Calibration ............................................................................................... 150 Balance Drift Optimization ..................................................................................... 151

STA 8000 Calibration ................................................................................................... 152 Weight Calibration, TG Drift Optimization and DTA Baseline Optimization ................. 152 Temperature and Heat Flow Calibration ................................................................. 153

STA 6000 Calibration ................................................................................................... 156 Manual Weight and Sensor Calibration and Baseline Optimization ............................ 156 Temperature and Heat Flow Calibration ................................................................. 158

DMA 8000 Calibration .................................................................................................. 160 Balance Zero calibration ........................................................................................ 161 Force Factor calibration ......................................................................................... 161 Spring calibration .................................................................................................. 161 Temperature calibration ........................................................................................ 162 PID calibration ...................................................................................................... 163

Introduction to Calibration of the Pyris Diamond DSC .................................................... 164 Jade DSC Calibration ................................................................................................... 166

Temperature Calibration ....................................................................................... 167 Heat Flow Calibration ............................................................................................ 168

Pyris 1 DSC Calibration ................................................................................................ 169 Temperature Calibration ....................................................................................... 170 Heat Flow Calibration ............................................................................................ 171


Running Samples ................................................................................................ 173 Running Samples ......................................................................................................... 174 Instrument Applications ............................................................................................... 175

Instrument Applications ......................................................................................... 175 Status Panel ......................................................................................................... 176

DSC 8500 Instrument Application ................................................................................. 177 DSC 8000 Instrument Application ................................................................................. 180 DSC 6000 Instrument Application ................................................................................. 183 DSC 4000 Instrument Application ................................................................................. 186 Pyris 1 TGA Instrument Application ............................................................................... 189 TGA 4000 Instrument Application ................................................................................. 192 TGA 8000 Instrument Application ................................................................................. 194

Instrument Viewer ................................................................................................ 194 Method Editor ....................................................................................................... 195 Data Analysis ........................................................................................................ 195 Pyris Player ........................................................................................................... 195

STA 8000 Instrument Application .................................................................................. 197 STA 6000 Instrument Application .................................................................................. 200 DMA 8000 Instrument Application ................................................................................. 203 Diamond DSC Instrument Application ........................................................................... 205 Jade DSC Instrument Application .................................................................................. 208 Pyris 1 DSC Instrument Application ............................................................................... 211 Methods ...................................................................................................................... 214

Sample Info Page .................................................................................................. 216 Initial State Page .................................................................................................. 218 Initial State Page for DMA 8000 ............................................................................. 221 Program Page ....................................................................................................... 224 Method Steps Section ............................................................................................ 224 Edit Step Section ................................................................................................... 225 Method Actions and Events .................................................................................... 225 Set End Condition Section ...................................................................................... 226 Step Info Section .................................................................................................. 227 AutoStepwise Step Info Section ............................................................................. 228 Variable Rate Scan Step Info Section – TGA 8000 only ............................................ 229 Program Page for DMA 8000 .................................................................................. 231 DMA 8000 Method Steps ....................................................................................... 234 Method Actions and Events .................................................................................... 237

Control Panel ............................................................................................................... 243 DSC 8500 Control Panel ............................................................................................... 244

Performing the DSC Clean Furnace Procedure ......................................................... 244 DSC 8000 Control Panel ............................................................................................... 248

Performing the DSC Clean Furnace Procedure. ........................................................ 248 DSC 6000 Control Panel ............................................................................................... 252 DSC 4000 Control Panel ............................................................................................... 254 Pyris 1 TGA Control Panel............................................................................................. 256 TGA 4000 Control Panel ............................................................................................... 259 TGA 8000 Control Panel ............................................................................................... 261

Table of Contents 7

STA 8000 Control Panel ............................................................................................... 264 STA 6000 Control Panel ............................................................................................... 266 DMA 8000 Control Panel .............................................................................................. 268 Diamond DSC Control Panel ......................................................................................... 271 Pyris 1 DSC Control Panel ............................................................................................ 273 Jade DSC Control Panel ............................................................................................... 275 Monitoring Data Collection ........................................................................................... 277

Instrument Viewer ................................................................................................ 277 Status Panel ......................................................................................................... 277 Using the Monitor ................................................................................................. 277 Pyris Manager ...................................................................................................... 278

Remote Monitor .......................................................................................................... 279 Starting the Remote Monitor ................................................................................. 279 Viewing the Instrument Monitor and Status Panel ................................................... 279 Stopping a Run in the Remote Monitor ................................................................... 280

Pyris Player ................................................................................................................. 281 Pyris Player Toolbars............................................................................................. 282 Pyris Player Setup Page ........................................................................................ 282 Pyris Player Edit Play List Page .............................................................................. 283 Creating and Running a Play List ........................................................................... 285 Pyris Player View Play List Page ............................................................................. 286 Pyris Player View Sample List ................................................................................ 287 Pyris Player View History Page ............................................................................... 288 Pyris Player Sample History Page ........................................................................... 290

Valet .......................................................................................................................... 292 Analyzing Data .................................................................................................... 295 Data Analysis .............................................................................................................. 296 Display Curves ............................................................................................................ 297 Optimizing the Data Display ......................................................................................... 298

Rescaling ............................................................................................................. 298 Shift Curves ......................................................................................................... 298 Change the Curve's Slope...................................................................................... 299 Annotate Curves ................................................................................................... 299

DMA 8000 (TTS) Time-Temperature Superposition ....................................................... 300 How Does TTS Work ............................................................................................. 300 Will TTS Work on my Sample? ............................................................................... 301 How to Use Time-Temperature Superposition ......................................................... 301

Math, Calc, and Curves Menus ..................................................................................... 306 Math, Calc, and Curves Menus ............................................................................... 306 Math Menu ........................................................................................................... 306 Calc Menu ............................................................................................................ 307 Curves Menus ....................................................................................................... 307

Viewing Methods and Results ....................................................................................... 308 View Results ......................................................................................................... 308 View Methods ....................................................................................................... 308

Saving Processed Data ................................................................................................ 310 Sharing Data ....................................................................................................... 311


Sharing Data ............................................................................................................... 312 Report Manager ........................................................................................................... 313

Report Manager .................................................................................................... 313 Select a Stored Template or Create a New Template ............................................... 314 Select the Output File ............................................................................................ 314 Specify Items in Report ......................................................................................... 315 Create the Report ................................................................................................. 319

Printing ....................................................................................................................... 320 Print dialog box ..................................................................................................... 320 Print Setup dialog box ........................................................................................... 320

Exporting Data ............................................................................................................ 322 Importing and Converting Data .................................................................................... 323 Index ................................................................................................................... 325 Index .......................................................................................................................... 326

Getting Started

Getting Started with Pyris 3

Getting Started with Pyris

The Pyris group of items is accessible by selecting Programs and then PerkinElmer Applications from the Windows Start menu. Items in the Pyris menu reflect how the software is organized. They are as follows:

Pyris Advanced Software

This provides options for the installation of advanced software components, such as StepScan or Pyris Kinetics, and Pyris Enhanced Security.

Pyris Help

Software Help is the online documentation for Pyris Software.

Pyris User Manuals

The options available under this heading allow you to view various Pyris documents in .PDF format.

Pyris Configuration

Use Pyris Configuration to dynamically configure the analyzers in your system. Pyris Config can be opened from the Pyris Manager Start Pyris button or from the Pyris program group.

Data Analysis

This Pyris application analyzes data collected by any analyzer. This application is not associated with a particular analyzer and can be used to analyze data and edit methods for any instrument attached to your thermal analysis system. More than one Data Analysis Application can be opened at a time.

Pyris Manager

The Pyris Manager provides access to the Instrument Application for each configured instrument in your system. From the Start Pyris button in Pyris Manager, you can also access the Data Analysis application, monitor the system status, run Pyris Configuration, access Pyris Help, and close all Pyris-related windows.

Pyris ReadMe

This text file contains the latest information on the version of Pyris installed on your computer. It lists the new features included in the software and any information on the software or hardware that did not get included in the online Help.


Access to Pyris Functions

Access to some of the functions provided by the Pyris software requires you to insert a USB key into your PC. Two keys are available: an Instrument Control key and an Advanced Instrument Control key.

Functions available without a USB key

Without an Instrument Control or Advanced Instrument Control key, your access is restricted to those functions associated with basic analysis of existing Pyris data files.

None of the instrument control or configuration options are available.

In addition, the following advanced options within Data Analysis are also not available:

• DSC Isothermal Kinetics

• DSC Scanning Kinetics

• DSC Purity

• DSC Specific Heat

• DSC Stepscan

• TGA Autostepwise

• TGA Decomposition Kinetics

If you attempt to access any of the functions that require a USB key, a message is displayed indicating that access is restricted.

NOTE: If you have installed Pyris Enhanced Security, access to any Pyris function requires that you insert the appropriate USB key.

Functions requiring an Instrument Control or Advanced Instrument Control key

Both the Instrument Control and Advanced Instrument Control keys provide access to the USB key-restricted instrument control and configuration options. You must insert either type of key to add an analyzer, for example.

If you have inserted an Instrument Control key and attempt to access any of the functions that require an Advanced Instrument Control key, a message is displayed indicating that access is further restricted.

Functions only available with an Advanced Instrument Control key

An Advanced Instrument Control key is required for access to the advanced USB key-restricted Data Analysis options listed above.

Using the Pyris Manager 5

Using the Pyris Manager

The Pyris Manager is the main location from which to operate the Pyris Series Thermal Analysis System. The Pyris Manager is used to start instrument applications and Data Analysis applications can be initiated from there. Analyzers can be added to and removed from the system dynamically with the Configuration utility which is accessed from the Pyris Manager task menu. The status of each analyzer in the system can be monitored in Pyris Manager as well.

To open the Pyris Manager

Double-click Pyris Manager in the Pyris Software folder in the Programs menu which is accessed via the Windows Start button. A shortcut to the Pyris Manager may be on the desktop and/or in the Start menu if either or both of these options were selected during installation.

Displaying the Pyris Manager

The Pyris Manager can be displayed horizontally or vertically on the screen. If it is horizontal and you want it displayed vertically, just click and drag the Pyris Manager down into the middle of the screen; it will redisplay vertically. To change from vertical to horizontal display, place the cursor in the Pyris Manager (but not on an instrument button or the Start Pyris button), click and hold down the left mouse button, and start moving the mouse to the left, to move the Manager from across the top to down the left-hand side of the screen. Or start moving the mouse to the top and the right to move the Pyris Manager from the left side up to across the top of the screen. If the Autohide feature is activated, the bar shrinks to a smaller area as it is moved. Just the Start Pyris button is displayed.

Place the cursor within the Pyris Manager and click the right mouse button to display the Pyris Manager pop-up menu:

• Select Always on top to keep the Pyris Manager available for display. How it behaves depends on whether Autohide is activated. When Always on top is activated, a checkmark appears next to item.

• Select Autohide to have the Pyris Manager “hide” when in Pyris or another application such a word processor. Always on top must be selected. When both are activated, the


Pyris Manager will roll off of the screen so that it does not take up room on your display but it is always available. For example, if it is displayed horizontally and moved to the bottom of the screen and you move the cursor up into the screen, the Pyris Manager will roll off of the screen. Bring the cursor back to the bottom of the screen, by the Windows task bar, and Pyris Manager will reappear. If you select Autohide when Always on top is not selected, the Pyris Manager will close automatically when you select an Instrument Application. When activated, a checkmark appears next to the item in the popup menu.

• You can change the display of all your open Pyris windows by selecting Cascade, Tile Horizontally, or Tile Vertically. These are the standard Windows features. Selecting any of these options does affect non-Pyris windows.

• You can minimize all open Pyris windows to the task bar at the bottom of the screen by clicking on Minimize All. Redisplay in maximum size all Pyris windows that are indicated on the task bar by clicking on Maximize All in the popup menu. Restore All restores all Pyris windows to their original position and size before they were minimized or maximized.

Features of the Pyris Manager

The Pyris Manager contains a Start Pyris button and a button for each configured instrument on your system. Beneath the Start Pyris button are left and right arrow buttons if the Pyris Manager is horizontal and up and down arrow buttons if the Pyris Manager is vertical. These are used to scroll the instrument buttons left or right or up and down if there are more buttons than can be displayed on the screen. Click the Start Pyris button to display the Pyris Task menu:

• Access Data Analysis Applications from here rather than from the Programs menu.

• Open and run Pyris Configuration to dynamically add an instrument to or remove an instrument from the system. Each configured thermal analyzer is represented by a button on the Pyris Manager.

• If you are running Enhanced Security Pyris, access the User Management utility to set security settings such as setting up users, groups, and password control. The User Management utility also gives you access to the login history and the audit trail of all changes made to Pyris security settings.

• Open online Pyris Help by clicking Help.

• Close all Pyris windows via Close All.

The instrument buttons on the Pyris Manager are used to enter the Instrument Application. They are also used to monitor the status of the instrument. If you place the cursor within the

Using the Pyris Manager 7

button but not in a display field and click on the right mouse button, the Change Status Information dialog box appears:

Here you can change the information displayed on the instrument button. Display the drop-down menus for both status lines and select the parameter you want displayed. The list of available items for both status lines is instrument-dependent.


Navigating in Pyris

It is easy to navigate around Pyris software components. You can go from Instrument Viewer to Method Editor to Data Analysis and other parts by a click of the mouse on the standard toolbar. The first four buttons on the standard toolbar are used to navigate between the four major parts of Pyris.

When a window such as Pyris Player or Calibration displays tabs, indicating that there are pages that make up the window, click on the tab to display the page on top of the other pages.

Another way to navigate is the use of the menu bar. Each menu item contains a specific drop-down list dependent on the analyzer and the window displayed.

Customizing Pyris 9

Customizing Pyris

You can customize Pyris software to suit your needs. You can change the way the screen looks, how curves are displayed, and the default values for many program parameters.

Dockable Toolbars, Status Panel, and Control Panel

All toolbars – standard, Pyris, and Rescale Tools – and the status panel can be attached to any side of the Pyris window or they can “float” over the window. The control panel can be attached to the left or right side of the Pyris window. When a toolbar, the status panel, or the control panel floats, it has a title bar. The graphic below shows the status panel and standard toolbar "floating" on the Pyris screen. Each one has a title bar.

Click the background of the toolbar or panel and drag it to the desired location. When you drag a dock able toolbar or panel to any edge of the Pyris window, it becomes attached to that side.


Customizing the Status Panel

The Status Panel consists of boxes each of which contains a parameter name and that parameter’s current value. Each box contains a drop-down list of parameters from which you select the parameter to be displayed in that box. As soon as you select a parameter, its current value is displayed in the lower part of the box. If you highlight the entry field in the status panel and then type the first letter of another parameter, then that parameter, or another parameter that begins with that letter, will be displayed. You can scroll through all parameters starting with that letter by continuously pressing that key.

The status panel must contain at least one parameter box. To resize the status panel (for example, to eliminate or add a parameter box), first detach the status panel from the window frame (click it and drag it away from the window frame), then click and drag the status panel border to include or exclude a box.

Customizing the Curves Display

Pyris software supports right-click menus in the graphics displays, for example, Instrument Viewer and Data Analysis. You can customize the display using the items available on these menus.

Using Pyris Enhanced Security 11

Using Pyris Enhanced Security

Pyris Enhanced Security

Pyris Enhanced Security is an optional add-on to Pyris software, which provides technical compliance to 21CFR Part 11.

NOTE: If you have installed Pyris Enhanced Security, access to any Pyris function requires that you insert the appropriate USB key. See Access to Pyris Functions for details.

Click on an item below to learn more about the features that Pyris Enhanced Security offers:

Audit Trails

Pyris Enhanced Security creates secure, computer generated, time-stamped audit trails, which record all significant actions performed by each user, including those on calibration, method editor and data analysis. The audit trails for data/system changes and for electronic signatures are displayed in a viewer, consisting of a tree control that houses the audit trail/signature information. For ease of use, the viewer offers a filter routine, which allows for a subset of the entire list to be viewed.

For more information on Audit Trails, see Audit Trail Viewer.

In addition, Pyris Enhanced Security provides an audit trail for changes in user management and login history. This audit trail is accessed through the User Management utility.

For more information on the audit trail for changes in user management, see Administration Audit Trail.

Electronic Signatures

Pyris Enhanced Security provides an electronic signature feature that is user definable, as well as a customizable reasons list. Users with assigned permission have the ability to place electronic signatures at any time by selecting the E-Signature option from the Tools menu. Pyris Enhanced Security's electronic signature feature captures the document that is being signed, the reason for the signature, the date/time and who is signing. If you choose not to implement electronic signatures, this feature can be disabled.

For more information on Electronic Signatures, see Electronic Signatures.

User Level Management and Security

Pyris Enhanced Security uses a secure login process that defines user groups, passwords and grants different permission levels, reflecting your laboratory workflow. The software initially provides one administrator user with all permissions and four predefined user groups. These groups can be used as is or modified as needed. In addition, new groups can be created and permissions as well as instrument access can be assigned to meet your laboratory's specific requirements.

For more information on User Level Management and Security, see Security Settings.

File Integrity

Pyris Enhanced Security assigns versions to files and data objects when changes have occurred. This prevents older versions of data files from being overwritten. Through File Integrity Assurance, the software detects external file tampering, creates an audit trail item and provides notification the next time the file is opened. You can view the version history


of files from the History directory, which is a subdirectory of the directory where the Pyris program is installed.

For more information on File Integrity, see File Versioning.

Recommendations

The installation of Pyris Enhanced Security Software will ensure technical compliance to the 21 CFR Part 11 regulations. In addition, the user’s organization must establish a range of policies and standard operating procedures that complement the capabilities provided by the software in order to ensure complete compliance to the rule.

1. According to CFR Ref 11.300(d), the regulations require a procedure for detecting attempts at unauthorized use and for informing security (for example, is the system capable of detecting and reporting to the system security unit any attempts at unauthorized use of passwords and/or identification codes?). In Pyris Enhanced Security, if unauthorized attempts to login take place, these events are recorded in the Audit Trail but the Administrator doesn’t get notified automatically. The Administrator needs to check Audit Trail login history on a regular basis.

2. According to CFR Ref 11.10(h), if it is a requirement of the system that input data or instructions can only come from certain input devices (for example terminals), does the system check the validity of the source of any data or instructions received?

NOTE: This applies where data or instructions can come from more than one device, and therefore the system must verify the integrity of its source, such as a network of weigh scales, or remote, radio controlled terminals.

Pyris Enhanced Security Software does not have the ability to automatically recognize the serial number of the instrument that is being used, so manual input of the serial number is required. If the instrument is switched, an SOP is required to assure that the user updates the instrument configuration.

Security Settings 13

Security Settings

The Security settings are only available to Administrators who are using the Enhanced Security Version of Pyris. You set up users, groups, and password settings from the User Management utility located under the Pyris Start menu.

Administrators are also able to view the Audit Trail, Login History and Database Report through the User Management utility.

Users

What are the default users?

The following users are pre-defined in the Enhanced Security Version of Pyris: Pyris Technician, Pyris Developer, Pyris User, and Pyris Administrator.

NOTE: It is possible to change the group membership of the default users. By default, the default users are only members of the default group with the same name. For example, the Pyris Technician is a member of the Pyris Technicians group, and the Pyris Developer is a member of the Pyris Developers group.

How do I add a new user?

1. From Pyris Manager click Start Pyris > User Management, type in your user name and password when prompted with the PerkinElmer login dialog box, and click OK. The Users, Groups, Password Control, Login History, Audit Trail, and Database Report Properties dialog box appears.

2. Select the Users tab and click New. The New User dialog box appears.

3. Enter the User name, Full name, Password, and repeat it in the Confirm password entry field. The password length is defined on the Password Control tab.

NOTE: The Password is case-sensitive. It can consist of letters, numbers and single spaces only.

4. Select Enabled if you wish the user to be able to login or Disabled if you do not wish him to be able to login at the current time.

5. Click OK. The User name drop-down list is updated with the new user.

NOTE: A new user will be forced to change their password when they first log in.

How do I delete a user?

1. Select the user from the User Name drop-down list on the Users tab and then click Delete. A message is displayed asking you to confirm that you wish to delete the user.

2. Click OK. The user is deleted.

NOTE: It is not possible to reuse a User name that has been deleted.


How do I assign a user to a group?

Users can be assigned to one or more groups.

1. Select the user from the User Name drop-down list on the User tab.

2. Select the Group from the list of Available groups for user and then click Add. The Group is added to the User is a member of list.

If you wish to create more than one new user and assign each of them to a group/groups you must click Apply after assigning the groups to the first user before creating the next new user, otherwise the group assignments for the currently selected user will be lost.

NOTE: When a group is added to the User is a member of list, it no longer appears in the Available groups for user list.

How do I remove a user from a group?

To remove a user from a group, select the User Name on the User tab, then, and select the group from the User is a member of list, and click Remove. The user is removed from the group. The group is removed from the User is a member of list, and is added to the Available groups for user list.

How do I disable an individual user?


2. Select the Users tab and highlight the user you wish to disable and click Edit. A New / Edit User dialog box appears.

3. To disable the user, select Disabled. When the disabled user attempts to login an error message is displayed informing the user that his login failed.

4. Click OK. The User is disabled.

NOTE: To enable the user select Enabled on this dialog box. You must also enter and confirm a new password when enabling a user.

NOTE: All user updates are recorded in the audit log.


Groups NOTE: The Groups are permissions-based. If you are a member of multiple groups, you

default to the maximum permissions rather than the minimum for the groups you are assigned to. The Instrument should have no permissions and a separate group should be used to set a user's permissions.

What are the default groups and what can members of these groups do? The following table lists the default groups together with what members of the group are able to do:

Group Member of the group is able to:

Pyris Technicians Run methods and view results.

Pyris Developers Read methods, delete methods and folders, copy and move methods, configure instruments, and set up instrument validation.

Pyris Users Read methods, copy and move methods, approve methods, view results, and approve results.

Pyris Administrators

Read methods, perform administration tasks, delete methods and folders, copy and move methods, and view results.

How do I create a new group?

1. From Pyris manager click Start Pyris > User Management, type in your user name and password when prompted with the PerkinElmer login dialog box, and click OK. The Users, Groups, Password Control, Login History, Audit Trail and Database Report Properties dialog box appears.

2. Select the Groups tab and click New. A New Group dialog box is displayed.

3. Enter a Group name and click OK. The drop-down list is updated to include the new group. By default, none of the options in the Members of the group are able to list are selected.

How do I define what members of a group are able to do?

The options available to each group are selected on the Groups tab. Each group can be assigned one or more options from the Members of the group are able to list:

Perform Administration Tasks

The user has Administration rights. The user is able to setup users, groups and their permissions, and define password controls. He can also determine the visibility of folders.

Run the Pyris Application

The user is able to access basic features such as running the Pyris Manager and accessing Data Analysis.

Create & Save Data Results

The user is able to create and save his results.

Create & Edit Method Files

The user is able to create and edit method files.

View Configuration Files

The user is able to gain Read-only access to Pyris Configure in order to review instrument' configurations.


Configure Instruments

The user is granted permission to add, remove and edit analyzers.

Flash EPROMs The user is able to update the Pyris EPROM in an analyzer.

Edit Preferences

The user is able to open, view, create and edit instrument-related preference files.

Create & Edit Reports Files

The user is able to create and edit report templates from the Report Manager.

Create & Edit PlayList Files

The user is able to create and edit PlayList files.

Calibrate Instruments

The user is able to calibrate an instrument and change calibration files.

Apply Electronic Signatures

The user is able to electronically sign data.

1. To assign one of the options, click in the box next to the option you wish to assign to the group. A tick indicates that the option is available for the group.

NOTE: Bear in mind that some permissions rely on access to certain parts of the software set by other permissions. For example, to Configure instruments you need the general access to Explorer given by Methods.

2. When all the required options are selected, click Apply. The available options for the group are updated.

How do I delete a group?

1. To delete a group, select the Group from the Name drop-down list and then click Delete. A message is displayed asking you to confirm that you wish to delete the selected group.

2. Click OK. The group is deleted.

How do I assign a user to a group?

Users can be assigned to one or more groups.


2. Select the Group from the list of Available groups for user and then click Add. The Group is added to the User is a member of list.

If you wish to create more than one new user and assign each of them to a group/groups you must click Apply after assigning the groups to the first user before creating the next new user, otherwise the group assignments for the currently selected user will be lost.

NOTE: When a group is added to the User is a member of list, it no longer appears in the Available groups for user list.


How do I add a user to an instrument group?

When an analyzer is added through the Pyris Configuration utility, a User Group with the exact name (this is case sensitive) of the analyzer must be created, so that different users can be assigned the use of different analyzers.

The analyzer group that is created has no permissions set. Therefore, users, which belong to groups with permissions must be added to a desired analyzer group. When a user is added to an analyzer group, permissions are combined. In other words, by being assigned to one of the four pre-defined groups, the user will have all the permissions available through that group. That way, a technician could be restricted to the use of only one analyzer in a three analyzer system (with only technician level access), while an administrator can have access to all three analyzers with full administrator level access.

1. After an Analyzer has been added, click Edit from the Pyris Configuration window. The Pyris (Instrument Name) Configuration window appears.

2. Enter the name of the Analyzer in the Name dialog box.

3. Enter the Serial Number of the analyzer in the Serial Number dialog box.

4. Click OK.

5. From the Pyris Manager click Start Pyris>User Management. The Users, Groups, Login History, Password Control, Audit Trail and Database Report Properties dialog box appears.

6. Select the Groups tab and click New. The New Group dialog box is displayed.

7. Enter the exact name you used for the analyzer in the Pyris Configuration dialog box and click OK. The drop-down list is updated to include the new group. By default, none of the options in the Members of the group are able to list are selected.


9. Select the analyzer group from the list of Available groups for user and then click Add. The Group is added to the User is a member of list.


How do I remove a user from a group?

To remove a user from a group, select the User Name on the User tab, then, select the group from the User is a member of list, and click Remove. The user is removed from the group. The group is removed from the User is a member of list, and is added to the Available groups for user list.

Locking out users NOTE: Make sure that the Lockout Duration for your Administrator account is set for a

period of time (Duration) and not set to Permanent. In the event that the Administrator cannot remember his password, and Lockout Duration is set to Permanent, there will be no way for the administrator to access the application.

How do I limit the number of failed login attempts?

1. From the Users, Groups, Signatures and Password Control dialog box select the Password Control tab.

2. Click Account Lockout. The Account Lockout dialog box is displayed.

3. Enter the Number of failed logins allowed before lockout. For example, if Number of failed logins allowed before lockout is set to 5, the user is allowed five failed attempts at login. On the fifth failed attempt they are locked out until the Administrator allows them access again (Permanent) or for a specified period of time (Duration). The default is lockout after 5 failed login attempts. The minimum number of failed login attempts before a user is locked out is 1. The maximum number of allowed failed login attempts before a user is locked out is 10.

4. Select the Lockout Duration as Permanent, until Administrator unlocks, or Duration. If you select Duration, enter the time (in minutes) for the lockout.

NOTE: If Number of failed logins allowed before lockout is set to 1 the user will be locked out when they have one incorrect login attempt. That is, they are not allowed an incorrect login attempt, otherwise they will be immediately locked out.

What is Permanent Lockout and Duration?

Permanent until administrator unlocks means that the user will be unable to login again until the administrator has unlocked their account and assigned a new password. Duration prevents the user being able to login again until the time specified has elapsed. Duration is grayed if Permanent is selected.

If Duration is selected, the default is 60 minutes. The minimum Duration is 1 minute and the maximum Duration is 32767 minutes (22.75 days).

NOTE: In the Enhanced Security version of software, details of failed login attempts are recorded in the Login History.

How do I reinstate Locked-Out Users?

If the Lockout is set to Permanent until administrator unlocks and the user has failed to login correctly within the allowed number of attempts, the administrator must assign a new password before they are able to login again.

When the administrator next logs in after a user has been locked out, a list of Locked Out Users is displayed.


1. Highlight the name of the user that you wish to reinstate and then click Edit. The Edit User dialog box appears.

2. Enter a new Password and repeat it in the Confirm password field.

3. Click OK. The user is removed from the list of Locked Out Users.

4. Click OK to close the Locked Out Users dialog box. The previously locked out user will now be able to log in using the new password, which they will be forced to change.

NOTE: If you click OK rather than Edit when the list of Locked Out Users is displayed, the list is closed and the application starts. Any locked out users will remain locked out. The list will be redisplayed each time you log in until any locked out users have each been assigned a new password.

NOTE: Users locked out for a specified duration can be unlocked by the administrator in the same manner.

Passwords NOTE: Passwords are case-sensitive.

How do I change a Password?

1. To change a user's password, select the user from the User name drop-down list on the User's tab and then click Edit. An Edit User dialog box appears.

2. Enter the new Password and repeat it in the Confirm password entry field.

3. Click OK. The new password is implemented. The next time the user logs in they will be forced to change their password.

How do I define when users must change their password?

NOTE: The settings on the Password Control tab apply to all users. It is not possible to define individual Password Controls for each user.

On the Password Control tab, Maximum password age defines the maximum number of days that users can retain the same password before they must change it. By default the password expires after 42 days. The minimum is 1 day and the maximum is 999 days.

The Maximum password age cannot be set less than or equal to the Minimum password age.

NOTE: If you want to set the Maximum password age to 1 day the Minimum password age must first be set to Allow changes immediately.

If it is not necessary for users to change their password, select Password never expires, under Maximum password age.

How do I define the minimum length of time that users must retain the same password before they are able to change it?


On the Password Control tab, Minimum password age defines the number of days that users must retain the same password before being allowed to change it. The default is to Allow changes after 1 days. This prevents users from changing their password several times in a short space of time in order to return to a previous password.

To allow users to be able to change their password immediately, select Allow changes immediately.

The Minimum password age cannot be set greater than or equal to the Maximum password age. The minimum is 1 day and the maximum is 999 days.

NOTE: If you want to set the Maximum password age to 1 day the Minimum password age must first be set to Allow changes immediately.

How do I define the length of a password?

Minimum password length on the Password Control tab defines the minimum number of characters that must be used in the password. By default, At least 6 characters is selected. The default number of characters that must be used in the password is 6. The minimum is 1 and the maximum is 16 characters.

Allow blank password is an alternative option. This means that users are not required to enter a password on login, providing the user has previously opted to not enter a password when they last changed their password, or if they have never logged in before.

NOTE: A second blank password cannot be used immediately when a blank password expires if Number of passwords to remember has been selected in the Password uniqueness section of the Password Control tab.

Can a password be reused?

Users are able to reuse a previous password. By default, Number of passwords to remember is set to 24.

Password uniqueness on the Password Control tab defines the number of new passwords that must be used before a previous password can be reused. For example, if the first password is 'security', and Number of passwords to remember is set to 3 entries, users must use 3 other passwords in addition to their current password before they are able to reuse 'security' as their password. The minimum is 1 and the maximum is 24.

If Do not keep password history is selected a user is able to reuse a password whenever they wish.

Administration Audit Trail NOTE: The Audit Trail can only be viewed by users able to perform administration tasks in

the Enhanced Security Version of Pyris.

The Administration Audit Trail records all changes to security settings in compliance with 21 CFR Part 11. All changes to users, groups, and password settings are recorded.

1. From Pyris Manager click Start Pyris > User Management, type in your user name and password when prompted with the PerkinElmer login dialog box, and click OK. The Users, Groups, Password Control, Login History, Audit Trail and Database Report Properties dialog box appears.

2. Select the Audit Trail tab.


The audit trail is displayed. For each change recorded, the following information is given in the Audit Trail:

• Function - the item that was changed, for example, Add New User

• Previous Value - the state of the item before it was changed

• Current Value - the new state

• Full Name - the full name of the user who made the change

• User Name - the login user name of the user who made the change

• Date Modified - the date and time of the change

Printing the Audit Trail

To print the Audit Trail, click Print. All the information currently held in the Audit Trail is printed.

Exporting the Audit Trail

1. To export the Audit Trail, click Export. A Save As dialog box appears.

2. Select the required destination and enter a filename. The Audit Trail is exported as a *. csv file and can be opened, for example, in Microsoft Excel.

NOTE: Exporting the Audit Trail does not clear the Audit Trail details from the dialog box.

Clearing the Audit Trail

To clear the Audit Trail, click Clear Audit. You are prompted with a message asking you to confirm that you want to delete the Audit Trail log. All details are removed.

NOTE: It is only possible to clear Audit Trail entries that have previously been exported. If the Audit Trail contains additional entries since it was last exported, only those entries that have been exported will be deleted. If none of the entries have been exported, a warning message will be displayed when you attempt to clear the Audit Trail.

Login History

The Login History can only be viewed by users, running the Enhanced Security Version of Pyris, who are members of a group that has permission to perform administration tasks.


2. Select the Login History tab. The login history appears. This details every login attempt, since the history was last cleared, by:

• Full Name


• User Name • Status - OK indicates that the user logged in with the correct password,

Failed indicates that a login was attempted with an incorrect password. • Logged In - date and time. • Logged Out - date and time.

NOTE: If a non-existent User Name is entered during login, a failed login attempt is recorded. Not Found is entered in the Full Name field of the Login History, and the incorrectly entered User Name is also recorded.

NOTE: There is no limit to the size of the Login History.

Printing the Login History

To print the Login History click Print. All the information currently held in the Login History is printed.

Exporting the Login History

1. To export the Login History click Export. A Save As dialog box appears.

2. Select the required destination and enter a filename. The Login History is exported as a *. csv file and can be opened, for example, in Microsoft Excel.

NOTE: Exporting the Login History does not clear the Login History details from the dialog box.

Clearing the Login History

To clear the Login History, click Clear History. You are prompted with a dialog box asking to confirm that you want to delete the Login History log. All Login details are removed. The first Login details to appear after the Login has been cleared will be the date and time that you log out.

NOTE: It is only possible to clear Login History entries that have previously been exported. If the Login History contains additional entries since it was last exported, only those entries that have been exported will be deleted. If none of the entries have been exported, a warning message will be displayed when you attempt to clear the Login History.

Database Report NOTE: The Database Report can only be viewed by users able to perform administration

tasks.

1. From Pyris Manager click Start Pyris > User Management, type in your user name and password when prompted with the PerkinElmer login dialog box, and click OK. The Users, Groups, Login History, Password Control, Audit Trail, and Database Report Properties dialog box appears.

2. Select the Database Report Properties tab. The database report appears.

The Database Report records all information about the security settings:


Password control - it records maximum password age, minimum password age, minimum password length, password uniqueness, lockout count and lockout duration.

Permissions - it records the number of permissions and lists all the permissions.

Users - it records the number of users. For each user it records the username, full name, status, last login, the group the user belongs to, and the permissions of that group.

Groups - it records the number of groups. For each group it records the group name, the users in the group, and the group permissions.

Printing the Database Report

To print the Database Report click Print. The database report is printed.

Exporting the Database Report

1. To export the Database Report click Export. A Save As dialog box appears.

2. Select the required destination and enter a filename. The Audit Trail can be exported as a *. csv file or a *.txt file.

Audit Trail Viewer

In the Enhanced Security Version of Pyris, every significant operational event that affects a file or analytical data performed with your software is recorded in an application log, which can be viewed from the Data Analysis application by selecting Tools>Audit Trail>View Log. System changes and electronic signature records are also accessible through the Audit Trail Viewer.

Click on one of the links below for information on: The Audit Trail Viewer Using the Audit Trail Viewer Creating an Electronic Signature Printing the Audit Trail

NOTE: After clicking on one of the links below you can click to return to the top of this page.

About this Window

If you are using the Enhanced Security Version of Pyris, use this window to view the audit trails of changes made to the following files:

• Data Files

• Method Files

• Play list Files

• Calibration Files

• Report Templates

• Pyris.Inst


For each audited file the following information is recorded and can be viewed by clicking on the folders displayed in the tree structure of the Audit Trail Viewer.

• Date and time of change

• Where the change was made (specifies the file or record that was modified)

• What was changed (indicates the parameter that was changed)

• Application Software

• Computer and Operating System

• Windows UserID

• The Pyris user who made the change

• Description of the change that was made (the before and after value of the altered field is displayed)

• Why the change was made

• Detailed description of change

NOTE: When you are entering numeric values by using (the spin buttons), an audit trail entry is automatically created each time you click on one of the arrows. Therefore, it is recommended that you simply type in the numeric value to avoid creating a lengthy audit trail.

Using this Window

1. Open the file for which you wish to view the audit trail.

2. From the Tools menu select Audit Trail>View Log. The Audit Trail is displayed with the name of the current audited file listed in the upper left portion of the window. OR If you wish to view the Audit Log for the Pyris.Inst file check View System Log. The Audit Trail for the Pyris.Inst file appears in the viewer.

3. From the Display Settings controls select from the drop down menus what information you wish displayed in the tree.

4. The Display Settings controls consist of four drop-down menus, which you use to specify what information is displayed in the audit trail tree. These controls only filter what information is displayed on your screen, they do not modify the actual audit trail.


5. Click Update Display. The tree display is updated to fit selected display settings.

6. Click on or to open or close the folders displayed in the tree. OR Double click on a folder to display a popup window that contains detailed audit trail information for a specific event.

7. Click Close to close the audit trail viewer dialog box.

To Electronically sign an audit trail

1. From the Tools menu, select Audit Trail > View Log.

2. Click Sign this Audit Trail. The Electronic Signature dialog box appears.

3. Select a reason from the Reason for Signing drop down menu. OR Type in your own reason in the Reason for Signing dialog box.

4. Type your Logon ID and Password in the corresponding dialog boxes.

5. If desired type in any comments in the Comment dialog box.

6. Click Apply Signature.

NOTE: If an administrator decides to apply an electronic signature to something in another user's session, the administrator can click on the check box next to Sign on Behalf of and select the user he wishes to sign for. Pyris will correctly validate the username and password of the user, and the audit trail recognizes that it was the administrator who signed.

Printing the current Audit Trail

Click Print this Audit Trail. An Audit Trail Print dialog box appears that gives two options: Summary - Prints out what you see in the Audit Trail Viewer. OR


Detail - Prints an expanded view of the items that are currently displayed in the Audit Trail viewer.

Electronic Signatures

Pyris Enhanced Security provides an electronic signature feature that is user-definable with a customizable reasons list. Users with assigned permission can place electronic signatures at any time by selecting Tools > E-Signature. Electronic signatures can be viewed from the Audit Trail Viewer.

NOTE: If you choose not to implement electronic signatures, this feature can be disabled by de-selecting this privilege from the Groups tab in User Management.

To Electronically sign an audit trail

1. Select Tools > E-Signature. The Electronic Signature dialog box appears.

2. Select a reason from the Reason for Signing drop down menu. OR Type in your own reason in the Reason for Signing dialog box. Type your Logon ID and Password in the corresponding dialog boxes.

3. If desired type in any comments in the Comment dialog box.

4. Click Apply Signature.

NOTE: If an administrator decides to apply an electronic signature to something in another user's session, the administrator can click on the check box next to Sign on Behalf of and select the user he wishes to sign for. Pyris will correctly validate the username and password of the user, and the audit trail recognizes that it was the administrator who signed.


File Versioning

Pyris Enhanced Security assigns versions to files and data objects when changes have occurred and a user performs the Save/Save As command. Version numbers are automatically generated for all files and data objects in the format filename####.ext, where # stands for the version number scheme.

A copy of each versioned file is stored in the History directory (which is a sub-directory of the directory where Pyris is installed). Meanwhile, the copy of the current file being used is saved in the directory where it resides with the format filename.ext.

The following types of files are versioned with Pyris Enhanced Security:

• Data Files

• Method Files

• Play List Files

• Configuration File (Pyris.inst)

• Calibration Files

• Report Templates


Save Preferences Page

The Save page appears when you select the Save tab in the Preferences window. The Save page contains the following fields:

Automatic Save Every

Click this box to enable the Automatic Save feature in the software. Real-time data files will automatically be saved in the time interval specified in the entry field. Type in a value or use the spin buttons to change the displayed value in one-minute increments. The default value is 30 minutes. This feature is useful for particularly long runs.

Use file name

Enter a default data file name to be used for automatic saves or if you do not enter a file name in the Save Data As field in the Method Editor. A date/time stamp in the format of YYMMDDHHMMSS (year, month, day, hour, minute, second) is appended to the file name every time it is used so data files are not overwritten. The default file name is QSAVE.XXX where XXX is the standard extension associated with the analyzer.

Activate Enhanced Security Features

Select the checkbox to activate Enhance Security and the Enable Save to Network Drive option will appear.

Enable Save to Network Drive

This checkbox will show when Enhanced Security is enabled. Select the checkbox to save data to network drives.

NOTE: A message box will appear "If the save destination is a network drive, the data files will be saved without Pyris Enhancement Security protection".

Path to Data Files

Enter the complete directory path in which to store data files. The default is C:\Program Files (x86)\PerkinElmer\Pyris\Data.

NOTE: If you upgraded an older version of Pyris Software, your data files are still available. The older default directory, C:\PE\Pyris\Data still contains the data files, unless you created another directory for the data files. You may want to move them to your new default directory, or make the old data file directory the entry here.

Path to Method Files

Enter the complete directory path in which to store method files.

The default is C:\Program Files (x86)\PerkinElmer\Pyris\Methods.

NOTE: If you upgraded an older version of Pyris Software, your method files are still available. The older default directory, C:\PE\Pyris\Methods still contains the method files, unless you created another directory for the method files. You may want to move them to your new default directory, or make the old method file directory the entry here.

Path to Player Lists

Enter the complete directory path in which to store play list files.

Save Preferences Page 29

The default is C:\Program Files (x86)\PerkinElmer\Pyris\Play Lists.

NOTE: If you upgraded an older version of Pyris Software, your play list files are still available. The older default directory, C:\PE\Pyris\Play Lists still contains the play list files, unless you created another directory for the play list files. You may want to move them to your new default directory, or make the old play list file directory the entry here.

Path to Calibration Files

Enter the complete directory in which to store calibration files. The default is C:\Program Files (x86)\PerkinElmer\Pyris\Calibrations.

Browse

Use this button to select the drive and the directory in which to save the data, method, or play list file.

Tools for Support of Validation and Compliance

Good Laboratory Practice (GLP) requirements place great emphasis on proper method development and auditing. Pyris software directly addresses this issue by providing a number of features and tools to help the integration of thermal analysis products into your quality system.

Validation and compliance tools and support features available in Pyris software are the following:

Simplified Method Development

Method generation has been simplified with the Method Editor of Pyris. Point-and-click interaction, scroll bars, spin buttons, and easy selection of options from lists of choices make method creation easier than ever. The use of pages to logically separate different portions of the method further simplifies method development. Method creation can be performed on the computer directly attached to the instrument or you can develop a method elsewhere, such as in the method development area, and then transfer it via network to the workstation at the instrument.

Raw Data and Method Storage

Raw data are permanently stored with the method used to collect it under a file name entered by the operator. The raw data and the validated method cannot be modified, with the exception of Sample ID, Operator ID, Comment, Sample Weight, and Sample Dimensions. In addition, calibration file information is stored with the data file. Because the data, method information, and calibration information cannot be modified, a reliable audit trail is available, supporting regulatory and compliance requirements. The parameters saved with the data file include:

Raw Data: Temperature, time, ordinate signal

Method: Complete method used to collect the data

Calibration: Name of the calibration file used

Method Validation

The Method Validation Stamp placed on a method indicates that it has been created under validated rules by qualified personnel (for example, the System Administrator). The stamp is transferred with the method to any work site. When data are collected using a


validated method, they are clearly “stamped” as such since the method is stored with the data. Any change made to the method (except to sample-specific information, such as weight/dimensions, sample ID, and operator ID) will automatically remove the validation mark. Lab managers can easily execute an audit trail and be assured that data were collected using a validated method, adhering to GLP and other regulatory requirements. The Validate Methods command is only available in Pyris ES, and requires users to be members of groups with permission to validate methods.

Security

Microsoft Windows operating system provides a complete security system for desktop computers (C2-level security as defined by the United States National Security Agency). This allows you to set up specific user accounts and to password-protect these accounts. In addition, the level of security protection can be defined, providing further system security.

Pyris Software Compliance

To assist you in complying with laboratory standards, Pyris software is developed under the formal requirements of the PerkinElmer Instruments Quality System. The integrity of the PerkinElmer Instruments Quality System is routinely audited and is certified by British Standards Institution as meeting the requirements of ISO 9001, the internationally recognized standard for Quality Assurance.

Troubleshooting 31

Troubleshooting

If a problem should occur while using Pyris Software, first check the Release Notes that are installed on your computer when Pyris is installed. In the Pyris Software group in the Programs menu, select Pyris Readme. The text file will be displayed in Wordpad on your screen. At the end of the notes there is information on existing known problems and workarounds. Also see the following topics:

Emergency Repair Disk Instrument Communication Long File Names

Instrument Communication

There may be an occasion when the computer loses communication with the analyzer. For example, the TAC 7/DX may be inadvertently turned off or unplugged. Should this occur, the Start button on the Control Panel will change to a Reset button:

and the Status will be listed as “Offline” or “Communications Error.”

If the status is “Offline,” check that the cables and power cords are in place and that there is power to the analyzer (and the TAC 7/DX). If the status is “Communications Error,” the problem may be caused by two applications trying to use the same communications port or by a hardware problem.

After fixing the problem, click the Reset button in the control panel to reset communications with the analyzer.

Long File Names

Pyris software supports long file names. The maximum length of the file name is 255 characters, including the drive and path name. However, some networks do not support long file names, even if you are connected to the network on a Windows workstation. The network will not allow a long file name to be saved to it, and when you begin a run, a short file name will not be generated automatically by the operating system.

If a method is set up to save the data in a long file name on a network drive, Pyris software will save the data to the root directory of the hard drive where the software resides. This is done to ensure that the data is saved properly. You can then move the data file anywhere after the run is over.

Emergency Repair Disk

The Repair Disk utility of Windows 2000 saves all the current system settings to an Emergency Repair Disk. You can then use the disk to restore your computer if files become damaged. The Repair Disk should be updated whenever there is a change in the configuration of the workstation, including adding or removing software, printer drivers, and hardware (for example, tape drive, sound card, multiport card, etc.). The ERD is usually created when Windows 2000 is installed. You can update the repair disk by running RDISK.EXE, which is located in the SYSTEM32 subdirectory of your Windows directory (usually \WINDOWS\SYSTEM32 or \WINNT35\SYSTEM32). You can also access it by going to the Windows online Help from the Start button menu and then displaying the help topic for Emergency Repair Disk or Repair Disk Utility. Both topics have hotspots to the utility.

Setting Up your Analyzer


Pyris Configuration

Before you can use Pyris Software to run experiments with your Pyris analyzers, you must configure the instruments. Configuration is dynamic, that is, when you add or remove an analyzer, you do not have to reboot the system in order for the configuration to take effect. The instrument's button is automatically added to or removed from the Pyris Manager panel.

You can run Pyris Configuration either during software installation or later, after Pyris software has been installed. You must run Pyris Configuration whenever you remove an analyzer from or add an analyzer to your system, or if you remove or add an accessory to the system.

You can open the Pyris Configuration utility by selecting Pyris Configuration in the Pyris Software folder in the Programs menu or by selecting Configure Analyzer from the Start Pyris button's Task menu. The utility must be able to detect the analyzer in order to configure it so the analyzer must be connected to the computer and powered on before you start configuration. Configuration is performed using the Pyris Configuration dialog box:

Analyzers/Ports Lists

Lists all configured analyzers and their respective COM ports (IP Address for the DSC 8500 and the DSC 8000). After you add an analyzer to your Pyris system, it appears in this list. The maximum number of analyzers permitted on a system is 10 if your computer has a multiport serial card installed. To edit or remove an analyzer, you must highlight it in this list and select the appropriate button.

Add Analyzer

Displays the Add Analyzer dialog box which is used to add an analyzer to your system’s configuration. If you already have the maximum number of analyzers permitted on your system when you select Add Analyzer, you receive an error message.

Setting Up your Analyzer 35

Edit

Displays the selected instrument's Configuration dialog box in which you can add or remove accessories or change the instrument's name. The accessories available for that particular analyzer are listed with check boxes in addition to the available purge gas accessories in a drop-down menu. Select the gas accessory from the menu and then click in the following boxes to select or deselect that accessory.

DSC 8500 Configuration DSC 8000 Configuration DSC 6000 Configuration DSC 4000 Configuration Pyris 1 TGA Configuration TGA 4000 Configuration TGA 8000 Configuration STA 8000 Configuration STA 6000 Configuration DMA 8000 Configuration Diamond DSC Configuration Jade DSC Configuration Pyris 1 DSC Configuration

Remove

Removes the highlighted analyzer from your system and the analyzer’s entry from the Analyzers list. It also frees up the associated port. A confirmation message appears before the analyzer is removed.


Add or Remove an Analyzer

Adding an Analyzer

When you add an analyzer to your system using Pyris Configuration, the system is automatically reconfigured so you do not have to close and then reboot your system in order for the change to take effect. Also, a button representing that instrument is added to the Pyris Manager panel.

1. Make sure the analyzers to be configured are installed, connected to the PC, and switched on.

2. Select Pyris Configuration from the Pyris Software menu which is displayed by clicking on the Start button, selecting Programs, and then selecting Pyris Software. OR Open the Pyris Manager and select Configure Analyzers from the Start Pyris button’s task menu.

3. Select the Add Analyzer button to add a new analyzer to the system.

4. Select the communications port where the new analyzer is connected, then select the Add button. You can configure one analyzer for each communication port on your computer. (If you have an EdgePort/4 or EdgePort/8 universal serial bus attached to your PC, COM5: refers to port 1 of the USB.)

5. Edit the analyzer name, if desired. Click on the check boxes for any accessories that are to be used, then select the OK button.

6. If you are running Pyris Enhanced Security enter in the Serial Number of the instrument in the Serial Number dialog box.

7. Repeat steps 3, 4, and 5 for each analyzer.

8. Select Close when all analyzers are configured.

Pyris Configuration is also displayed when you select Edit in the Pyris Configuration dialog box for a previously configured analyzer.

NOTE: If you are adding a DSC 8000 or DSC 8500 you must select TCPIP as the Port type and then type in the IP Address of the analyzer in the edit box that becomes enabled. You can find the IP Address for the analyzer on a sticker, located on the back of the instrument.

Removing an Analyzer

1. In the Pyris Configuration window, highlight the analyzer you wish to remove.

2. Select the Remove button.

3. You are asked if you are sure you want to remove this analyzer. By clicking on Yes, you remove the analyzer from the configuration files and the instrument's button is removed from the Pyris Manager. You do not have to physically detach the analyzer from the computer if you might need to reconfigure the analyzer back onto the system later.


Configure your Analyzer

Instrument Configuration

The instrument's Configuration dialog box is where you can add or remove accessories or change the instrument's name. The accessories available for that particular analyzer are listed with check boxes in addition to the available purge gas accessories in a drop-down menu. Select the gas accessory from the menu and then click in the following boxes to select or deselect that accessory.

Click on a link to see more details of the configuration for each instrument: DSC 8500 Configuration DSC 8000 Configuration DSC 6000 Configuration DSC 4000 Configuration Pyris 1 TGA Configuration TGA 4000 Configuration TGA 8000 Configuration STA 8000 Configuration STA 6000 Configuration DMA 8000 Configuration Diamond DSC Configuration Jade DSC Configuration Pyris 1 DSC Configuration


DSC 8500 Instrument Configuration

The DSC 8500 Configuration dialog box appears when you select the Edit button in the Pyris Configuration dialog box when the DSC 8500 analyzer is highlighted in the Analyzers list. It is also displayed when there is a DSC 8500 attached to the computer and it is detected by the Pyris software when you select the Add button on the Add Analyzer dialog box. The analyzer must be switched on when you configure it into the system; otherwise, it will not be recognized when you select the Add button. This topic provides you with a description of each field on the DSC 8500 Configuration dialog box.

NOTE: If you are adding a DSC 8500 you must select TCPIP as the Port type. An edit box is then enabled on the Add Analyzer dialog box. Type the IP Address of the analyzer in the edit box; you can find the address for the analyzer on a sticker located on the back of the instrument.

Analyzer Name

If you are adding a DSC 8500 the system will display a default name in this field. Type the name you wish to assign to the analyzer, using a maximum of eight characters. The name identifies the analyzer in Pyris Software; it also appears in the Instrument button on the Pyris Manager panel and in the title bar of the Instrument Application.

Serial Number

You can enter the serial number of the analyzer for further identification; it is not a required entry.

NOTE: If you are running Pyris Enhanced Security you must type in the serial number of the analyzer.


IP Address (or host name)

Displays the Ethernet address for the analyzer. This is the IP address that you entered on the Add Analyzer dialog box. The IP address for the analyzer is displayed on a sticker on the back of the instrument.

Port Number

Displays the port number for the analyzer.

Accessories

This section lists the available accessories for the analyzer. For the DSC 8500, the following accessories are available:

Cooling Accessory

Select the cooling accessory you are using from the drop down list. Available choices are: None, Intracooler 2, Intracooler 3, and CLN2.

Autosampler

Check this option if you have an autosampler installed. You can test the configuration by clicking the Test button. The message “An autosampler was found” should be displayed if the autosampler is connected properly.

Check the Dust Cover Interlock option if you want the autosampler to pause when the cover is raised. We recommend that you use this option to prevent access to the autosampler during operation.

Purge Gas

Use the Purge Gas A drop down menu to select a purge gas. You can select a second purge gas from the Purge Gas B drop down menu.

High Pressure Cell

Check this option if you have a High Pressure Cell installed.

Photo Calorimeter

Check this option if you have a Photo Calorimeter installed.

Flow-Through Cover

Check this option if you have a Flow-Through Cover installed.

Firmware Version

Click the Firmware Version button to display the version of firmware in the analyzer.


DSC 8000 Instrument Configuration

The DSC 8000 Configuration dialog box appears when you select the Edit button in the Pyris Configuration dialog box when the DSC 8000 analyzer is highlighted in the Analyzers list. It is also displayed when there is a DSC 8000 attached to the computer and it is detected by the Pyris software when you select the Add button on the Add Analyzer dialog box. The analyzer must be switched on when you configure it into the system; otherwise, it will not be recognized when you select the Add button. The fields in this dialog box are as follows:

NOTE: If you are adding a DSC 8000 you must select TCPIP as the Port type. An edit box is then enabled on the Add Analyzer dialog box. Type the IP Address of the analyzer in the edit box; you can find the address for the analyzer on a sticker located on the back of the instrument.

Analyzer

Name

If you are adding a DSC 8000 the system will display a default name in this field. Type the name you wish to assign to the analyzer, using a maximum of eight characters. The name identifies the analyzer in Pyris Software; it also appears in the Instrument button on the Pyris Manager panel and in the title bar of the Instrument Application.

Serial Number




IP Address (or host name)

Displays the Ethernet address for the analyzer. This is the IP address that you entered on the Add Analyzer dialog box. The IP address for the analyzer is displayed on a sticker on the back of the instrument.

Port Number

Displays the port number for the analyzer.

Accessories

On the Configuration dialog box this section lists the available accessories for the analyzer. For the DSC 8000 the following accessories are available:

Cooling Accessory

Select the cooling accessory you are using from the drop down list. Available choices are: None, Intracooler 2, Intracooler 3, and CLN2.

Autosampler

Check this option if you have an autosampler installed. You can test the configuration by clicking on the Test button. The message "An autosampler was found" should be displayed if the autosampler is connected properly.

Check the Dust Cover Interlock option if you want the autosampler to pause when the cover is raised. We recommend that you use this option to prevent access to the autosampler during operation.

Purge Gas

Use the Purge Gas A drop down menu to select a purge gas. You can select a second purge gas from the Purge Gas B drop down menu.

High Pressure Cell

Check this option if you have a High Pressure Cell installed.

Photo Calorimeter

Check this option if you have a Photo Calorimeter installed.

Flow-Through Cover

Check this option if you have a Flow-Through Cover installed.

Firmware Version



DSC 6000 Configuration

The DSC 6000 Configuration dialog box appears when you select the Edit button in the Pyris Configuration dialog box when the DSC 6000 analyzer is highlighted in the Analyzers list. It is also displayed when there is a DSC 6000 attached to the computer and it is detected by the Pyris software when you click the Add button on the Add Analyzer dialog box. The analyzer must be switched on when you configure it into the system; otherwise, it will not be recognized when you click the Add button. The fields in this dialog box are as follows:

Name

If you are adding a DSC 6000, the system will display a default name in this field. Type the name you wish to assign to the analyzer, using a maximum of eight characters. The name identifies the analyzer in Pyris Software; it also appears in the Instrument button on the Pyris Manager panel and in the title bar of the Instrument Application.

Port

Displays the COM port to which the analyzer is attached and that you selected in the Add Analyzer dialog box.

Serial Number

Displays the serial number of the analyzer.

Accessories

Lists the available accessories for the analyzer. For the DSC 6000, the following accessories are available:

• Integrated Gas Selector

• CryoFill - Select this option if your DSC 6000 was installed with CryoFill.

• Autosampler - Select this option if you have an autosampler installed on your DSC 6000. The COM Port for the autosampler is the same as that for the analyzer.


You can test the configuration by clicking the Test button. The message “An autosampler was found” should be displayed if the autosampler is connected properly.

Firmware Version



DSC 4000 Configuration

The DSC 4000 Configuration dialog box appears when you click the Edit button in the Pyris Configuration dialog box when the DSC 4000 analyzer is highlighted in the Analyzers list. It is also displayed when there is a DSC 4000 attached to the computer and it is detected by the Pyris software when you select the Add button on the Add Analyzer dialog box. The analyzer must be switched on when you configure it into the system; otherwise, it will not be recognized when you click the Add button. The fields in this dialog box are as follows:

Name

If you are adding a DSC 4000, the system will display a default name in this field. Type the name you wish to assign to the analyzer, using a maximum of eight characters. The name identifies the analyzer in Pyris Software; it also appears in the Instrument button on the Pyris Manager panel and in the title bar of the Instrument Application.

Port


Serial Number


Accessories

Lists the available accessories for the analyzer. For the DSC 4000 the following accessories are available:


• Autosampler - Check this option if you have an autosampler installed on your DSC 4000. The COM Port for the autosampler is the same as that for the analyzer. You can test the configuration by clicking on the Test button. The message “An autosampler was found” should be displayed if the autosampler is connected properly.


Firmware Version



Pyris 1 TGA Configuration

The Pyris 1 TGA Configuration dialog box appears when you select the Edit button in the Pyris Configuration dialog box when the Pyris 1 TGA analyzer is highlighted in the Analyzers list. It is also displayed when there is a Pyris 1 TGA attached to the computer and it is detected by the Pyris software when you click the Add button on the Add Analyzer dialog box. The analyzer must be switched on when you configure it into the system; otherwise, it will not be recognized when you click the Add button. The fields in this dialog box are as follows:

Name

If you are adding a Pyris 1 TGA, the system will display a default name in this field. Type the name you wish to assign to the analyzer, using a maximum of eight characters. The name identifies the analyzer in Pyris Software; it also appears in the Instrument button on the Pyris Manager panel and in the title bar of the Instrument Application.

Port


Serial Number


Accessories

Lists the available accessories for the analyzer. For the Pyris 1 TGA, the following accessories are available:

• Cooling Jacket Accessory


• Accupick

• Autosampler - Select this option if you have an autosampler installed on your Pyris 1 TGA. The COM Port for the autosampler is the same as that for the analyzer. You can test the configuration by clicking the Test button. The message “An autosampler was found” should be displayed if the autosampler is connected properly.

Firmware Version



TGA 4000 Configuration

The TGA 4000 Configuration dialog box appears when you select the Edit button in the Pyris Configuration dialog box when the TGA 4000 analyzer is highlighted in the Analyzers list. It is also displayed when there is a TGA 4000 attached to the computer and it is detected by the Pyris software when you select the Add button in the Add Analyzer dialog box. The analyzer must be switched on when you configure it into the system; otherwise, it will not be recognized when you select the Add button. The fields in this dialog box are as follows:

Name

If you are adding a TGA 4000, the system will display a default name in this field. Type the name you wish to assign to the analyzer, using a maximum of eight characters. The name identifies the analyzer in Pyris Software; it also appears in the Instrument button on the Pyris Manager panel and in the title bar of the Instrument Application.

Port


Serial Number Displays the serial number of the analyzer.

Accessories

Lists the available accessories for the analyzer.

• Autosampler - Check this option if you have an autosampler installed on your analyzer.

• The COM port for the autosampler is the same as that for the analyzer. Test the configuration by clicking the Test button. The message "An autosampler was found" should be displayed if the autosampler is connected properly.


Firmware Version

Displays the version of firmware in the analyzer.


TGA 8000 Configuration

The TGA 8000 Configuration dialog box appears when you select the Edit button in the Pyris Configuration dialog box when the TGA 8000 analyzer is highlighted in the Analyzers list. It is also displayed when there is a TGA 8000 attached to the computer and it is detected by the Pyris software when you select the Add button on the Add Analyzer dialog box. The analyzer must be powered on when you configure it into the system; otherwise, it will not be recognized when you select the Add button. The fields in this dialog box are as follows:

Name

If you are adding a TGA 8000, the system will display a default name in this field. Type the name you wish to assign to the analyzer, using a maximum of eight characters. The name identifies the analyzer in Pyris Software for Windows; it also appears in the Instrument button on the Pyris Manager panel and in the title bar of the Instrument Application.

Port


Serial Number



Accessories

Lists the available accessories for the analyzer.

Remote Control

• Check Enable if you wish to control the TGA 8000 via an iPad or iPhone.


• Use the Maximum Clients spin box to select how many mobile devices can connect to the TGA 8000.

For more information on the mobile application for controlling the TGA 8000 see Configuring Remote Control of the TGA 8000 with a Mobile device on page 53.

Firmware Version

Click on the Firmware Version button to display the version of firmware in the analyzer.

Configuring Remote Control of the TGA 8000 with a Mobile Device

You use the Remote Control dialog to define which mobile devices can connect to the TGA 8000.

To access the Remote Control dialog select Tools > Remote Control... from the TGA 8000 Instrument Application.

Using the Remote Control dialog to define which mobile devices can control the TGA 8000 Note: In order to control the TGA 8000 with a mobile device you must first download the

Pyris Application for iPhone/iPad from the Apple Store onto your mobile device.

On the mobile device that will be controlling the TGA 8000

1. Install the Pyris App for iPhone/iPad onto your mobile device.

2. Open the Pyris App and enter the IP of the computer connected to the TGA 8000. You can find the IP Address of the TGA 8000 by opening Pyris on your computer selecting Tools > Remote Control. The IP Address is displayed in the Local IP field as shown below:


3. Test connection on mobile device and click Done. The mobile device now appears in the Clients table on the Remote Control dialog in Pyris.

From the Remote Control Dialog in Pyris

1. You can prohibit a specific mobile device by clicking on the device listed in the Clients table and then clicking Refuse.

2. Click Start to allow remote control of the TGA 8000.

3. Click Stop on the Remote Control dialog if you do not want any mobile device to control the instrument.


STA 8000 Configuration

To display the STA 8000 Configuration dialog box:

1. Ensure that the STA 8000 is connected to the computer and switched on.

2. Click the Start Pyris button in the corner of the screen.

3. Click Configure Analyzer.

4. If the STA 8000 is being connected to the computer for the first time, click Add Analyzer. Otherwise, highlight the STA 8000 in the list of connected instruments and click Edit.

The fields in this dialog box are as follows:

Name

If you are adding an STA 8000, the system will display a default name in this field. Type the name you wish to assign to the analyzer, using a maximum of eight characters. The name identifies the analyzer in the Pyris software; it also appears in the Instrument button on the Pyris Manager panel and in the title bar of the Instrument Application.

Port


Serial Number


NOTE: If you are running Pyris Enhanced Security, you must type in the serial number of the analyzer.

Accessories

Lists the available accessories for the analyzer. For the STA 8000, only the integrated gas selector is currently available.


Purge Gas

• Purge Gas A – Specify the identity of Purge Gas A.

• Purge Gas B – Specify the identity of Purge Gas B.

Firmware Version



STA 6000 Configuration

To display the STA 6000 Configuration dialog box:

1. Ensure that the STA 6000 is connected to the computer and switched on.

2. Click on the Start Pyris button in the corner of the screen.

3. Select Configure Analyzer.

4. If the STA 6000 is being connected to the computer for the first time, select Add Analyzer. Otherwise, highlight the STA 6000 in the list of connected instruments and select Edit.


Name

If you are adding an STA 6000, the system will display a default name in this field. Type the name you wish to assign to the analyzer, using a maximum of eight characters. The name identifies the analyzer in the Pyris Software; it also appears in the Instrument button on the Pyris Manager panel and in the title bar of the Instrument Application.

Port


Serial Number


Accessories

Lists the available accessories for the analyzer. For the STA 6000 the following accessories are available:



• Autosampler - Check this option if you have an autosampler installed on your analyzer. The COM Port for the autosampler is the same as that for the analyzer. You can test the configuration by clicking the Test button. The message "An autosampler was found" should be displayed if the autosampler is connected properly.

Purge Gas

• Purge Gas A - Specify Purge Gas A.

• Purge Gas B - Specify Purge Gas B.

Firmware Version



DMA 8000 Configuration

To configure the DMA 8000 when connecting to it for the first time:

1. Ensure that the DMA 8000 is connected to the computer and switched on.

2. Click the Start Pyris button in the corner of the screen.

3. Click Configure Analyzer.

4. Click Add Analyzer.

5. Select the first of the two COM ports used by the DMA 8000, and click Add. These COM port numbers can be found in the Device Manager, accessed from the Control Panel in Microsoft Windows. Select Administrative Tools > Computer Management > Device Manager. Pyris will connect to the DMA 8000 and display the Configuration dialog box.

NOTE: Refer to Connecting the System Components in the DMA 8000 Hardware Help for full details of how to set up the COM ports needed by the instrument.


Name

If you are adding a DMA 8000, the system will display a default name in this field. Type the name you wish to assign to the analyzer, using a maximum of eight characters. The name identifies the analyzer in the Pyris software; it also appears in the Instrument button on the Pyris Manager panel and in the title bar of the Instrument Application.

Port

Displays the COM ports to which the analyzer is attached. The first is the port that you selected when you first connected to the instrument, and the second is a virtual COM port used by the system.

Serial Number

The serial number of the analyzer is displayed for further identification.


Oven

Lists the available oven types for the analyzer: Standard Air Oven (with or without the high temperature option), Bath (Dry) or Bath (Wet). You can select which oven you are using with your analyzer. This setting has no effect on the software; it is for information only.

NOTE: Once you have connected to the DMA 8000, the software will warn you that there is no calibration (*.dm8c) file available. It will then find the calibration file stored on the DMA 8000 (which contains the serial number in its filename), and import it as a default calibration file to allow the instrument to be controlled.


Diamond DSC Configuration

The Diamond DSC Configuration dialog box appears when you select the Edit button in the Pyris Configuration dialog box when the Diamond DSC analyzer is highlighted in the Analyzers list. It is also displayed when there is a Diamond DSC attached to the computer and it is detected by the Pyris software when you select the Add button in the Add Analyzer dialog box. The analyzer must be switched on when you configure it into the system or it will not be recognized when you select the Add button. The fields in this dialog box are as follows:

Name

If you are adding a new Diamond DSC, the system will display a default name in this field. Type the name you wish to assign to the analyzer, using a maximum of eight characters. The name identifies the analyzer in the Pyris Software; it also appears in the Instrument button on the Pyris Manager panel and in the title bar of the Instrument Application.

Port


Serial Number


Accessories

Lists the available accessories for the Diamond DSC. The first selection is for the purge gas accessory. Click on the drop-down arrow to display the available choices:

• Thermal Analysis Gas Station (TAGS): Select this accessory if a TAGS is attached to your analyzer. The TAGS can control up to 4 purge gases. Selection of this accessory is reflected in the Gas Change box on the Program page of the Method Editor. The gas program can have the TAGS switch from one gas to another at selected times or temperatures. The flow rate can also be changed.

• GSA 7 Gas Switching Accessory: Select this accessory if you are using a GSA 7. Selection of this accessory is reflected in the Gas Change box on the Program page of the Method Editor. The gas program can have the GSA 7 switch the purge gas at a selected time.

• No Gas Accessory

The next four accessories are:

• CryoFill: Click the box if your Diamond DSC is attached to the CryoFill LN2 Cooling System for subambient operation.

• High-Pressure Cell: Select this accessory if you are going to use the high-pressure cell on the Diamond DSC.

• Autosampler: Select this accessory if the Diamond DSC Autosampler is installed on your analyzer. If you connected the autosampler directly into the COM1 or COM2 port on the computer instead of to the Autosampler port on the Diamond DSC, indicate that port in the Port field. Test the configuration by clicking the Test button. The message


“An autosampler was found” should be displayed if the autosampler is connected properly.

Firmware Version


Update Flash EPROM

Select this button when you want to update the EPROM in the analyzer. This would occur if you receive an updated version of the software. Clicking on the button displays the Pyris Flash ROM Utility dialog box in which you select the ROM file to use for updating the Pyris EPROM. Data are then transferred from the file to the analyzer’s memory.

NOTE: Do not update the firmware at the same time that you add the analyzer to the configuration list. If you need to add the analyzer and update the firmware, first add the analyzer and close the Configuration dialog box. Then reopen the Pyris Configuration dialog box, highlight Diamond DSC's name, and click the Edit button. Click Update Flash EPROM.


Jade DSC Configuration

The Jade DSC Configuration dialog box appears when you select the Edit button in the Pyris Configuration dialog box when the Jade DSC analyzer is highlighted in the Analyzers list. It is also displayed when there is a Jade DSC attached to the computer and it is detected by the Pyris software when you select the Add button on the Add Analyzer dialog box. The analyzer must be switched on when you configure it into the system; otherwise, it will not be recognized when you select the Add button. The fields in this dialog box are as follows:

Name

If you are adding a Jade DSC, the system will display a default name in this field. Type the name you wish to assign to the analyzer, using a maximum of eight characters. The name identifies the analyzer in Pyris Software; it also appears in the Instrument button on the Pyris Manager panel and in the title bar of the Instrument Application.

Port


Serial Number



Accessories

Lists the available accessories for the analyzer. For the Jade DSC the following accessories are available:


• CryoFill - Check this option if your Jade DSC was installed with CryoFill.


• Autosampler - Check this option if you have an Autosampler installed on your Jade DSC. The COM Port for the autosampler is the same as that for the analyzer. You can test the configuration by clicking on the Test button. The message “An autosampler was found” should be displayed if the autosampler is connected properly.

Firmware Version

Click on the Firmware Version button to display the version of firmware in the analyzer.


Pyris 1 DSC Configuration

The Pyris 1 DSC Configuration dialog box appears when you select the Edit button in the Pyris Configuration dialog box when the Pyris 1 DSC analyzer is highlighted in the Analyzers list. It is also displayed when there is a Pyris 1 DSC attached to the computer and it is detected by the Pyris software when you select the Add button in the Add Analyzer dialog box. The analyzer must be switched on when you configure it into the system or it will not be recognized when you select the Add button. The fields in this dialog box are as follows:

Name

If you are adding a new Pyris 1 DSC, the system will display a default name in this field. Type the name you wish to assign to the analyzer, using a maximum of eight characters. The name identifies the analyzer in Pyris Software; it also appears in the Instrument button on the Pyris Manager panel and in the title bar of the Instrument Application.

Port


Serial Number



Accessories Lists the available accessories for the Pyris 1 DSC. The first selection is for the purge gas accessory. Click on the drop-down arrow to display the available choices:

• Thermal Analysis Gas Station (TAGS): Select this accessory if a TAGS is attached to your analyzer. The TAGS can control up to 4 purge gases. Selection of this accessory is reflected in the Gas Change box on the Program page of the Method Editor. The gas program can have the TAGS switch from one gas to another at selected times or temperatures. The flow rate can also be changed.

• GSA 7 Gas Switching Accessory: Select this accessory if you are using a GSA 7. Selection of this accessory is reflected in the Gas Change box on the Program page of the Method Editor. The gas program can have the GSA 7 switch the purge gas at a selected time.

• No Gas Accessory

The next four accessories are:

• CryoFill: Click in the box if your Pyris 1 DSC is attached to the CryoFill LN2 Cooling System for subambient operation.

• DPA 7 Photocalorimetric Accessory: This selection is grayed out because the accessory is not available for use with the Pyris 1 DSC at this time.

• High-Pressure Cell: Select this accessory if you are going to use the high-pressure cell on the Pyris 1 DSC.


• Autosampler: Select this accessory if the Pyris 1 DSC Autosampler is installed on your analyzer. If you connected the autosampler directly into the COM1 or COM2 port on the computer instead of to the Autosampler port on the Pyris 1 DSC, indicate that port in the Port field. Test the configuration by clicking on the Test button. The message “An autosampler was found” should be displayed if the autosampler is connected properly.

Firmware Version


Update Flash EPROM

Select this button when you want to update the EPROM in the analyzer. This would occur if you receive an updated version of the software. Clicking on the button displays the Pyris Flash ROM Utility dialog box in which you select the ROM file to use for updating the Pyris EPROM. Data are then transferred from the file to the analyzer’s memory.

NOTE: Do not update the firmware at the same time that you add the analyzer to the configuration list. If you need to add the analyzer and update the firmware, first add the analyzer and close the Configuration dialog box. Then reopen the Pyris Configuration dialog box, highlight Pyris 1 DSC's name, and click on the Edit button. Click on Update Flash EPROM.


Setting Preferences

Preferences

You can change the default values for many functions in Pyris software by using the Preferences item on the Tools menu. Preferences is available on the Tools menu in Instrument Application and Data Analysis Application. Each Preferences window contains nine tabbed pages when opened in Instrument Viewer and four tabbed pages when opened in Data Analysis:

Instrument

Instrument-specific default values are set using the Instrument page.

Analyzer Constants

For all analyzers, enter the default Load Temperature and Go To Temp Rate to be used for all methods. For DSCs, enter the maximum temperature allowed. For example, set the maximum temperature to 600 °C to eliminate the chance of melting aluminum in the sample holder. For the DMA 8000, the Load Strain and Load Frequency parameters are set here.

Data

Depending on the type of experiments you run, for the DSC 8000/8500 you can select either a low or a high range for the maximum ordinate value. For the Pyris 1 TGA, there is an additional ultrasensitive range for the Y data. For some analyzers, you can specify the Ordinate Filter Factor for data smoothing. The DSC 4000, DSC 6000, Jade DSC, and TGA 4000 allow you to set the Display Language and Furnace Constant, and the DSC 4000, DSC 6000 and Jade DSC also include a Heat Flow Conversion parameter. The DMA 8000 has additional parameters such as Poisson's Ratio and Broken Sample Threshold.

Environment

Select from the drop-down list the cooling device you are using with the analyzer. For certain DSC analyzers, specify whether you are using helium purge or liquid nitrogen for cooling. It is essential that these settings accurately depict the system in use. Data may be affected by inaccurate settings.

General

In all graphical windows (all Data Analysis windows, the Instrument Viewer, and the Monitor), you can display up to four Y-axes. Curves associated with each Y axis are displayed in a specific line type. Use the General page to assign a line type to each of the four Y-axes and to curves whose Y-axes are not shown. In the General page you also select whether you want tooltips to be activated.

Colors

You can specify the colors to be used in all graphical windows (all Data Analysis windows, the Instrument Viewer, and the Monitor) on the Color page. Specify the color of the first 12 data files displayed, the grid, and the background.

Graph

You can specify the title to appear in graphical windows and printouts and the font, type size, and type style to be used for all annotations in graphical windows in the Graph page. Auto-Rescale


When the Full Scale functions are selected in the Rescale Tools toolbar, the X-axis and Y-axis scales change so that all of the data can be displayed. White space can be automatically placed between the curves and each side of the graphical area by using the Auto-Rescale settings. The amount of white space is determined as a percentage of the full range of the displayed data; that percentage is specified in the Graph page. A percentage of zero causes the curves to touch the axes.

Save

You can specify the time between automatic saves in the Save page. Autosave is for real-time data only. You can also specify a default file name for data collected during sample runs. If you do not specify a file name in the Save Data As field in your method, the data collected during the run will be saved as the file specified here.

Specify the default directory paths for data, method, play list, and calibration files. Unless you specify otherwise, files will be saved in the directories entered here. System Administrators (as identified by the Windows user name and password) can select the box Data Files are in a Secure Directory. The files placed in this directory will be designated as read-only files for all other users, except the Administrator.

Real-Time Curves

In the Real-Time Curves page you select the real-time curve types to be displayed in Instrument Viewer. You can select up to four curves. The selections displayed in the drop-down list for each curve depend on the instrument. You also can select the X-axis to display at the start of a run: time or temperature.

Remote Access

The Remote Access page is used to set the level of access of remote PCs to monitor the analyzers running on your PC.

When the optional Remote Monitor software is installed, users at remote PCs can monitor the status of analyzers running on another PC (connected via a network). The PC that is running the analyzers can limit the level of access that any remote PC can have to its analyzers. Access levels are:

• No Access: forbids any other PC to monitor the status of analyzers running on this PC.

• Status Panel: allows other PCs to monitor via the status panel the status of analyzers running on this PC, but a run cannot be stopped from a remote PC.

• Stop Run and Status Panel: allows other PCs to monitor the status of analyzers running on this PC, and allows a run to be stopped from a remote PC.

Purge Gas

You can specify the purge gas connected to the purge gas inlet of the analyzer or the gases attached to the gas switching accessory by the entries made in the Purge Gas page. The selection made here appears in the Initial State page in the method as the default purge gas. It can be changed in the control panel. You can also enter the initial flow rate of the purge gas.

Autosampler

If your analyzer has an autosampler, this page is used to set the sample temperature range in which the autosampler can safely load and unload a sample. The setpoint value is the temperature to which the analyzer will be programmed if the sample temperature is not within the minimum and maximum temperature range. When the program temperature is


equal to the setpoint and the sample temperature is +5 °C of the program temperature, the operation will proceed. Number of retries and initial checking apply in some cases.


General Preferences Page

The General page appears when you select the General tab in the Preferences window. The General page contains the following fields:

Line Types

You can select the line type to be used for displaying up to four curves and then select a line type for each of those curves whose axes are not shown. Display the selection of line types by clicking on the down arrow for the drop-down list. The order of display for the Y-axes is as follows:

1. Y1 axis left inside axis

2. Y2 axis right inside axis

3. Y3 axis left outside axis

4. Y4 axis right outside axis

Tooltips

Tooltips are the familiar text displays that popup when your cursor moves over a specific area of the screen such as a toolbar button or field in a screen. The tooltip's text can be short or a more descriptive long version. You may also turn tooltips off altogether.

DMA Reports

Indicates how you want the DMA data displayed and reported: as force (mN) or stress (Pa).

Use Relay Box

If you have a relay box as an external device, select the check box to have the Pyris software search for an external device connection. When a connection is establish, you can use the Methods Plus or Valet to trigger an external event.

Configure X10

An X10 device is used to trigger a signal that can turn an external device on or off. It is often used in conjunction with an Intracooler. The settings for the X10 must be entered on the General Preferences page in the section shown below.

There are two dials on the X10 front panel. One dial sets the House Code and the other dial sets the Device Code.

COM Port: Enter the communications port used for the X10.

House Code: Enter the letter set on the dial.


Device Code: Enter the number set on the dial.

After entering the two codes, click Add. You can then select the X10 device in the drop-down list. Once you have selected the X10 device, it can be used in Methods Plus or Valet to trigger an external event.

To remove the X10 device, you must re-enter the codes, then click Remove.

After you have completed the instrument preferences, click OK to accept the selections made. Click Cancel to end the Preferences window and any selections made will be not be saved.


Color Preferences Page

The Colors page appears when you select the Colors tab in the Preferences window. The Colors page contains the following fields:

Set Color For

Displays the colors for graphical window components, including the background, grid, and the first 12 curves displayed. Select an item in the list and then select a color in the Colors box.

Colors

Displays all the possible colors that can be assigned to the graphical window components listed in the Set Color For list box. The color assigned to the currently selected item in the list is displayed in a double box.

Color Options

The choices for color handling are offered as the following:

1. Use one color per File

2. Use one color per curve Each curve displayed on the screen will be given the next color identified in the list box. This list will be followed regardless of the file that the new curve is generated from.

3. Use Color 1 for Heating segments The choice is offered to use the first three colors for heating segments, cooling segments and isothermal segments. This may not have the desired effect when used for data from some TMA and DMA modes. If this item is chosen, Colors 4 through 12 will be used, as in case 2 when curves are more than one segment.

These options are followed when new curves are created. Curves are created by the following actions:

• Selection of a curve type from the Curves menu. This applies to both Runtime and post-run.

• Execution of a calculation that generates a curve. This includes, but is not limited to, Derivative, Specific Heat (any variety – 1,2,3 curve or StepScan)

• Advanced Calculations do not necessarily follow these rules.

NOTE: When File > New Data, File > Open Data, and File > Add Data are selected, the curves are displayed in the color saved with the curve.

• This bypasses the color list and uses the color that each curve had when it was saved.

NOTE: Background and Grid colors are used based on the colors identified in the list, regardless of the choice of scheme. These are not saved with the data.

Graph Preferences Page

The Graph page appears when you select the Graph tab in the Preferences window. The Graph page contains the following fields: Title


Enter the title that will appear on your printouts if you check in the Include Title box in the Page Setup dialog box. The default title is "PerkinElmer Thermal Analysis."

Font

Displays the Font dialog box. Below the button are the name of the selected font, the font size, and an example.

User Logo Setup

Displays the complete directory path of the Logo file.

Print At

Prints the logo at a specified location on an 8.5 x 11 paper.

Save Preferences Page

The Save page appears when you select the Save tab in the Preferences window. The Save page contains the following fields:

Automatic Save Every

Click this box to enable the Automatic Save feature in the software. Real-time data files will automatically be saved in the time interval specified in the entry field. Type in a value or use the spin buttons to change the displayed value in one-minute increments. The default value is 30 minutes. This feature is useful for particularly long runs.

Use file name

Enter a default data file name to be used for automatic saves or if you do not enter a file name in the Save Data As field in the Method Editor. A date/time stamp in the format of YYMMDDHHMMSS (year, month, day, hour, minute, second) is appended to the file name every time it is used so data files are not overwritten. The default file name is QSAVE.XXX where XXX is the standard extension associated with the analyzer.

Activate Enhanced Security Features

Select the checkbox to activate Enhance Security and the Enable Save to Network Drive option will appear.

Enable Save to Network Drive

This checkbox will show when Enhanced Security is enabled. Select the checkbox to save data to network drives.

NOTE: A message box will appear "If the save destination is a network drive, the data files will be saved without Pyris Enhancement Security protection".

Path to Data Files

Enter the complete directory path in which to store data files. The default is C:\Program Files (x86)\PerkinElmer\Pyris\Data.

NOTE: If you upgraded an older version of Pyris Software, your data files are still available. The older default directory, C:\PE\Pyris\Data still contains the data files, unless you created another directory for the data files. You may want to move them to your new default directory, or make the old data file directory the entry here.


Path to Method Files

Enter the complete directory path in which to store method files.

The default is C:\Program Files (x86)\PerkinElmer\Pyris\Methods.

NOTE: If you upgraded an older version of Pyris Software, your method files are still available. The older default directory, C:\PE\Pyris\Methods still contains the method files, unless you created another directory for the method files. You may want to move them to your new default directory, or make the old method file directory the entry here.

Path to Player Lists

Enter the complete directory path in which to store play list files.

The default is C:\Program Files (x86)\PerkinElmer\Pyris\Play Lists.

NOTE: If you upgraded an older version of Pyris Software, your play list files are still available. The older default directory, C:\PE\Pyris\Play Lists still contains the play list files, unless you created another directory for the play list files. You may want to move them to your new default directory, or make the old play list file directory the entry here.

Path to Calibration Files

Enter the complete directory in which to store calibration files. The default is C:\Program Files (x86)\PerkinElmer\Pyris\Calibrations.

Browse

Use this button to select the drive and the directory in which to save the data, method, or play list file.

Real-Time Curves Preferences Page

The Real-Time Curves page appears when you select the Real-Time Curves tab in the Preferences window. The Real-Time Curves page contains the following fields:

Curve #1

Select the default curve type for the first real-time curve displayed. The available curve types are the same as listed on the Curves menu for each analyzer.

Curve #2

Select the default curve type for the second real-time curve displayed. The available curve types are the same as listed on the Curves menu, minus the curve selected for Curve #1.

Curve #3

Select the default curve type for the third real-time curve displayed.

Curve #4

Select the default curve type for the fourth real-time curve displayed.


X-Axis Displayed at Start of Run

Select Sample Temperature or Time as your X-axis display in the Instrument Viewer as the run starts. You can change the X-axis using Rescale X during the run.

At Start of Each Run

If you change the types of curves displayed while in Instrument Viewer and/or the X-axis, you can have the software use those settings for subsequent runs instead of changing them back to those set in this Preferences page. Click in the radio button next to Use Current Settings. If you always want the Preferences page settings used at the start of each run, select Use Settings Shown Here.

Remote Access Preferences Page

The Remote Access page appears when you select the Remote Access tab in the Preferences window. You must have the optional Remote Monitor software installed on your computer in order to see this tab.

The Remote Access page is used to set permission for others on a network to access your computer and analyzers. There are three permission levels:

No Access

Forbids any other PC from accessing the analyzers running on your PC.

Status Panel and Curve Display only

Allows other PCs on the network to monitor the status of the analyzers running on your PC and displays the Instrument Viewer screen for the remote analyzer.

Stop Run, Status Panel, and Curve Display

Allows other PCs on the network to monitor the status of and stop a run on the analyzers running on your PC and displays the Instrument Viewer screen for the remote analyzer.

Purge Gas Preferences Page

The Purge Gas page appears when you select the Purge Gas tab in the Preferences window. Use this page to select the purge gas connected to each available port on the analyzer or gas switching accessory attached to the analyzer. The gas switching accessory must be configured into the system during Configuration in order for the correct number of gas ports to be displayed on this page. If no accessory is configured, only Gas A will be displayed. The DSC 4000, DSC 6000, Jade DSC, TGA 4000, STA 6000 and STA 8000 each have two gases.

If a gas box type GSA 7 or Air Cooling Unit is being used, then there are two purge gas ports: Gas A and Gas B. A TAGS attached to your thermal system provides four purge gas ports. The entries made on this page are displayed in the Initial State page of the Method Editor and at the bottom of the control panel.

Gas A

Select the purge gas attached to the Gas A port of your analyzer, GSA 7, or TAGS from the drop-down list. If you change the purge gas attached to the port, you must update the entry here. It is important that these settings reflect the actual system. Data may be affected by inaccurate information.


Initial Flow Rate

Enter the initial flow rate by typing in the value or using the spin buttons. This value is displayed on the Initial State page of the Method Editor and at the bottom of the control panel.

Autosampler Preferences Page

The Autosampler page appears when you select the Autosampler tab in the Preferences window. This page is included in the Preferences window if the analyzer has an autosampler.

Autosampler Load Range

This section defines the temperature at which samples will be allowed to load or unload. If the current sample temperature is outside of the range defined by the Minimum Temperature and Maximum Temperature values, for any autosampler operation, whether it is in a play list or not, the analyzer will be programmed to the Temperature Setpoint (the Temperature Setpoint must fall between the Maximum and Minimum Temperatures) before the operation is allowed to proceed. The Maximum Temperature should be at least 10 °C greater than the Minimum Temperature. The Go To Temp rate is used to go to the Temperature Setpoint. The program temperature must be equal to the Temperature Setpoint and the sample temperature must be within 5 °C of the program temperature in order to proceed. All autosamplers are allowed to operate at the analyzer temperature limits.

Environment Tab Page

The Environment tab page is available when using the DSC 8500 and the DSC 8000. From this page, you define the purge gas that is connected to each available port on the analyzer or gas switching accessory as well as defining the cooling device you are using. You can also use this page to set a threshold that determines when Pyris notifies you to check the purge gas.

The entries made on this page are displayed on the Initial State page of the Method Editor and at the bottom of the control panel.

NOTE: When you switch gases during a run, Pyris will switch the gas back to the gas A setting defined on this page, at the end of a run.

NOTE: Whenever you select a Purge Gas and/or Cooling Device in Configuration, this screen is updated with your selections. In turn, whenever you make changes to your Purge Gas Settings and/or Cooling Device selection in Preferences, the DSC 8500 or DSC 8000 Configuration screen is automatically updated.


Purge Gas Settings

Gas A

Use the drop down list to select the gas that is attached to the Gas A port on the analyzer.

Initial Flow Rate for Gas A

Enter the initial flow rate by typing in the value or using the spin buttons. This value is displayed on the Initial State page of the Method Editor and at the bottom of the Control Panel.

Gas B

Use the drop down list to select the gas that is attached to the Gas B port on the analyzer.

Initial Flow Rate for Gas B

Enter the initial flow rate by typing in the value or using the spin buttons. This value is displayed on the Initial State page of the Method Editor and at the bottom of the Control Panel.

Warn user if flow rate changes by

If the flow rate changes by the % specified in this spin box during a run, then Pyris will warn you to check the purge gas. The default value for this field is 10%. You can specify a percentage of 1 to 100.


Cooling Device

Select the Cooling Device currently attached to your analyzer. If you selected a cooling device on the Configuration screen for your DSC 8000 or 8500, then the cooling device you selected in Configuration is shown as the selected cooling device in Preferences.


DSC 8500 Instrument Page

The DSC 8500 Instrument page appears when you select the DSC 8500 tab in the Preferences window. The DSC 8500 Instrument page is available only when you are using a DSC 8500 Instrument Application. This Help topic provides you with information on the settings available to you from this tab page.

Analyzer Constants

Load Temperature

Use the Load Temperature spin box to specify the default Load Temperature which is used in all methods as the default End Condition. When you click the Go To Load button from the control panel, the analyzer automatically heats or cools to the load temperature. You can enter a temperature ranging from –170 °C to 755 °C .

Go To Temp Rate

Use the Go To Temp Rate box to specify the rate at which the analyzer is to heat or cool in order to go to the load temperature or the user-specified temperature entered in the control panel. Proper selection of the heating rate increases the efficiency of your analysis at the desired sensitivity. Slower heating rates improve peak resolution while faster heating rates improve the usable sensitivity. Heating rates greater than 40 °C/min are usually used for rapidly heating or cooling the DSC 8500 to the beginning temperature or the next program step or to selected isothermal temperatures in the temperature program.

You can enter a heating rate between 0.1 and 750.0 °C/min.

Signal Processing

Wavelet Analysis

Check this option if your data contain weak, broad transitions that are difficult to see clearly above the noise in the baseline. A factor of 2 is recommended as a starting point. Use this feature with caution when scanning at fast heating rates (100 °C/min or higher) or when


sharp transitions occur, such as melting endotherms. Factors of 3 or higher may be beneficial for slow scanning rates where you expect broad transitions.

NOTE: Wavelet factors greater than 2 may cause peak distortion on sharp peaks such as indium. If you see an exotherm before a sharp melting peak, then the wavelet number may be too high. We recommend repeating the analysis with different factors to ensure that no peak distortion is occurring. If it is, decrease the factor or turn off the wavelet analysis by unchecking the check box.

Filtering

Check to enable filtering; and then specify how much of the heat flow signal is filtered by the analyzer: 0 = no data smoothing, 1 = minimal data smoothing, 3 = normal data smoothing, and 6 = maximum data smoothing. Values for factor are 0-6 inclusive.

Sample Cover Operation

Minimum Temperature

Use this spin box to specify the minimum temperature for opening/closing the cover assembly. When the analyzer is below the specified temperature, you will not be able to open the cover using the Open/Close Cover button on the control panel.

Maximum Temperature

Use this spin box to specify the maximum temperature for opening/closing the cover assembly. When the analyzer is above the specified temperature, you will not be able to open the cover using the Open/Close Cover button on the control panel.

Override automatic closing of sample covers.

Check this option to disable automatic closing of covers. When this option is checked and you select to start a run the covers will not automatically close. If this option is checked and the covers have been open for more than 6 minutes you will be prompted with a warning message to close the covers.

Data

AutoZero/AutoSlope

Check this option to have Pyris align the final data point of the highest and lowest temperature isotherms and set both to zero, thereby sloping all the scanning data in the process.

Limit Autorescale to

When this option is checked you can enter a maximum rescale value (in milliwatts) to show a flatter baseline.

Range

Select the default data range sensitivity for the ordinate scale. The data range is indicative of the amount of dynamic energy the analyzer can detect. High range is 720 mW full scale and low range is 320 mW full scale.




Analyzer Constants

Load Temperature

Use the Load Temperature spin box to specify the default Load Temperature which is used in all methods as the default End Condition. When you click the Go To Load button from the Control Panel, the analyzer automatically heats or cools to the load temperature. You can enter a temperature ranging from –170 °C to 755 °C.

Go To Temp Rate

Use the Go To Temp Rate spin box to specify the rate at which the analyzer is to heat or cool in order to go to the load temperature or the user-specified temperature entered in the control panel. Proper selection of the heating rate increases the efficiency of your analysis at the desired sensitivity. Slower heating rates improve peak resolution while faster heating rates improve the usable sensitivity. Heating rates greater than 40 °C/min are usually used for rapidly heating or cooling the DSC 8000 to the beginning temperature or the next program step or to selected isothermal temperatures in the temperature program.


Signal Processing Wavelet Analysis

Check this option if your data contain weak, broad transitions that are difficult to see clearly above the noise in the baseline. A factor of 2 is recommended as a starting point. Use this feature with caution when scanning at fast heating rates (100 °C/min or higher) or when


sharp transitions occur, such as melting endotherms. Factors of 3 or higher may be beneficial for slow scanning rates where you expect broad transitions.

NOTE: Wavelet factors greater than 2 may cause peak distortion on sharp peaks such as Indium. If you see an exotherm before a sharp melting peak, then the wavelet factor may be too high. We recommend repeating the analysis with different factors to ensure that no peak distortion is occurring. If it is, decrease the factor or turn off the wavelet analysis by unchecking the check box.

Filtering

Check to enable filtering; and then specify how much of the heat flow signal is filtered by the analyzer: 0 = no data smoothing, 1 = minimal data smoothing, 3 = normal data smoothing, and 6 = maximum data smoothing. Values for factor are 0-6 inclusive.

Sample Cover Operation

Minimum Temperature

Use this spin box to specify the minimum temperature for opening/closing the cover assembly. When the analyzer is below the specified temperature, you will not be able to open the cover using the Open/Close Cover button on the control panel.

Maximum Temperature

Use this spin box to specify the maximum temperature for opening/closing the cover assembly. When the analyzer is above the specified temperature, you will not be able to open the cover using the Open/Close Cover button on the control panel.

Override automatic closing of sample covers.

Check this option to disable automatic closing of covers. When this option is checked and you select to start a run the covers will not automatically close. If this option is checked and the covers have been open for more than 6 minutes you will be prompted with a warning message to close the covers.

Data

AutoZero/AutoSlope

Check this option to have Pyris align the final data point of the highest and lowest temperature isotherms and set both to zero, thereby sloping all the scanning data in the process.

Limit Autorescale to

When this option is checked you can enter a maximum rescale value (in milliwatts) to show a flatter baseline.

Range

Select the default data range sensitivity for the ordinate scale. The data range is indicative of the amount of dynamic energy the analyzer can detect. High range is 720 mW full scale and low range is 320 mW full scale.




Analyzer Constants

Load Temperature

Use the Load Temperature spin box to specify the default Load Temperature which is used in all methods as the default End Condition. When you click the Go To Load button from the control panel, the analyzer automatically heats or cools to the load temperature. You can enter a temperature between –180 °C and 445 °C.

Go To Temp Rate

Use the Go To Temp Rate spin box to specify the rate at which the analyzer is to heat or cool in order to go to the load temperature or the user-specified temperature entered in the control panel. Proper selection of the heating rate increases the efficiency of your analysis at the desired sensitivity. Slower heating rates improve peak resolution while faster heating rates improve the usable sensitivity. Heating rates greater than 40 °C/min are usually used for rapidly heating or cooling the DSC 6000 to the beginning temperature or the next program step or to selected isothermal temperatures in the temperature program.


Data

Ordinate Filter

Check this option to allow for data smoothing.

The Ordinate Filter check box, when checked, filters out noise from the Y signal (heat flow).


Furnace Constant

During the installation of the DSC 6000, your PerkinElmer Service Engineer will enter the Furnace Constant value that is specified on the DSC 6000 Calibration Data sheet in this text box.

NOTE: The DSC 6000 Calibration Data Sheet ships with your instrument.

Heat Flow Conversion

During the installation of the DSC 6000, your PerkinElmer Service Engineer will enter the Heat Flow Conversion (or calorimetric sensitivity) value that is specified on the DSC 6000 Calibration Data Sheet in this text box.


R0

R0, the thermal resistance constant of the DSC 6000, is set at the factory. However, the value may vary from the factory set value as a result of the purge gas and sample pans used in experiments. In order to maximize the accuracy for kinetic and purity results, it may be necessary to adjust the R0 value. Varying R0 will change the slope of the leading edge of a melt curve. Click here for instructions on what to do about changing R0.

Environment

Cooling Device

Select the cooling device that is attached to your DSC 6000 from the drop down list.

Available cooling devices include:

• Circulating Water (tap water or any chiller unit)

• Intracooler

• Cooling Can (Portable cooling device, PCD)

• CryoFill (CryoFill models only)

This parameter has no effect on the software; it is for information only.




Analyzer Constants

Load Temperature

Use the Load Temperature box to specify the default Load Temperature which is used in all methods as the default End Condition. When you click the Go To Load button from the control panel, the analyzer automatically heats or cools to the load temperature.

Go To Temp Rate




Data Ordinate Filter



Furnace Constant

During the installation of the DSC 4000, your PerkinElmer Service Engineer will enter the Furnace Constant value that is specified on the DSC 4000 Calibration Data sheet in this text box.



During the installation of the DSC 4000, your PerkinElmer Service Engineer will enter the Heat Flow Conversion (or calorimetric sensitivity) value that is specified on the DSC 4000 Calibration Data Sheet in this text box.


R0

R0, the thermal resistance constant of the DSC 4000, is set at the factory. However, the value may vary from the factory set value as a result of the purge gas and sample pans used in experiments. In order to maximize the accuracy for kinetic and purity results, it may be necessary to adjust the R0 value. Varying R0 will change the slope of the leading edge of a melt curve. Click here for instructions on what to do about changing R0.

Environment

Cooling Device Select the cooling device that is attached to your DSC 4000 from the drop down list. Available cooling devices include:


• Intracooler

• Cooling Can (Portable cooling device, PCD)



Pyris 1 TGA Instrument Page

The Pyris 1 TGA Instrument page appears when you select the Pyris 1 TGA tab in the Preferences window. The Pyris 1 TGA Instrument page is available only when in the Pyris 1 TGA Instrument Application.

Analyzer Constants

Load Temperature

Enter the default Load Temperature which is used in all methods as the default End Condition. When the Go To Load button on the control panel is selected, the analyzer automatically heats or cools to the load temperature.

Go To Temp Rate

Enter the rate at which the analyzer is to heat or cool in order to go to the load temperature, the temperature setpoint, or the user-specified temperature entered in the control panel. Scanning rates from 0.1 °C/min to 200 °C/min for a standard furnace or 0.1 °C/min to 100 °C/min for a high temperature furnace can be used. The exact scanning rate used depends on the experiment you are performing and the end result you are trying to achieve.

Most typical TGA experiments use a rate ranging from 5 °C/min to 50 °C/min. However, you may want to heat or cool very rapidly to a selected temperature and then hold there isothermally or scan at a controlled rate. In such cases, very fast heating or cooling rates (for example, 100 °C/min to 200 °C/min) are used to raise or lower the sample temperature very quickly.

Y Data

The Pyris 1 TGA has three balance mechanism ranges. The Pyris software stores a calibration value for each of these ranges. When you change the selection here, a new set of values is sent to the analyzer.

High Range

Sets the full-scale range of Y values (weight in milligrams) to 0 – 1300 mg.

Low Range


Ultrasensitive Range


Ordinate Filter Factor

This value is a measure of how much of the ordinate signal (weight) is filtered by the analyzer; 0 = no data smoothing, 1 = minimal data smoothing, 3 = normal data smoothing, and 6 = maximum data smoothing.


TGA 4000 Instrument Page

The TGA 4000 Instrument page appears when you select the TGA 4000 tab in the Preferences window. The TGA 4000 Instrument page is available only when in TGA 4000 Instrument Application.

Analyzer Constants

Load Temperature

Enter the default Load Temperature which is used as the default End Condition in all methods. When the Go To Load button on the control panel is selected, the analyzer automatically heats or cools to the load temperature.

Go To Temp Rate

Enter the rate at which the analyzer is to heat or cool in order to go to the load temperature or the user-specified temperature entered in the control panel. Proper selection of the heating rate increases the efficiency of your analysis at the desired sensitivity. Slower heating rates improve peak resolution while faster heating rates improve the usable sensitivity. Heating rates greater than 40 °C/min are usually used for rapidly heating or cooling the TGA 4000 to the beginning temperature or the next program step or to selected isothermal temperatures in the temperature program. The maximum heating rate is 200 °C/min.


Data

Display Language

Select the language in which the LCD display on the analyzer is to display its information.

Ordinate Filter

The ordinate filter filters out noise from the Y signal (weight). Click on the box to allow data smoothing. There is a 12.5-second delay from the time an event occurs until the time it is observed on the screen when the Ordinate Filter is used.

Furnace Constant

The furnace constant is calculated at the factory and is supplied on the TGA 4000 Data Sheet shipped with the instrument. Enter the value from the sheet here.

Environment

Cooling Device

Select the cooling device attached to your TGA 4000 from the drop-down list. The only available cooling device is Circulating Water (the option for circulating tap water and any circulating chiller unit). This parameter has no effect on the software; it is for information only.

Cooling Air Operating Temperatures

Cooling air to cool the furnace is provided by a small air pump mounted inside the instrument and is enabled and disabled by clicking on the Cooling Air button on the control panel. The Lower and Upper entries define the temperatures at which the pump will turn off and turn on. If the Cooling Air feature is enabled, if the furnace temperature is above the value entered in the Upper field, the pump starts. Once the furnace has cooled down to the temperature in the Lower field, the pump stops. The minimum for Lower is 0 °C and the maximum for Upper is 995 °C.


TGA 8000 Instrument Page

The TGA 8000 Instrument page appears when you select the TGA 8000 tab in the Preferences window. This page is available only when you are using a TGA 8000 Instrument Application.

The image below shows the TGA 8000 Instrument page:

Analyzer Constants Load Temperature

Use the Load Temperature spin box to specify the default Load Temperature which is used in all methods as the default End Condition. When you select Go To Load button from the Control Panel, the analyzer automatically heats or cools to the load temperature. You can enter a temperature ranging from –20-50°C.

Go To Temp Rate

Enter the rate at which the analyzer is to heat or cool in order to go to the load temperature, the temperature set point, or the user-specified temperature entered in the control panel. You can specify a rate ranging from 0.1 °C/min to 500 °C/min.

Most typical TGA experiments use a rate ranging from 5 °C/min to 50 °C/min. However, you may want to heat or cool very rapidly to a selected temperature and then hold there isothermally or scan at a controlled rate. In such cases, very fast heating or cooling rates (for example, 100 °C/min to 200 °C/min) are used to raise or lower the sample temperature very quickly.


Y Data

The TGA 8000 has three balance mechanism ranges. The Pyris software stores a calibration value for each of these ranges. When you change the selection here, a new set of values is sent to the analyzer.

High Range


Low Range


Ultrasensitive Range



This value is a measure of how much of the ordinate signal (weight) is filtered by the analyzer; 0 = no data smoothing, 1 = minimal data smoothing, 3 = normal data smoothing, and 6 = maximum data smoothing.


STA 8000 Instrument Page

The STA 8000 tab page is where you set instrument-specific default values for the STA 8000.

To access this page:

1. Check that you are running the STA 8000 instrument application.

2. Select Preferences from the Tools menu and click the STA 8000 tab.

The STA 8000 tab page displays the following parameters that you can define:

Analyzer Constants

Load Temperature

Enter the default Load Temperature which is used as the default End Condition in all methods. When the Go To Load button on the control panel is clicked, the analyzer automatically heats or cools to the load temperature.

Go To Temp Rate

Enter the rate at which the analyzer is to heat or cool in order to go to the load temperature or the user-specified temperature entered in the control panel. Heating rates greater than 40 °C/min are commonly used for rapidly heating or cooling the STA 8000 to the starting temperature, the next program step or to selected isothermal temperatures in the temperature program. The maximum heating rate is 100 °C/min below 1000 °C and 25 °C/min above 1000 °C.

Maximum Temperature

Enter the maximum temperature of the furnace. Pyris will then prevent any method from using a temperature above this value.

Data

Ordinate Filter

The ordinate filter filters out noise from the Y signal (weight). Click the box to allow data smoothing. There is a delay of 12.5 seconds from the time an event occurs until the time it is observed on the screen when the Ordinate Filter is used.

Environment

Cooling Device

Select the cooling device attached to your STA 8000 from the drop-down list. The only option for the STA 8000, Circulating Water, is for circulating tap water and any circulating chiller unit. This parameter has no effect on the software; it is for information only.


STA 6000 Instrument Page

The STA 6000 tab page is where you set instrument-specific default values for the STA 6000.

To access this page:

1. Check that you are running the STA 6000 instrument application.

2. Select Preferences from the Tools menu and click the STA 6000 tab.

The STA 6000 tab page displays the following parameters that you can define:

Analyzer Constants

Load Temperature

Enter the default Load Temperature which is used as the default End Condition in all methods. When the Go To Load button on the control panel is selected, the analyzer automatically heats or cools to the load temperature.

Go To Temp Rate

Enter the rate at which the analyzer is to heat or cool in order to go to the load temperature or the user-specified temperature entered in the control panel. Heating rates greater than 40 °C/min are commonly used for rapidly heating or cooling the STA 6000 to the starting temperature, the next program step or to selected isothermal temperatures in the temperature program. The maximum heating rate is 100 °C/min.

Maximum Temperature

Enter the maximum temperature of the furnace. Pyris will then prevent any method from using a temperature above this value.

Data

Ordinate Filter

The ordinate filter filters out noise from the Y signal (weight). Click the box to allow data smoothing. There is a delay of 12.5 seconds from the time an event occurs until the time it is observed on the screen when the Ordinate Filter is used.

Environment

Cooling Device

Select the cooling device attached to your STA 6000 from the drop-down list. The option Circulating Water is for circulating tap water and any circulating chiller unit.



DMA 8000 Instrument Page

The DMA 8000 Instrument page appears when you select the DMA 8000 tab in the Preferences window. The DMA 8000 Instrument page is available only when you are using a DMA 8000 Instrument Application. This Help topic provides you with information on the settings available to you from this tab page.

Analyzer Constants

Load Temperature

Use the Load Temperature box to specify the default Load Temperature which is used in all methods as the default End Condition. When you click the Go To Load button from the control panel, the analyzer automatically heats or cools to the load temperature.

Go to Temp Rate


You can enter a heating rate between 0.1 and 20 °C/min.

Load Strain (mm)

Click to increase the strain in 0.01 mm intervals.


Load Frequency (Hz)

Click to increase the frequency in 1 Hz intervals.

Environment

Cooling Device

Select the cooling device that is attached to your DMA 8000 from the drop down list.

Available cooling devices include:


• Liquid Nitrogen (Dewar)

• CLN2


Cryo Valve Control

Check this checkbox to cause Pyris to automatically control the flow of coolant to the environmental chamber using the cryogenic valve.

The control is based on the temperature settings below:

• Valve On - the temperature at which the cryogenic valve is opened.

• Valve Off - the temperature at which the cryogenic valve is closed.

Either enter the required values or use the spin buttons to select them.

Data

Strain Control Window

This setting affects the accuracy of the strain control in the DMA 8000. Setting this value too low may cause excessive adjustment as the instrument attempts to control the strain within narrower tolerance limits. The default setting of 0.05 (5%) should be reduced to 0.01 if highly strain-dependent materials such as carbon-filled rubbers are being analyzed.

Number Of Averages

This is the number of points over which averaging occurs during the experiment. Increasing this value reduces the size of the data file, which can be useful for very long experiments such as a frequency or strain multiplex analysis.

Poisson's Ratio

This is a measure of how the material volume changes with deformation under tension. For an isotropic material, it can be used to convert between the modulus and the shear modulus. The default value of 0.35 is suitable for most glassy polymers.


Broken Sample Threshold (%)

The percentage of the sample stiffness below which the sample is deemed to be broken. Setting this value to zero turns off the detection of broken samples in the DMA 8000.

Purge Gas

The Purge Gas tab in Preferences allows you to select which gas you will use with your analyzer. This is for information only, and does not control the switching of the gases. The software will inform you if there are any actions set up in the Initial State page which use a different gas so you can alter the method.


Diamond DSC Instrument Preferences Page

The Diamond DSC page appears when you select the Diamond DSC tab in the Preferences window. This page contains the following fields:

Analyzer Constants

Load Temperature

Enter the default Load Temperature which is used in all methods as the default End Condition. When the Go To Load button on the control panel is selected, the analyzer automatically heats or cools to the load temperature.

Go To Temp Rate

Enter the rate at which the analyzer is to heat or cool in order to go to the load temperature, the temperature setpoint, or the user-specified temperature entered in the control panel. Scanning rates from 0.1 °C/min to 200 °C/min for a standard furnace or 0.1 °C/min to 100 °C/min for a high temperature furnace can be used. The exact scanning rate used depends on the experiment you are performing and the end result you are trying to achieve.

Maximum Temp.

Enter the default maximum temperature that the analyzer will be allowed to reach. This parameter helps prevent the melting of sample pans. For example, since aluminum melts at 660 °C, enter a maximum temperature of 600 °C.

Environment

CAUTION: If you are running LN2, make sure you check the Liquid Nitrogen in Use check box, or if you are using helium, check the Helium Purge in Use check box. It is important that you check the appropriate check boxes to limit the upper temperature. If these boxes are not checked to lower the temperature, the instrument can be damaged.

Cooling Device

Select the cooling device attached to your analyzer from the drop-down list. This parameter has no effect on the software; it is for information only.

Helium Purge in Use

If you are using the CryoFill Liquid Nitrogen Cooling System, you must use helium for the purge gas. In this case, select this check box. The thermoconductivity of helium is high so when you click in the Helium Purge in Use check box, the system will limit the maximum Go To Load temperature to 300 °C.

Liquid Nitrogen in Use

When using the CryoFill LN2 Cooling System, select this box.


Data

Range

Select the default data range sensitivity for the ordinate scale. The data range in indicative of the amount of dynamic energy the analyzer can detect. High range is 720 mW full scale and low range is 320 mW full scale.

Lag Compensation

This value compensates for the lag of the analyzer in maintaining the scanning rate when heating up to the designated temperature. It helps the analyzer get up to the designated scanning rate faster. Although the thermal lag is small for power-compensated DSC analyzers (that is, the peak shifts up by about 1.3C as the scan rate in increased from 5C/min to 20C/min), it may be significant for some applications. In cases where temperature must be independent of scan rate, correction of measured temperature for differences in scan rate can be performed. See Determine the Lag or Rate Compensation for an explanation on how to determine the value to enter.

Disable Zero Offset

The zero offset (measured when no sample is in place) can be disabled.

Limit Autorescale

Allows you to enter a maximum rescale value (in milliwatts) to show a flatter baseline.

Filter

The following options are available to filter the heat flow signal:

• Time Constant

• Adaptive Boxcar



This value is a measure of how much of the ordinate signal (heat flow) is filtered by the analyzer; 0 = no data smoothing, 1 = minimal data smoothing, 3 = normal data smoothing, and 6 = maximum data smoothing. Values for factor are 0-6 inclusive. This control is enabled only when Time Constant is selected.


Jade DSC Instrument Page

The Jade DSC Instrument page appears when you select the Jade tab in the Preferences window. The Jade DSC Instrument page is available only when you are using a Jade DSC Instrument Application. This Help topic provides you with information on the settings available to you from this tab page.

Analyzer Constants

Load Temperature

Use the Load Temperature spin box to specify the default Load Temperature which is used in all methods as the default End Condition. When you select Go To Load button from the Control Panel, the analyzer automatically heats or cools to the load temperature. You can enter a temperature ranging from –180 °C to 450 °C.

Go To Temp Rate

Use the Go To Temp Rate spin box to specify the rate at which the analyzer is to heat or cool in order to go to the load temperature or the user-specified temperature entered in the control panel. Proper selection of the heating rate increases the efficiency of your analysis at the desired sensitivity. Slower heating rates improve peak resolution while faster heating rates improve the usable sensitivity. Heating rates greater than 40 °C/min are usually used for rapidly heating or cooling the Jade DSC to the beginning temperature or the next program step or to selected isothermal temperatures in the temperature program.

You can enter a temperature rate ranging from 0.1 to 100.0 °C/min.


Data

Ordinate Filter



Furnace Constant

During the installation of the Jade DSC, your PerkinElmer Service Engineer will enter the Furnace Constant value, that is specified on the Jade DSC Calibration Data sheet, in this text box.

NOTE: The Jade DSC Calibration Data Sheet ships with your instrument.


During the installation of the Jade DSC, your PerkinElmer Service Engineer will enter the Heat Flow Conversion (or calorimetric sensitivity) value that is specified on the Jade DSC Calibration Data Sheet, in this text box.

NOTE: The Jade DSC Calibration Data Sheet ships with your instrument.

R0

R0, the thermal resistance constant, of the Jade DSC is set at the factory. However, the value may vary from the factory set value as a result of the purge gas and sample pans used in experiments. In order to maximize the accuracy for kinetic and purity results, it may be necessary to adjust the R0 value. Varying R0 will change the slope of the leading edge of a melt curve. Click here for instructions on what to do about changing R0.

Environment

Cooling Device

Select the cooling device that is attached to your Jade DSC from the drop down list. Available cooling devices are: Available cooling devices include Circulating Water and CryoFill. This parameter has no effect on the software; it is for information only.


Pyris 1 DSC Instrument Page

The Pyris 1 DSC Instrument page appears when you select the instrument's tab in the Preferences window.

Analyzer Constants

Load Temperature

Enter the default Load Temperature which is used in all methods as the default End Condition. When the Go To Load button in the control panel is selected, the analyzer automatically heats or cools to the load temperature entered here.

Go To Temp Rate

Enter the rate at which the analyzer is heat or cool in order to go to the load temperature, the temperature setpoint, or the user-specified temperature entered in the control panel. Scanning rates greater than 100°C/min are normally used only for rapidly heating or cooling the analyzer to starting temperatures or to selected isothermal temperatures. Typical experimental scanning rates range from 5°C/min to 40°C/min.

Maximum Temperature

Enter the default maximum temperature that the analyzer will be allowed to reach. This parameter helps prevent the melting of sample pans. For example, since aluminum melts at 660°C, enter a maximum temperature of 600°C.

Data

Range

Select the default data range sensitivity for the ordinate scale. The data range in indicative of the amount of dynamic energy the analyzer can detect. High range is 720 mW full scale and low range is 320 mW full scale.


This value is a measure of how much of the ordinate signal (heat flow) is filtered by the analyzer; 0 = no data smoothing, 1 = minimal data smoothing, 3 = normal data smoothing, and 6 = maximum data smoothing.

10 s Delay in Use

Use of this parameter reduces noise and drift in the data. It provides a 10-second buffer that helps smooth the data as it goes through a filter. This parameter should be unchecked when you are going to run a StepScan scan. When turned off, the instrument returns to a DSC 7 noise level.

Environment

Cooling Device

Select the cooling device attached to your analyzer from the drop-down list. Available cooling devices are Intracoolers 1P and 2P, CryoFill, ice bath, and water bath. This parameter has no effect on the software; it is for information only.


Helium Purge in Use

If you are using the CryoFill Liquid Nitrogen Cooling System, you must use helium for the purge gas. In this case, select this check box. The thermoconductivity of helium is high so when you click in the Helium Purge in Use check box, the system will limit the maximum Go To Load temperature to 300°C.

Liquid Nitrogen in Use

When using the CryoFill LN2 Cooling System, select this box.

Calibration


Calibration An analyzer is calibrated when it is first installed by a PerkinElmer Instruments Service Engineer. An analyzer remains calibrated, even when the system is turned off, as long as there are no major changes to operating conditions. The Calibration option is available when you are in Method Editor or Instrument Viewer. When selected, a Calibration window opens up, displaying tabbed pages, one for each type of calibration available for that particular analyzer. Click on the desired tab and that calibration routine's page is displayed. When the Calibration window is opened, the values of the calibration file in effect are displayed. Select Open from the File menu to open another existing calibration file. Click on Save and Apply to apply the calibration values from that file to the analyzer. Select Close to exit calibration and continue with your work. You can create a calibration file and save it without applying its values to the analyzer by selecting Save or Save As from the File menu. If you select Close from a calibration window and the current values have not been saved, you will be prompted to save them at this time. If you do not save the calibration values, they will not be applied to the instrument. You can restore the default calibration values at any time by using the commands in the Restore menu. The Restore menu appears when the Calibration window is displayed. The options in the menu are instrument-specific.

Calibration 107

DSC 8000 and DSC 8500 Calibration

Calibration of the DSC 8000 and the DSC 8500 is a multi-step process that involves: • Optimizing the baseline • Calibrating for Sample Temperature • Calibrating the furnace • Calibrating Heat Flow • Performing a SmartScan

To access the DSC 8000 or the DSC 8500 Calibration screen, from the Instrument Viewer or Method Editor select Calibrate Instrument from the Calibrate menu.

The Calibration dialog box appears. From this dialog box you can select to perform Calibration or Restore the Defaults. In this dialog box, the active calibration file is displayed along with the current calibration settings.

Things to consider before starting any calibration

Before starting any calibration, always confirm that any sample holder maintenance has been done. There are two levels of sample holder maintenance. The first level is for typical "clean" analyzers and involves performing a "conditioning run" to 50 degrees above your maximum operating temperature at 100 °C/min, then confirming the gas pressures are set. Level 2 sample holder maintenance should be performed when the sample holder is visually contaminated. If the sample holder is visually contaminated perform the following tasks:

• Clean the guard rings.

• Clean the underside of the sample cover.

• Reform and clean the platinum covers.

• Do a “clean” run from the Pyris Control Panel with the sample holder open to air.

• Remember to bake the platinum covers.

• Do a “conditioning run” to 50 degrees above your maximum operating temperature at 100 °C/min.


Baseline Optimization for the DSC 8000 and DSC 8500 NOTE: To access the DSC 8000 or the DSC 8500 Calibration screen, from the Instrument

Viewer or Method Editor select Calibrate Instrument from the Calibrate menu.

In differential scanning calorimetry (DSC) and differential thermal analysis (DTA), it is recommended that one scan the analyzer before analyzing samples under the conditions you will be using for your samples to check the baseline curvature and noise level. This is done by placing empty sample pans in the sample and reference holders and performing a run using the method you will use for the samples.

The instrument's baseline may be curved or display noise for a number of reasons. There may be trace amounts of residue from a previous experiment attached to the sample holder. Decomposed or sublimated compounds may condense on the sample holder to distort the instrument baseline. Clean the sample holder with ethanol or acetone. If this does not solve the baseline problem, the cause may be the purge gas flow. Linearity of the baseline will be reduced if the purge gas flow rate is not constant or the purge gas contains a large amount of water vapor.

Another cause for an irregular instrument baseline may be the power supply. The mains supply is generally not sufficiently stable for sensitive instruments. Voltage spikes decrease the operating life of the instrument and produce a lot of noise on the baseline. The electrical characteristics of the instrument change over time. The instrument should be readjusted (balance and slope) to maintain a good instrument baseline.

Instrument baseline recorded for successive scans under the same conditions should be identical. If not, moisture may have condensed on the sample holder. Increase the flow of dry purge gas.

To perform baseline optimization:

1. Create a method via the Method Editor that covers the temperature range of interest. The temperature range should cover the intended temperature range of experiments. The minimum temperature should be at least 10 degrees higher than the lowest obtainable temperature of the cooling device. Scanning rates can be set at faster than typical analytical rates. Commonly used rates for baseline optimization are 50 to 100 °C/min.

2. Collect data and perform a peak calculation.

3. From the Instrument Viewer or Method Editor select the Calibrate Instrument command from the Calibrate Menu. The Calibration dialog box is displayed.

4. Press the Calibrate button. The Baseline Optimization screen is displayed.

Calibration 109

5. Click on Enter Values and change the Coarse and Fine Balance value using the table below.

Setting Change in Baseline Optimization Value

Change to Baseline

Coarse +1 -11 mW

Fine +1 -0.25 mW

Slope +1 -6.5 mW

6. Click OK to close the dialog box.

7. Click Accept Values. A warning message is displayed that informs you the Sample Temperature, Furnace, and Heat Flow calibrations are about to be reset to default.


9. Keep clicking the Next button to advance to the end of the calibration wizard.

10. Once you have reached the end of the wizard save the calibration.

11. Perform another baseline run and calculate the Peak Height.

12. Determine the ratio of balance value (number of units change) to peak height (change), for example, 4 units of fine balance = 0.2 mW of curvature change.

13. Return to the Baseline Optimization screen and use the Enter Values button to make the needed changes to balance correction.


15. Click Accept Values. A warning message is displayed that informs you the Sample Temperature, Furnace, and Heat Flow calibrations are about to be reset to default.


17. Keep clicking the Next button to advance to the end of the calibration wizard.

18. Once you have reached the end of the wizard, save the calibration.

19. Run the baseline with the new values.

20. From the last baseline data determine delta Y.

21. Using delta Y, determine the amount of slope correction needed.

22. Access the Baseline Optimization screen again and make necessary changes to the slope value, using the Enter Values button.



Change to Baseline

Coarse +1 -11 mW

Fine +1 -0.25 mW

Slope +1 -6.5 mW

6. Click OK to close the dialog box. 7. Click Accept Values.

A warning message is displayed that informs you the Sample Temperature, Furnace, and Heat Flow calibrations are about to be reset to default.

8. Click OK to close the dialog box. 9. Keep clicking the Next button to advance to the end of the calibration wizard. 10. Once you have reached the end of the wizard, save the calibration. 11. Rerun the baseline to confirm changes.

How do I enter values for Baseline Optimization?

1. Click the Enter Values button. The Enter Values for Baseline Optimization dialog box appears:

2. Enter the following information in the dialog box: Coarse Balance: A setting to roughly adjust the optimization of the baseline curvature. Fine Balance: A setting to fine-tune the optimization of the baseline curvature. Slope: A value to adjust the slope of the baseline.


Change to Baseline

Coarse +1 -11 mW

Fine +1 -0.25 mW

Slope +1 -6.5 mW

3. Click on OK to close the dialog box.

4. Click on Accept Values to modify the calibration based on the values you entered.

NOTE: The values are applied; however, in order to save these values to the calibration file, you click the Next button until you get to the end of the wizard and then save the calibration.

Calibration 111

DSC 8000 and DSC 8500 Sample Temperature Calibration

Temperature calibration is based on a run or series of runs in which a temperature standard (for example, indium) is heated through its melting point. The recorded melting point of this standard is compared to the known melting point, and the difference is calculated for temperature calibration. The DSC 8000 and DSC 8500 can be calibrated for sample temperature using up to 3 standards. Indium is a fixed standard and must always be used.

NOTE: To access the DSC 8000 or DSC 8500 Calibration screen, from the Instrument Viewer or Method Editor select Calibrate Instrument from the Calibrate menu.

NOTE: The lowest permissible scan rate for calibration is 2 °C/min. If you are running at scanning rates less than 2 °C/min, DO NOT calibrate with zinc. It has been found that zinc, when run at slow scan rates, will alloy to the sample pan and furnace.

You have two options for performing Sample Temperature Calibration:

• Automatic Sample Temperature Calibration - If you select this option you only need to enter the following information about a standard: name of standard, weight of the standards, the expected onset temperature, and the scan rate. Once you have entered this information Pyris will automatically perform Sample Temperature Calibration.

• Manual Sample Temperature Calibration - If you do not want to have Pyris automatically perform Sample Temperature Calibration, but rather want to run standards outside of calibration and calculate the melting point for each standard, then you can select the manual Sample Temperature Calibration option. If you select this option you will still need to use the wizard to enter information about the standard. You must enter the following information about each standard you run: name of standard, weight of the standard, the expected onset temperature, the measured temperature, and the scan rate.


How do I perform Automatic Sample Temperature Calibration? To perform Automatic Sample Temperature Calibration:

1. Select the Click Start to have Pyris automatically perform Sample Temperature Calibration... button. The Start... button becomes enabled.

2. Add, Edit and Delete Standards using the buttons, located in the upper right-hand side of the wizard.

NOTE: You must enter a weight for each standard you want to run.

3. Click the Start… button. A message appears informing you that Sample Temperature, Furnace, and Heat Flow calibrations will be reset to their defaults.

Calibration 113

4. Click OK. A message appears that prompts you to place your standard sample pan into the instrument and an empty pan in the reference holder.

5. After placing your first standard into the sample holder and an empty pan in the reference holder, click OK. You are returned to the Sample Temperature Calibration wizard and on this screen you can view the status of the calibration. You can also stop the current procedure by clicking the Stop button. If you click the Stop button, you are prompted with a message asking if you are sure you want to cancel the current calibration procedure. If you click OK, Pyris stops the current procedure, and you are returned to the Sample Temperature Calibration screen.

6. As Pyris performs Sample Temperature Calibration, you are prompted to place your second and third (depending upon the number of standards you defined) standard in the sample holder:

7. After you have followed the instructions that prompt you to place a standard into the sample holder and an empty pan in the reference holder, click OK. You are returned to the Sample Temperature Calibration in Progress… window.

8. When the Calibration routine has finished, the Data Analysis window appears and you are prompted with a message that reads: “Is the calibration data correct?” The values that you must verify as correct are displayed on the dialog box.


Once you have confirmed that the displayed values are correct, click Yes.

9. If you click Yes, you are returned to the Sample Temperature Calibration screen and are informed that Sample Temperature Calibration is complete. To save the data, you must continue to perform all of the calibration routines until you reach the Finish page; or, if you want to just save the Sample Temperature Calibration data, you can click Next to advance to the end of the wizard and then save the data.

10. If you click No, then you are returned to the Sample Temperature Calibration screen and must rerun calibration.

How do I manually perform Sample Temperature Calibration? To Manually Perform Sample Temperature Calibration:

1. Perform a run for each reference material to be used under the same conditions that you run your samples.

2. After each run, perform a peak area calculation and include the onset temperature. Record the ΔH and the onset temperature results.

3. In the Instrument Viewer or Method Editor, select Calibrate Instrument from the Calibrate menu. The Calibration window appears.

4. Click Calibrate and then click Next until you reach the Sample Temperature Calibration screen.

Calibration 115

5. Select the Click Accept Value to manually calibrate Sample Temperature with the values determined outside the wizard button.

6. Use the Add button to enter the name of the reference material used, the expected onset temperature, the measured onset temperature, and the scan rate used. Perform this step for each standard you ran.

7. Click Accept Values.

8. To save the data, you must continue to perform all of the calibration routines until you reach the Finish page; or, if you want to just save the Sample Temperature Calibration data, you can click Next to advance to the end of the wizard and then save the data.


DSC 8000 and DSC 8500 Furnace Calibration

The furnace calibration is designed to allow accurate furnace temperatures to be maintained even when the furnace ages.

NOTE: To access the DSC 8000 or the DSC 8500 Calibration screen, from the Instrument Viewer or Method Editor select Calibrate Instrument from the Calibrate menu.

To perform a furnace calibration:

1. Advance to the Furnace Calibration wizard screen.

2. Enter a Starting and Ending Temperature.

3. Click Start… You are prompted with a message informing you that the Furnace and Heat Flow Calibrations are about to be set to their defaults.

4. Click OK. You are prompted with a message stating that you must empty the furnaces before proceeding.

5. Remove the sample and reference pans and then click OK.

You are returned to the Furnace Calibration screen and the status of the calibration is displayed.

6. If you want to stop the calibration, click the Stop button.

7. When the calibration is complete you are notified on the screen.

8. Click Next to continue to Heat Flow Calibration.

Calibration 117

DSC 8000 and DSC 8500 Heat Flow Calibration NOTE: To access the DSC 8000 or the DSC 8500 Calibration screen, from the Instrument

Viewer or Method Editor select Calibrate Instrument from the Calibrate menu.

NOTE: The lowest permissible scan rate for calibration is 2 °C/min. If you are running at scanning rates of less than 2 °C/min, DO NOT calibrate with zinc. It has been found that zinc, when run at slow scan rates, will alloy to the sample pan and furnace.

You have three options when performing Heat Flow Calibration. The options are as follows:

• Calibrate using indium values obtained during automatic Sample Temperature Calibration.

• Calibrate using a heat of fusion standard.

• Calibrate using the specific heat of sapphire.

How do I perform Heat Flow Calibration using the indium values I obtained during automatic Sample Temperature Calibration? To calibrate Heat Flow Calibration using Indium Values from Sample Temperature Calibration:

1. Advance to the Heat Flow Calibration wizard screen.

2. Select the Use the heat of fusion value for this calibration that was obtained during the Temperature Calibration button.


3. Check Use the area value (heat flow measurement) for Indium that was obtained during Sample Temperature Calibration for your Heat Flow Calibration.

4. When this option is checked, the Heat Flow Calibration details tree is automatically updated to display the Indium values from Sample Temperature Calibration.

5. NOTE: When you check the option to use the values from the Temperature Calibration, you do not need to enter the weight of the indium standard or any other value. All of the information necessary for the heat of fusion standard is displayed on screen.

6. Click Accept Values.

7. NOTE: The Accept Values button is only enabled when “Use the area value….” box is checked.

Calibration 119

8. A message is displayed that prompts you to select if you want to create the heat flow calibration using the values specified on the wizard.

9. Click Yes. The calibration is applied.

10. To save the data, you must continue to perform all of the calibration routines until you reach the Finish page; or, if you want to just save the Heat Flow Calibration data, you can click Next to advance to the end of the wizard and then save the data.


How do I perform Heat Flow Calibration using a heat of fusion standard?

You can select to use a heat of fusion standard for calibration and then manually enter the obtained values from outside of calibration, or have Pyris automatically perform the calibration.

1. Perform the run for the reference material to be used.

2. Calculate the peak area and keep note of the reference material, the weight, the expected heat flow, the measured heat flow, and the scan rate used for the run.

3. From the Instrument Viewer or the Method Editor, select Calibrate Instrument from the Calibrate menu.

4. On the Calibration screen click Calibrate and then use the Next button to advance to the Heat Flow Calibration screen.

Calibration 121

5. Select Use the heat of a heat of fusion standard for your calibration.

6. Click Next. The DSC 8000 Heat Flow Calibration Wizard – Fusion Standard screen is displayed.


7. Select the Manually calibrate Heat Flow… button.

8. Click on the standard listed on the screen and then click the Edit… button. The Add/Edit a Heat Flow standard screen appears.

Calibration 123

9. Enter the name of the reference material, the weight, the expected heat flow, the measured heat flow, and the scan rate.

10. Click Accept Values. You are prompted with a dialog box that asks you if you want to create the heat flow calibration using the values you specified on the wizard.

11. Click Yes, and the Heat Flow Calibration Complete screen is displayed.


To have Pyris automatically perform Heat Flow Calibration using a heat of fusion standard:

1. From the Instrument Viewer or the Method Editor, select Calibrate Instrument from the Calibrate menu.

2. On the Calibration screen click Calibrate and then use the Next button to advance to the Heat Flow Calibration screen.

Calibration 125

3. Select Use the heat of fusion value for this calibration....

4. Click Next. The DSC 8000 Heat Flow Calibration Wizard – Fusion Standard screen is displayed.


5. Select the Click Start… to have Pyris automatically… button.

6. Click on the standard listed on the screen and then click the Edit… button. The Add/Edit a Heat Flow standard screen appears.

Calibration 127

7. Enter values for the following fields: Standard Name, Expected heat of fusion, Temperature, Scan Rate, and Weight. Standard Name: Enter the name of the reference material used in the calibration run. Expected: Enter the expected heat of fusion for the calibration material. This information is provided with the reference material. Measured: Enter the measured heat of fusion from the peak area with onset calculation performed on data previously collected for each calibration material. This is not required. If measured values are not available, use the Click Start... radio button to automatically collect data and recalibrate. Temperature: Enter the melting point "book value" for the onset of melting. Weight: Enter the weight (in mg) of the sample used in the calibration run.

8. Click Start…, You are prompted with message that informs you that the Heat Flow Calibration is about to be set its default value.

9. Click OK. A message is displayed that prompts you to place the standard in the instrument..

10. Click OK. The calibration beings. Next, Pyris Data Analysis is displayed and you are prompted to select whether or not the data collected are OK. The values of the data in question are displayed on a dialog box.

11. If the data are OK, click Yes. When Heat Flow Calibration is complete the Heat Flow Calibration dialog box shows a message stating that the calibration is complete.



How do I perform Heat Flow Calibration using the Specific Heat of Sapphire?

You can select to use the Specific Heat of Sapphire for Heat Flow calibration. In this case, you would perform the following actions:

1. Advance to the Heat Flow Calibration wizard screen.

2. Select Use the specific heat of sapphire for your calibration.

3. Click Next. The DSC Heat Flow Calibration Wizard – Specific heat of Sapphire screen is displayed.

Calibration 129

4. Enter the appropriate data on the DSC 8000 Heat Flow Calibration Wizard – Specific Heat of Sapphire screen and then click Start. Starting and Ending Temperatures: Enter the temperature range over which the calibration is to be optimized. It is not necessary to optimize the calibration over the entire range if most of your experiments will be performed over only a smaller portion of the range. To determine the temperature range, decide upon the lowest temperature of interest and subtract one to two times the scanning rate. For example, if the lowest temperature of interest is 250 °C and the scanning rate is 25 °C/min, the minimum temperature should be: 250 – (25 x2) = 200 °C. To determine the upper temperature limit, decide upon the highest temperature of interest and add one to two times the scanning rate. For example, if the highest temperature of interest is 350 degrees and the scanning rate is 25 °C /min, the upper temperature should be:


350 + (25 x2) = 400 °C. In this case, suitable standards would be indium (156.6 °C) and zinc (419.47). NOTE: If you change your experiments to use a different temperature range than the range used for calibration, you may have to create a new calibration. Scan Rate: This is the preferred heating and cooling scan rate. Enter the same scan rate as planned for your measurements. Sapphire Sample Weight: Enter the weight (in mg) of the sapphire sample in mg. R0: Enter the thermal resistance constant for your sample pan. The value depends on the type of pan you are using, the way the pan has been crimped, and the temperature of the reaction. For most experiments, using aluminum pans, use the default value of 72.00 C/W. To calculate the thermal resistance value, see Thermal Resistance Constant of a Sample Pan.

5. After you click the Start button a message appears informing you that the Heat Flow calibration will be set to default.

6. Click OK. The Heat Flow Calibration is set to default and you are prompted with a second message that instructs you to empty the reference furnace and the sample furnace.

7. After emptying the reference and sample furnaces, click OK. Heat Flow calibration begins and the status of the calibration are displayed on screen.

8. During the calibration you are prompted to place your Sapphire sample into the instrument and an empty pan in the reference holder. Once the sample and reference plan are installed click OK.

9. When Heat Flow Calibration is complete the Heat Flow Calibration a message appears stating that the calibration is complete.


Calibration 131

DSC 8000 and DSC 8500 SmartScan NOTE: If the analyzer has been sitting at a low temperature for a long time, it should be

pre-heated over the desired temperature range.

SmartScan Calibration reduces curvature to produce a flat baseline.

To perform SmartScan:

1. Check the Enable SmartScan check box.

2. Enter a Starting Temperature for your calibration. Enter a starting temperature that is slightly lower than your lowest temperature you plan to use for your analyses; however, do not enter a starting temperature that is within 20 °C of the lowest temperature of your cooling device.

3. Enter an Ending Temperature. For the ending temperature, enter the highest temperature that you expect to use to collect quantitative data plus 10 °C beyond that temperature.

4. Specify the number of Calibration Points. We suggest you use the default value. However, for slow scanning rates, for example 5 °C/min, increase the number of calibration points. If you are running fast scanning rates, then decrease the number of calibration points to no less than 10.

5. The Duration field specifies how long the calibration will take.

6. Click Start... to begin calibration.

7. Once SmartScan has started, follow the prompts on the screen.

8. When SmartScan is finished use the Next button to advance to the Finish screen and save your calibration.


DSC 6000 Calibration

There are two calibration routines for a DSC 6000:

• Temperature

• Heat Flow

The DSC 6000 analyzer has been pre-calibrated at the factory for both temperature and heat flow. Temperature calibration and heat flow calibration should be checked using the precrimped samples of indium and zinc before obtaining data. Some conditions that could affect the current calibration of the DSC 6000 are:

1. If the operating range of your experiments changes, you may need to recalibrate the temperature. Run a standard in the new range of interest to determine if the current calibration is valid.

2. If you change the purge gas type or flow rate, verify that the temperature is still calibrated.

3. If you change the coolant, you may need to recalibrate.

4. If the DSC 6000 has been turned off for a long time (that is, weeks or months), it may appear to require recalibration. If so, condition the analyzer by performing several heating and cooling runs with an empty sample holder, then check the calibration by running standard materials.

Before calibrating the DSC 6000, it is sometimes necessary to restore default calibration values. Typically, it is better to restore defaults when you are changing the temperature range that you are using. If you are changing the purge gas or flow rate, or if the analyzer has not been used for some time, restoring defaults may be necessary. The Temperature calibration can be slightly modified by running a new reference sample while the existing calibration is applied. You can restore default calibration values by selecting the appropriate calibration routine from the Restore menu while in the Calibration window. You can even restore all calibration values by clicking All. This activates the Save and Apply button; click it and then, in the Save As dialog box, select the calibration file to be used or enter a new file name under which to save the values displayed in the calibration window.

NOTE: After you restore the calibration for a DSC 4000, DSC 6000, Jade DSC or a Pyris 6 DSC and click Save and Apply to close the Calibration window, the sample purge gas values must be reapplied on the Control Panel.

For Temperature and Heat Flow calibrations, run high-purity reference materials (typically indium and zinc) with known temperature and energy transitions. The data obtained from these runs are used in the Pyris software calibration routines to calibrate the DSC 6000. Once the analyzer is calibrated, it will remain calibrated even when the system is turned off, as long as there are no changes in the operating conditions.

Calibration 133

Temperature Calibration NOTE: If you are restoring default calibration values, do so before completing the reference

material sample runs.

1. From the Calibration dialog box, select the Temperature tab. The Temperature page displays.

2.

3. To perform the DSC 6000 temperature calibration, complete a scan for each reference material under the same conditions that you use to run your samples.

4. After each run is completed, perform a Peak Area calculation and include the Onset temperature.

5. Record the H (J/g) and Onset results; you will need the Onset result for Temperature calibration and you can use the H result for Heat Flow calibration.

6. When all of the reference materials have been run and calculations performed, enter the reference material name, expected onset temperature, measured onset temperature, and calibration method name used in the table on the Temperature page.

7. Click the check box in the Use column for each reference that is to be used in the calibration.

8. When all of the information has been entered, click the Save and Apply button to save the calibration values and apply them. Go on to the next calibration procedure or click Close to close the Calibration window and begin using the new calibration values.


Heat Flow Calibration

1. From the Calibration dialog box, select the Heat Flow tab. The Heat Flow page displays. A Heat Flow calibration uses a single standard. The Heat Flow calibration value can be slightly modified by running a new reference sample while the existing calibration is applied.

2. To perform the DSC 6000 Heat Flow calibration, complete a scan for the reference material under the same conditions that you run your samples or use one of the scans completed for the Temperature calibration.

3. After the run is completed, perform a Peak Area calculation and record the H (J/g) result.

4. Enter the reference material name, the expected H, the measured H, the weight of the reference material, and the calibration method name in the Calibration table.

5. When all of the information has been entered, click the Save and Apply button to save the calibration values and apply them. Click Close to close the Calibration window and begin using the new calibration values.

Calibration 135

DSC 4000 Calibration

There are two calibration routines for a DSC 4000:

• Temperature

• Heat Flow

The DSC 4000 analyzer has been pre-calibrated at the factory for both temperature and heat flow. Temperature calibration and heat flow calibration should be checked using the precrimped samples of indium and zinc before obtaining data. Some conditions that could affect the current calibration of the DSC 4000 are:




4. If the DSC 4000 has been turned off for a long time (that is, weeks or months), it may appear to require recalibration. If so, condition the analyzer by performing several heating and cooling runs with an empty sample holder, then check the calibration by running standard materials.

Before calibrating the DSC 4000, it is sometimes necessary to restore default calibration values. Typically, it is better to restore defaults when you are changing the temperature range that you are using. If you are changing the purge gas or flow rate, or if the analyzer has not been used for some time, restoring defaults may be necessary. The temperature calibration can be slightly modified by running a new reference sample while the existing calibration is applied. You can restore default calibration values by selecting the appropriate calibration routine from the Restore menu while in the Calibration window. You can even restore all calibration values by selecting All. This activates the Save and Apply button; click it and then, in the Save As dialog box, select the calibration file to be used or enter a new file name under which to save the values displayed in the calibration window.


For temperature and heat flow calibrations, run high-purity reference materials (typically indium and zinc) with known temperature and energy transitions. The data obtained from these runs are used in the Pyris software calibration routines to calibrate the DSC 4000. Once the analyzer is calibrated, it will remain calibrated even when the system is turned off, as long as there are no changes in the operating conditions.




1. From the Calibration dialog box, select the Temperature tab. The Temperature page displays.

2. To perform the DSC 4000 temperature calibration, complete a scan for each reference material under the same conditions that you use to run your samples.


4. Record the H (J/g) and Onset results; you will need the Onset result for Temperature calibration and you can use the H result for Heat Flow calibration.


6. Click on the check box in the Use column for each reference that is to be used in the calibration.

7. When all of the information has been entered, click the Save and Apply button to save the calibration values and apply them. Go on to the next calibration procedure or click Close to close the Calibration window and begin using the new calibration values.

Calibration 137



2. To perform the DSC 4000 Heat Flow calibration, complete a scan for the reference material under the same conditions that you run your samples or use one of the scans completed for the Temperature calibration.

3. After the run is completed, perform a Peak Area calculation and record the H ( J/ g) result.


5. When all of the information has been entered, click the Save and Apply button to save the calibration values and apply them. Click Close to close the Calibration window and begin using the new calibration values.


Pyris 1 TGA Calibration There are three calibration routines for the Pyris 1 TGA:

• Temperature

• Weight

• Furnace

Once your Pyris 1 TGA is calibrated, it should remain so for a long time, provided there are no major changes in operating conditions. The conditions that could affect the current calibration are:

1. If the operating range of your experiments changes, you may need to recalibrate the temperature. Run a standard in the new range of interest to determine if the current calibration is still valid.

2. If you install a new furnace, verify that the temperature is calibrated.


4. If you install a new thermocouple or change the position of the thermocouple, verify that the temperature is still calibrated.

5. If you change the hangdown wire or sample pan, verify that the weight is still calibrated.

6. If the analyzer has been turned off for a long time (that is, weeks or months), it may appear to require recalibration. In this case, condition the Pyris 1 TGA by performing several heating and cooling runs with an empty sample pan, then check the calibration by running standard materials.

Before calibrating the Pyris 1 TGA, it is sometimes necessary to restore the default calibration values. Typically, it is better to restore defaults when changing the temperature range that you are using. If you are changing the purge gas or flow rate, or if the analyzer has not been used for some time, you may need to restore defaults. The Temperature calibration can be slightly modified by running a new reference sample while the existing calibration is applied. You can restore default calibration values by selecting the appropriate calibration routine from the Restore menu while in the Calibration window. You can even restore all calibration values by selecting All. This activates the Save and Apply button, click it and then, in the Save As dialog box, select the calibration file to be used or enter a new file name under which to save the values displayed in the calibration window.

Temperature Calibration

For the Pyris 1 TGA Temperature calibration, run Curie point calibrations for high-purity reference materials. (For the high-temperature furnace Pyris 1 TGA Temperature calibration, refer to ASTM Method E1582 for another procedure.) The data obtained from these runs are used in the Pyris software calibration routines to calibrate the Pyris 1 TGA temperature.

Select the Temperature tab to display the Temperature page of the Calibration window. If you are restoring default calibration values, do so before completing the reference material sample runs.

Calibration 139

To perform the Pyris 1 TGA Temperature calibration, complete a scan for each reference material under the same conditions that you will run your samples. After each run is completed, perform an Onset calculation at the end of the Curie point transition. Record the Onset temperature.

When all of the reference materials have been run and calculations performed, enter the reference material name, expected onset temperature, measured onset temperature, and calibration method name in the table on the Temperature page. Click the check box in the "Use" column for each reference that is to be used in the calibration.

When all of the information has been entered, click the Save and Apply button to save the calibration values and apply them. Go on to the next calibration procedure or select Close to close the Calibration window and begin using the new calibration values.

If you are performing a Furnace calibration next, it is essential to Save and Apply the new temperature calibration first.

Weight Calibration

In a Weight calibration, you compare the known weight of a reference material with the actual weight read from the Pyris 1 TGA. The Weight calibration value can be slightly modified by recalibrating while the existing calibration is applied. Enter the known weight of the reference material in the Weight page of the Calibration window, then select the Begin Calibration button and follow the instructions in the dialog boxes. The instructions are slightly different for a Pyris 1 TGA with an autosampler.

Furnace Calibration

The Pyris 1 TGA Furnace calibration is a nine-point calibration between two specified temperature limits. It linearizes the Pyris 1 TGA furnace by matching the program temperature to the thermocouple temperature over the range that you enter.

NOTE: If you have just completed a Temperature calibration procedure, you must Save and Apply the new Temperature calibration before starting the Furnace calibration.

Select the Furnace tab to display the Furnace page of the Calibration window. Enter the Minimum and Maximum temperature limits, then select the Begin Calibration button and follow the instructions in the dialog box. You can minimize the Instrument Application window while the Pyris 1 TGA furnace is being calibrated so you can use other applications on the computer. To accept the Furnace calibration values, click Save and Apply.


TGA 4000 Calibration

There are three calibration routines for a TGA 4000:

• Furnace

• Temperature

• Weight

The TGA 4000 analyzer has been calibrated by the service engineer during installation. Under normal conditions, the TGA 4000 does not need temperature recalibration. If it is necessary to calibrate the TGA 4000, furnace calibration must be performed before temperature calibration. Temperature calibration should be checked using the two or three of the reference materials provided and the weight calibration should be checked using the reference weight provided before performing any runs.

Once your TGA 4000 is calibrated, it should remain so for a long time, provided there are no major changes in operating conditions. The conditions that could affect the current calibration are

1. If the operating temperature range of your experiments changes, you may need to recalibrate the temperature. Run a standard in the new range of interest to determine if the current calibration is still valid.


3. If you install a new sample thermocouple, or if the existing one has been disturbed, verify that the temperature is still calibrated.

4. If you change the sample pan, verify that the weight is still calibrated.

5. If the analyzer has been turned off for a long time (that is, weeks or months), it may appear to require recalibration. In this case, condition the TGA 4000 by performing several heating and cooling runs with an empty sample holder, then check the calibration by running standard materials.

Before calibrating the TGA 4000, it is sometimes necessary to restore default calibration values. Typically, it is better to restore defaults when changing the temperature range used. If you are changing the purge gas or flow rate, or if the analyzer has not been used for some time, you may need to restore defaults. The Temperature calibration can be slightly modified by running a new reference sample while the existing calibration is applied. You can restore default calibration values by selecting the appropriate calibration routine from the Restore menu while in the Calibration window. You can even restore all calibration values by selecting All. This activates the Save and Apply button; click it and then, in the Save As dialog box, select the calibration file to be used or enter a new file name under which to save the values displayed in the calibration window.

Furnace Calibration

The TGA 4000 Furnace calibration is a nine-point calibration between two specified temperature limits. It linearizes the TGA 4000 furnace by matching the program temperature to the thermocouple temperature over the range that you enter.

Calibration 141

The Furnace calibration must be done before the Temperature calibration.

Select the Furnace tab to display the Furnace page of the Calibration window. Enter the Minimum and Maximum temperature limits, then select the Begin Calibration button and follow the instructions in the dialog box. You can minimize the Instrument Application window while the TGA 4000 furnace is being calibrated. To accept the Furnace calibration values, click Save and Apply.


For the TGA 4000 Temperature calibration, run Curie point calibrations for the high-purity reference materials provided with the instrument. The data obtained from these runs are used in the Pyris software calibration routines to calibrate the TGA 4000 temperature. Once the analyzer is calibrated, it will remain calibrated even when the system is turned off, as long as there are no changes in the operating conditions.


To perform the TGA 4000 Temperature calibration, you complete two scans for each reference material under the same conditions that you run your samples. The first run should use the lower scanning rate (for example, 5 °C/min) and the second run the higher scanning rate (for example, 50 °C/min). You must run at least two reference materials. After each run is completed, perform an Onset calculation at the end of the Curie point transition. Record the Onset temperature.

When all of the reference materials have been run and calculations performed, in the Temperature calibration page enter the reference material name, expected onset temperature, measured onset temperature, and the scanning rates used.

When all of the information has been entered, click the Save and Apply button to save the calibration values and apply them.

Weight Calibration

In a Weight calibration, you compare the known weight of a reference material with the actual weight read from the TGA 4000. The Weight calibration value can be slightly modified by recalibrating while the existing calibration is applied.

Enter the known weight of the reference material in the Weight page of the Calibration window, then select the Begin Calibration button and follow the instructions in the dialog boxes. You can cancel the calibration at any time by selecting the Cancel button in any dialog box.


TGA 8000 Calibration

The TGA 8000 is calibrated at the factory and this calibration file is loaded from the CD upon installation. There is also a default calibration which removes all of the calibration adjustments and reverts to the hardware presets.

The TGA must be calibrated before obtaining accurate data. Calibration is performed using the Pyris Software calibration routine which is accessed from the Calibrate menu through the Method Editor window. There are four independent calibration routines accessed through the three tabs on the Calibration menu item that should be performed for a TGA with or without an autosampler:

• Weight Calibration

• Temperature Calibration

• Baseline Optimization

• Balance Optimization

In general, the calibrations should be performed in the above order; however, the weight calibration will be done first and will likely only need to be done again if the TGA is moved or re-leveled.

Before redoing the baseline calibration, restore the default baseline using the Restore function in the Calibrate menu. The 8-hour Baseline Drift Optimization needs only to be performed once, provided the full calibration was not set to defaults.

The Temperature and Baseline Calibration may be re-done to optimize the TGA for optimum temperature and weight loss accuracy. For many routine separations this level of calibration accuracy is unnecessary. It is wise to Save and Apply each calibration that is performed under a new and descriptive file name so it can be recalled in the future using the File > Open menu item.

Conditions that can affect the current calibration

Once your TGA 800 is calibrated, it should remain so for a long time, provided there are no major changes in operating conditions. The conditions that could affect the current calibration are:


2. If you install a new furnace, verify that the temperature is calibrated.


4. If you install a new thermocouple or change the position of the thermocouple, verify that the temperature is still calibrated.

5. If you change the hangdown wire or sample pan, verify that the weight is still calibrated.

Calibration 143

6. If the analyzer has been turned off for a long time (that is, weeks or months), it may appear to require recalibration. In this case, condition the TGA 8000 by performing several heating and cooling runs with an empty sample pan, then check the calibration by running standard materials.

Weight Calibration

In a Weight calibration, you compare the known weight of a reference material with the actual weight read from the TGA 8000.

NOTE: The weight calibration will be different depending on which Y Range you are using. Most people use the Low Range, which gives a dynamic range of +/- 160 mg. You can specify the Y Range to use on the TGA 8000 Preferences tab.

In order to perform the weight calibration, you will need the 100 mg calibration weight (P/N 09200501) in the Spares Kit (P/N N5320026).

About Weight Calibration

The Weight Calibration tab contains the following fields:

Operator

Enter an operator name up to 40 characters; it will be saved with the calibration file.

Date and Time

This is display only and is automatically updated when a calibration routine is completed successfully and the values are calculated.

Range

This is display-only. The Range is selected in the Instrument Page in Preferences. It is an indication of the amount of dynamic energy that the analyzer can detect. You should have a good sense of the transition energy of the materials that you will be running. The Low selection will work with most experiments.

Reference Weight

Enter the weight of the reference material used in the calibration routine. This is provided with the reference material.

Measured Weight

The weight of the reference material as measured by the analyzer during calibration is displayed.

Begin Calibration

For a TGA 8000 without an autosampler, clicking on this button displays the first weight calibration dialog box which instructs you to prepare the analyzer for a zero reading, that is, read the weight of the empty sample pan.

After following the instructions, clicking on OK, and performing the Read Zero calibration, the second weight calibration dialog box is displayed which instructs you to place the reference weight in the sample pan for a weight reading.

For a TGA 8000 with an autosampler, the first weight calibration dialog box instructs you to place an empty crucible at position 1 of the autosampler tray.


The second weight calibration dialog box instructs you to place the reference weight in the empty crucible in position 1. After you click on OK, the furnace will be raised and the weight will be read.

Save and Apply

Applies the calibration value to the analyzer and saves the values in the calibration file you designate in the Save As dialog box.

To perform Weight Calibration:

1. Select Preferences from the Tools menu, and then select the TGA 8000 tab.

2. In the Y Data section select the range you plan to use and click OK.

3. Select Calibrate Instrument from the Calibrate menu.

4. Select the Weight tab.

5. Type a name in the Operator ID field (optional).

6. Enter the weight of the calibration weight in the Ref. Weight field.

NOTE: Remove any pan from the hangdown wire because once you click Begin Calibration you cannot remove it.

7. Click Begin Calibration. A dialog box appears with instructions to remove anything in the sample pan. Autosampler system only: If you have an autosampler, remove any sample from crucible 1. The autosampler should be in the Safe position.

8. Follow the instructions in the dialog box, then click OK. The analyzer is tared for a zero reading. Autosampler system only: If you have an autosampler, after accepting the reading, the crucible is unloaded and the furnace is lowered. After approximately 30 seconds, the autosampler rotates the tray so that position 1 is easily accessible.

9. When prompted, place and center the calibration weight in the sample pan and then click the OK button, The value of the calibration weight is read and displayed in the dialog box. Click OK to accept the reading when the weight is stable. . Autosampler system only: If you have an autosampler, place the reference weight in crucible 1 and click OK. The value of the calibration weight is read and displayed. When the signal settles, click OK to accept the reading. The furnace goes to the Cool position and the crucible is returned to the tray.

10. The just measured value is automatically displayed in the Measured field.

11. Click the Save & Apply button to send the new calibration value to the analyzer and save the calibration file. The weight calibration is complete.

Calibration 145

12. Click the Close button to exit the Calibration window. OR Click on the Temperature tab to perform Temperature calibration.


The temperature calibration is performed for a TGA 8000 with or without an autosampler. Perform the procedure below to calibrate the TGA for temperature.

About TGA 8000 Temperature Calibration

To perform the TGA 8000 Temperature calibration, you complete two scans for each reference material under the same conditions that you run your samples. The first run should use the lower scanning rate (for example, 5 °C/min) and the second run the higher scanning rate (for example, 50 °C/min). You must run at least two reference materials. After each run is completed, perform an Onset calculation at the end of the Curie point transition. Record the Onset temperature.

When all of the reference materials have been run and calculations performed, enter the reference material name, expected onset temperature, measured onset temperature, and the scanning rates used on the Temperature Calibration page.

When all of the information has been entered, click the Save and Apply button to save the calibration values and apply them.

The items on the Temperature Calibration tab are as follows:

Operator


Date and Time

This is display-only and is automatically updated when a calibration routine is completed successfully and the values are calculated.

Reference Material

Enter the names of the reference materials used in the calibration runs.

Expected Onset

Enter the expected onset temperatures for each calibration reference material. That information is provided with the reference material.

Measured Onset at Rate 1 or Rate 2

Two runs are performed for each of the reference materials you choose to use for calibration. Enter the measured onset results at the two scanning rates for each reference material.

Rate 1 and Rate 2

Enter the scanning rates used for the two runs per reference material. The recommended rates are 5°C/min and 20°C/min.


Use

When Use is checked for a particular line, the calibration values on that line will be used in calculating the calibration factors.

Save and Apply

Applies the values entered in the table to the analyzer and saves the values in the file specified in the Save As dialog box. You can overwrite the current calibration file.

To perform Temperature Calibration:

The temperature calibration is performed for a TGA 8000 with or without an autosampler. Perform the procedure below to calibrate the TGA for temperature.

NOTE: For a temperature calibration use the magnetic standards of test metals Alumel, Nickel, Perkalloy and Iron supplied in the Spares kit. The runs should use the same conditions under which you would run your samples. Temperature calibration uses the Curie transition of the materials, that is, the point at which the magnetic properties disappear.

1. Select Preferences from the Tools menu, then select the TGA 8000 tab.

2. In the Y Data section set the range to Low Range +/-160mg, leave the Ordinate Filter ON, and click OK. Precondition the TGA by running the method: InstrumentCondition.tg8m. The default location for the file is: C:\Program Files (x86)\PerkinElmer\Pyris\methods The calibration method is displayed.

3. Cut 2-3mm lengths of test metals Alumel, Nickel, Perkalloy and Iron, put them into a platinum pan, and then cover them with thin coating of alumina powder.

4. Without an autosampler system, attach the pan onto the hangdown wire, raise the furnace, and observe the angle of the pan bale/stirrup. With an autosampler system, load the sample into a pan in position 1. Click the Autosampler Control button in the Pyris software's control panel. Click Load Sample. The tray will move and hook the pan onto the hangdown wire. Click the OK button to close the dialog box.

5. From the Method Editor, select Open Method from the File menu. Double-click the method file: PreCalAlumelNickelPerkalloyIron.tg8m. (The default location for the file is Program Files\Pyris\Methods). The calibration method is displayed.

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

7. Tare the weight by clicking the Zero Weight button in the Control Panel. The analyzer reads the weight of the sample which is entered into the Zero field of the Enter Sample Weight box in the Method Editor.

8. Lower the furnace then open the furnace door and carefully place the magnet (P/N N5370466) around the furnace tube, then raise the furnace.

Calibration 147

9. Rotate the magnet until the pan rotates from the magnetic field to its pre-magnet angle. Make sure the sample pan is not touching the sidewall of the furnace during this procedure. If it is, swivel the magnet until the pan is centered.

10. Click the Sample Weight icon on the Control Panel.

11. Click the Start Method button in the Control Panel.

12. After the run, move the sample pan without disturbing the contents to a spot on the autosampler carousel. It will be rerun later.

13. You are now ready to calculate the Onset Value for all four calibration standards.


Calculating the Onset Value

This is done in the Data Analysis window..

1. Click the Data Analysis icon on the toolbar, then open the data file in the Data Analysis window.

2. Make sure that the curve is displayed with the following axes: X = Temperature (change by selecting Rescale X from the Display menu and then select Temperature in the dialog box). Y = Weight (change by selecting Weight from the Curves menu).

3. In the Curves menu select the Weight curve..

4. In the Step Select dialog select step 2 and step 5 through 12. (These two curves contain data for heating the Curie samples at 20 and 5 degrees per minute. (You can delete the original weight data curve..

5. Select Onset from the Calc menu.

6. Using the steepest slope and the trailing baseline use the Onset Calculation to determine the Curie points of the four materials at these two rates.

7. Input the values into the Calibration file.

8. Select Instrument view.

9. Click the sample curve to be analyzed.

10. Select Derivative on the Math menu so the derivative curve goes to the background. Move the two red X marks on the curve. Position the left limit X at the inflection point of the first derivative curve and place the right limit X past the inflection point on the level part of the curve.

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

12. Adjust the tangents of each point until they cross and each is tangential at the point selected.

Calibration 149

Perform this Onset calculation on each of the eight Curie temperatures (4 at 5 °C/min and 4 at 20 or 25 °C/min.

13. Click the Calculate button in the Adjust Tangents dialog box. The onset temperature is calculated for the sample and displayed on the screen (Onset X).

14. In the Method Editor, select Calibrate Instrument from the Calibrate menu.

15. Click the Temperature tab in the Calibration window. Enter the name of each reference material, the Expected Onset values, the Measured Onset values, and click the check box in the Use column for each reference material used in the calibration. (Four temperatures at two rates.)

16. Check the standards you plan to use and uncheck the others.

17. Click Save and Apply to send the calibration values to the analyzer and save the current calibration file current calibration file (SN_weightcal_st.tg8c). The temperature calibration is now complete.

18. Click Close to exit the Calibration window. OR Perform TG Drift Calibration as described below.


TG Drift Calibration

If the instrument has just been installed or the cooling system has changed, you should perform a TG Drift Optimization to correct for the effect of the balance temperature on the measured weight. The Baseline Drift optimization takes approximately 10 min.

NOTE: It is not necessary to perform a TG Drift Optimization after installation unless the cooling system has been changed. Ensure that the box is not checked at other times to prevent the optimization being performed unnecessarily.

1. From the Pyris menu, select Calibrate Instrument from the Calibrate menu.

2. Select the TG Drift tab on the Calibration window.

3. Uncheck Perform Balance Optimization (~7 hours) and check Perform Baseline Optimization.

4. For a TGA 8000 without an autosampler, place a clean empty sample pan in the stirrup at the end of the hangdown wire. Place it there manually with tweezers while the autosampler is in the Safe position. For an autosampler system, place a pan in Position 1 on the autosampler tray and use the Autosampler Control dialog box to load a sample..

5. Enter the Minimum and Maximum temperatures between which the baseline will be determined (the defaults are 30 °C and 1150 °C).

6. Equilibrate at the initial temperature.

7. Select a scanning Rate (°C/min) that you will be using for scanning analyses, e.g., 20 °C/min.

8. Click Begin Calibration. An estimate of the amount of time needed to perform the calibration is displayed and it begins to count down.

9. When the calibration is complete, click Save & Apply to send the new calibration value to the analyzer and save the file (SN_weightcal_st_balanceopt.tg8c).

10. Click Close to exit the Calibration window. OR Follow the instructions provided below to perform Baseline Drift Optimization.

Calibration 151

Balance Drift Optimization If the instrument has just been installed or the cooling system has changed, you should perform a TG Drift Optimization to correct for the effect of the balance temperature on the measured weight.


1. From the Pyris menu, select Calibrate Instrument from the Calibrate menu.

2. Select the TG Drift tab on the Calibration window.

3. Uncheck Perform Baseline Optimization.

4. Check Perform Balance Optimization (~7 hours) if you have just installed the TGA 8000 or changed the cooling system. This routine, which uses a predefined method, will be performed immediately before the Baseline Optimization.

5. For a TGA 8000 without an autosampler, place a clean empty sample pan in the stirrup at the end of the hangdown wire. Place it there manually with tweezers while the autosampler is in the Safe position. For an autosampler system, use the Autosampler Control dialog box to load a sample.

6. Enter the minimum and maximum temperatures between which the baseline will be determined (the defaults are 50 °C and 1150 °C).

7. Select a scanning Rate (°C/min) that you will be using for scanning analyses, e.g., 20 °C/min.

8. Click Begin Calibration. An estimate of the amount of time needed to perform the calibration is displayed and it begins to count down.

9. When the calibration is complete, click Save & Apply to send the new calibration value to the analyzer and save the file (SN_weightcal_st_balanceopt_baselineopt20C.tg8c). .

10. Click Close to exit the Calibration window.

The TGA 8000 calibration is now complete.


STA 8000 Calibration The following procedure involves using the calibration file that is located on the Pyris CD that is shipped with your STA 8000. Calibration of the STA 8000 involves the following steps:

• Weight Calibration • DTA Baseline Optimization • Temperature Calibration • Heat Flow Calibration

Weight Calibration, TG Drift Optimization and DTA Baseline Optimization

This procedure will allow you to skip the temperature and heat flow calibrations. The weight should be recalibrated if the analyzer is physically moved, or if measuring the weight of a reference reveals that the balance calibration has drifted. Calibrating the weight will not default the temperature or heat flow calibrations. If the instrument has just been installed or the cooling system has changed, you should perform a TG Drift Optimization to correct for the effect of the balance temperature on the measured weight. If the coolant temperature, purge gas flow rate or sensor has changed, then a Differential Thermal Analyzer (DTA) baseline optimization should be performed, which fits an equation to the thermal analysis curve between two selected temperatures to flatten the baseline. This will default the temperature and heat flow calibrations.

1. On the Pyris toolbar click Calibrate > Calibrate Instrument. The current calibration values are displayed.

2. If you want to use different calibration values, click File > Open on the toolbar. Select the calibration file you want to use and click Open. A message asks if you want to apply the selected file; click OK.

3. Click Start Calibration.

4. Click the Run Calibration button and follow the prompts to run and save the weight calibration. Calibrate the weight using a Class '0' 100 mg weight or the weight provided with the analyzer.

5. Click Next to move to the Baseline Optimization screen.

6. Enter the starting and ending temperatures and the scan rate. Use values that are similar to those used in typical experiments.

7. Check the box marked Perform TG drift optimization (~8 hours) if you have just installed the STA 8000 or changed the cooling system. This routine, which uses a predefined method, will be performed immediately before the DTA Baseline Optimization.


Calibration 153

8. Click Run Calibration to begin the optimization routine(s). A message asks if you want to set the temperature and heat flow calibrations to their default values; click OK. The optimization will proceed; it takes 1–2 hours to complete (this extends to ~10 hours if the TG Drift Optimization is selected).

9. If temperature and heat flow calibrations are implemented, run experiments to verify the calibration using reference samples. See the Installation and Hardware Help for further information. If necessary, run a new calibration for the temperature and heat flow as described below.

Temperature and Heat Flow Calibration

There are two methods of calibrating the temperature and heat flow. You can manually enter the required measurements from experiments run separately using the reference materials, or the Pyris software can run the experiments itself and extract the required measurements. If you use the Pyris software to run the calibrations, then you should repeat the weight calibration and baseline optimization procedures.

NOTE: The recommended calibration standards for temperature in the STA 8000 are indium, aluminium and gold. The user can substitute these for different standards using the calibration wizard in the Pyris software. Palladium should be used instead of gold if your experiments require temperatures above 1300 °C. The recommended calibration standards for heat flow are indium and gold/palladium. For both calibrations, use standards that bracket the temperature range of your experiments whenever possible.

To enter the data manually:

1. On the Pyris toolbar click Calibrate > Calibrate Instrument, click Start Calibration and click Next to reach the Temperature Calibration screen.

2. Highlight Indium, click Edit and then enter the Measured and Expected values, the Scan Rate and the Sample Weight.

NOTE: The effect of scan rate on the temperature measurement can be calibrated by running a second test on the standards using a different scan rate, which must be at least twice that of the first. If this option is used, a second value for the measured temperature must also be entered in the sample data.

3. Repeat step 2 for aluminium and gold.

4. If you want to use a different standard, highlight the standard you want to alter, click Edit and OK and enter the required information as in step 2.

5. Click the Accept Values button. A message asks if you want to set the heat flow calibration to its default value; click OK.

6. After the calibration has been accepted, click Next to see the Heat Flow Calibration screen.

7. Enter the required information for the heat flow standards you want to use, including the measured heat of fusion values and the scan rates from your experiments. If you made changes to the standards in the temperature calibration screen, you may need to make similar changes in the heat flow calibration screen.

NOTE: Be particularly careful to check that the heat of fusion value is correct for the standard you want to use.


8. Click Next.

9. Click Finish and Yes to save the data. When the Save dialog box appears, type in a filename and save the file. The calibration window returns to the first page. Your calibration values are displayed and the title bar at the top of the window shows your newly saved filename.

10. Close the calibration window. To run the calibration using the Pyris software:

1. On the Pyris toolbar click Calibrate > Calibrate Instrument. The first page of the calibration wizard displays the current calibration values.

2. If the default values are displayed (no corrections), click Start Calibration.

3. If there is another file implemented, click File > Open, select the default file and click Open; a message asks if you want to apply the selected file; click OK. OR Click Restore All Defaults which will restore all the values to a "no correction" status.

4. Perform the weight calibration and DTA baseline optimization as described in the previous procedure.

5. Click Next to see the Temperature Calibration screen.

6. Highlight a standard and click Edit to change the material or its properties if required. If the optional second scan rate is used, ensure that this is at least twice the value of the first scan rate. A maximum scan rate of 20 °C/min is recommended for experiments.

7. Enter an arbitrary value for the weight of each standard. The STA 8000 will measure the actual sample weight when it runs the experiment.

8. Click Run Calibration.

9. When prompted, zero the weight of the empty sample pan, and then place 10–20 mg of the sample into the pan to measure the sample weight. The software then runs the experiment by automatically selecting the appropriate method for the standard.

10. When prompted, repeat step 9 for the other standards selected.

11. After the temperature calibration is completed, click Next to see the Heat Flow Calibration screen. The heat flow calibration can be applied using the experiments from the temperature calibration, or by running new experiments.

12. To use the temperature calibration data, check the box labelled Use the area value... and click Accept Values. OR To run a new experiment, select the standard and click Run Calibration. Follow the instructions on the screen to run the experiment.

Calibration 155

NOTE: The option to use area values from previous experiments is only available if a valid temperature calibration has been run by the software. Otherwise, heat flow values have to be either entered manually or measured in new experiments.

13. Once the heat flow calibration is completed, click Finish and Yes to save and apply the data. When the Save dialog box appears, type in a filename and save the file. You cannot write over the default calibration file. You are returned to the first page of the calibration wizard. Your calibration values are displayed and the title bar, at the top of the window, shows the newly saved filename.

14. Close the calibration window.

See the Pyris Installation and Hardware Help for further information on sample preparation.

The calibration of the STA 8000 is complete.


STA 6000 Calibration

The following procedure involves using the calibration file that is located on the Pyris CD that is shipped with your STA 6000.

Calibration of the STA 6000 involves the following:

• Weight Calibration

• Sensor Calibration

• DTA Baseline Optimization

• Temperature Calibration

• Heat Flow Calibration

Manual Weight and Sensor Calibration and Baseline Optimization

This procedure will allow you to skip the temperature and heat flow calibrations. The weight should be calibrated if the analyzer is physically moved, or if measuring the weight of a reference reveals that the balance calibration has drifted. Calibrating the weight will not default the temperature or heat flow calibrations. If the coolant temperature, purge gas flow rate or sensor has changed, then a Differential Thermal Analyzer (DTA) baseline optimization should be performed, which fits an equation to the thermal analysis curve between two selected temperatures to flatten the baseline. This will default the temperature and heat flow calibrations.

1. On the Pyris toolbar click Calibrate > Calibrate Instrument. The current calibration values are displayed.

2. If you want to use different calibration values, click File > Open on the toolbar. Select the calibration file you want to use and click Open. A message asks if you want to apply the selected file; click OK.

3. Click Start Calibration.

4. Click the Run Calibration button and follow the prompts to run and save the weight calibration. Calibrate the weight using a Class '0' 100mg weight or the weight provided with the STA.

5. Click Next to move to the Sensor Calibration screen. This step can be skipped without affecting the other calibrations.

6. Enter the start and end temperatures for testing the furnace thermocouple, and click Run Calibration. The default values of 30 and 1000 °C are generally suitable. The process will take approximately 1 hour.

7. Click Next to move to the Baseline Optimization screen.

Calibration 157

8. Enter the starting and ending temperatures and the scan rate. Use values that are similar to those used in typical experiments.

9. Click Run Calibration to begin the optimization. A message asks if you want to set the temperature and heat flow calibrations to their default values; click OK. The optimization will proceed; it takes 1–2 hours to complete.

10. If Temperature and Heat Flow calibrations are implemented, run experiments to verify the calibration using reference samples. See the Installation and Hardware Help for further information. If necessary, run a new calibration for the temperature and heat flow as described below.


Temperature and Heat Flow Calibration

There are two methods of calibrating the temperature and heat flow. You can manually enter the required measurements from experiments run separately using the reference materials, or the Pyris software can run the experiments itself and extract the required measurements. If you use the Pyris software to run the calibrations, then you will need to repeat the weight and sensor calibrations and baseline optimization procedures.

NOTE: The recommended calibration standards for temperature in the STA 6000 are indium and silver. The user can substitute these for different standards, or add a third. Heat flow is calibrated using indium.

To enter the data manually:

1. On the Pyris toolbar click Calibrate > Calibrate Instrument, and click Next to reach the Temperature Calibration screen.

2. Highlight Indium, click Edit and then enter the Measured and Expected values, the Scan Rate and the Sample Weight.

3. NOTE: The effect of scan rate on the temperature measurement can be calibrated by running a second test on the standards using a different scan rate. A value of 5 °C/min is recommended. A scan rate of more than 20 °C/min should be used with caution because the measurement of melting temperature will be less accurate.

4. Repeat step 2 for silver.

5. Click on the Accept Values button. A message asks if you want to set the heat flow calibration to its default value; click OK.

6. After the calibration has been reset, click Next to see the Heat Flow Calibration screen. The measured and expected heat of fusion values should be the same.

7. Click Next.

8. Click Finish and Yes to Save. When the Save dialog box appears, type in a filename and save the file. The calibration window returns to the first page. Your calibration values are displayed and the title bar at the top of the window shows your newly saved filename.


To run the calibration using the Pyris software:

1. On toolbar click Calibrate > Calibrate Instrument.

2. The first page of the calibration wizard displays the current calibration values. If they are the default values (no corrections), click Start Calibration.

3. If there is another file implemented, click File > Open, select the default file and click Open; a message asks if you want to apply the selected file; click OK. OR Click Restore All Defaults which will restore all the values to a "no correction" status.

Calibration 159

4. Perform the weight and sensor calibration and baseline optimization as described in the previous procedure.

5. Click Next to see the Temperature Calibration screen.

6. Highlight the standards and click Edit to change the material or scan rate. A maximum scan rate of 20 °C/min is recommended. Enter an arbitrary sample weight if prompted. The Pyris software will measure the actual sample weight when it runs the experiment.

7. Click Run Calibration.

8. The software prompts you to zero the weight of the empty sample pan, and then place the sample into the pan to measure the sample weight. The software then runs the experiment by automatically selecting the appropriate method for the standard.

9. When prompted by the software, repeat step 8 for the other standards selected.

10. After the temperature calibration is completed, click Next to see the Heat Flow Calibration screen. The heat flow calibration can be applied using the experiments from the temperature calibration, or by running new experiments.

11. To use the temperature calibration data, check the box labeled Use the area value..., select the standard from the list in the box, and click Accept Values. OR To run a new experiment, select the standard and click Run Calibration. Follow the instructions on the screen to run the experiment.

12. Once the heat flow calibration is completed, click Finish and Yes to save and apply the data. When the Save dialog box appears, type in a filename and save the file. You cannot write over the default calibration file. You are returned to the first page of the calibration wizard. Your calibration values are displayed and the title bar, at the top of the window, shows the newly saved filename.


The calibration of the STA 6000 is complete.


DMA 8000 Calibration

There are five calibration routines for the DMA 8000:

Balance Zero

This calibration determines and records the zero displacement position and the force required to return to the zero position, when the head is oriented non-horizontally. It should be performed daily or whenever the orientation of the head or the test geometry needs to be changed.

Force Factor

This calibration determines and records the conversion factor for the drive motor from machine units (DAC bits) into newtons (N). It should be performed at least once per month, depending on the level of usage of the instrument. A reference weight is required for this calibration; we recommend using part number N533-0315, which is designed to fit over the clamps on the driveshaft.

Spring Calibration

This calibration determines and records the stiffness and damping of the spring, which allows the drive characteristics to be determined. The drive characteristics have the greatest effect on results when samples of low stiffness are being measured in tension mode. If such samples are being analyzed then perform this calibration once a month. If you are using other geometry modes then it should be performed once a year, or to check if the instrument has been damaged for some reason.


This calibration corrects the response of the thermocouple using the result of melting a sample of indium.

PID Calibration

This calibration determines and records the values used by the temperature controller's control algorithm. It normally only needs to be performed when you are changing the type of furnace being used.

To calibrate the DMA 8000:

1. Click Calibration from the Method Editor and then click Calibrate Instrument. Five tabs are displayed, one for each calibration.

2. Perform the required calibrations (see below), and then click Save & Apply to apply all the calibrations.

3. Enter a filename for the calibration file, and click Save. The five tabs are updated to show the date for each calibration being applied in the software.

4. Click Close.

Calibration 161

Balance Zero calibration

1. Select the Balance Zero tab.

2. Enter your name in the Operator box to record who carried out the calibration.

3. Click Begin Calibration. The Balance/Zero Calibration dialog box is displayed.

4. When the dialog box shows that the instrument is Ready, click Start.

5. Follow the instructions on the screen. The head should be oriented in the position to be used in your experiment. The calibration progress is shown in the tab.

6. Click OK when complete, and then click Apply and Close.

Force Factor calibration

1. Select the Force Factor tab.


3. Click Begin Calibration. The Force Factor Calibration dialog box is displayed.

4. Enter the mass of the reference weight in grams.


6. Follow the instructions on the screen. The central tower of the DMA 8000 should be oriented in the vertical position for this calibration. The calibration progress is shown in the tab.

7. Place the reference weight on to the driveshaft when instructed to do so by the software, and click OK. You will then be prompted to remove the weight.


Spring calibration

1. Select the Spring Calibration tab.


3. Click Begin Calibration. The Spring Calibration dialog box is displayed.


5. Follow the instructions on the screen. The central tower of the DMA 8000 should be oriented in the horizontal position for this calibration. The calibration progress is shown in the tab.



Temperature calibration

1. Select the Temperature tab.


3. Enter expected and measured values for the ambient temperature and the measured indium melting onset temperature. The expected value for indium is 156.6 °C.

4. Click Apply and Close.

To measure the melting onset temperature of indium:

1. Flatten a piece of indium and place it in a material pocket (refer to the Hardware Help for further details).

2. Load the material pocket into the DMA 8000 using the single cantilever geometry mode.

3. Perform a temperature scan experiment between ambient temperature and 200 °C.

4. Analyze the data to find the onset temperature at the point where the stiffness or modulus changes suddenly, and use this value in the temperature calibration.

Calibration 163

PID calibration

1. Select the PID Calibration tab.


3. Click Begin Calibration. The PID Calibration dialog box is displayed.

4. Enter the Set Point value in °C. For isothermal work choose the temperature at which you will be working. If you are not doing primarily isothermal work, choose a temperature close to the transition point of your material or in the middle of the temperature range that you will be using. For general use a typical value of 100°C is adequate.

5. Click Start.

6. Follow the instructions on the screen. The environmental chamber should be at ambient temperature when starting this calibration. If you are using a cooling system, the starting temperature should be at least 70°C below the set point.

7. Click Apply and Close when complete.


Introduction to Calibration of the Pyris Diamond DSC

The Pyris Diamond DSC is calibrated when it is first installed by a PerkinElmer Service Engineer. The analyzer remains calibrated, even when the system is turned off, as long as there are no major changes to operating conditions (such as a cooling block temperature change or switching to a different purge gas). As part of maintaining proper operating conditions for your instrument, it is recommended also that the DSC be calibrated every three to six months after installation or whenever you change the sample holder.

Although instrument calibration will remain steady for several months over a given calibration range, it is advisable to check the calibration more frequently as part of your standard operating procedure. This can be done by setting up a Pyris Player to run your calibrants as samples. The data produced can be analyzed within Player using a tolerance test to confirm that the current calibration is still valid. An example of such a player is included on the install disk. What you need to know before starting the calibration

NOTE: For scanning rates higher than 100 °C/min, manual procedure is required to perform a Temperature Calibration.

To perform a Temperature calibration or the Heat Flow calibration of a DSC analyzer, you should use standard calibration reference materials. If your lab must comply with ISO 9000, PerkinElmer Instruments provides ISO 9000 compatible reference materials. Reference materials comply with ISO instrumentation calibration. Certified reference materials (CRM) are traceable to national or international standards through an unbroken chain of custody. Not every calibration material is a CRM. The reference materials usually used for ambient operation are indium and zinc, which are supplied with the instrument for calibration purposes. CRM can be ordered from NIST or GLB (United Kingdom). Other reference materials are also available from PerkinElmer Instruments. Please see the topic, Standard Reference Materials.

Before starting calibration, the sample and references furnaces should be checked to confirm that they are empty. Best calibration results will be obtained if the furnace lids are aligned correctly. Check that the required dry purge gas is flowing and that the cooling system has had time to equilibrate the sample holder before starting to calibrate the analyzer.

In addition, refer to the calibration information and precautions in the installation and hardware help. To start the Calibration wizard:

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


There are two different approaches to calibration:

• E-Z Cal

• Advanced Calibration

Calibration 165

Buttons in the Calibration wizard

Starts the E-Z Calibration wizard. E-Z Calibration is recommended for routine use of the instrument. It automates the calibration routine and requires only minimal user input.

Starts the Advanced Calibration wizard. Advanced Calibration is for experienced users and provides greater flexibility in calibration. The user can choose from a wider variety of standards and, in some cases, different algorithms.

Restores values for all calibrations to system defaults (where no correction is applied) and resets the instrument to the default calibrations. A message is displayed first allowing you to cancel this action.

Closes the wizard without making any changes to your current calibration.

How the Calibration wizard works

The Calibration wizard automates the instrument calibration by performing the data collection and calculations necessary for you. It does this by generating a Pyris Playlist and instrument method according to the parameters you select. The Playlist and method are then run and the calibration recalculated by the generated datable calibration data, method and Playlist (including complete history) are tracked and saved.

The calibration wizard also gives you the option of typing in values from previous runs and using them. In this case, you would use standard reference materials and collect data to enter in the calibration wizard. Perform a peak area with onset calculation for each data file. The onset temperature obtained is used in the temperature calibration. You can also use the heat of fusion value obtained in the enthalpy calibration. In the Advanced Calibration wizard, you then enter standard values and click on “Accept Standards” to recalculate and apply the calibration.

It is recommended that you save your calibrations. When you finish using the Calibration wizard, you are prompted to save the calibration file.


Jade DSC Calibration

There are two calibration routines for a Jade DSC:

• Temperature

• Heat Flow

The Jade DSC analyzer has been pre-calibrated at the factory for both temperature and heat flow. Temperature calibration and heat flow calibration should be checked using the precrimped samples of indium and zinc before obtaining data. Some conditions that could affect the current calibration of the Jade DSC:




4. If the Jade DSC has been turned off for a long time (that is, weeks or months), it may appear to require recalibration. If so, condition the analyzer by performing several heating and cooling runs with an empty sample holder, then check the calibration by running standard materials.

Before calibrating the Jade DSC, it is sometimes necessary to restore default calibration values. Typically, it is better to restore defaults when you are changing the temperature range that you are using. If you are changing the purge gas or flow rate, or if the analyzer has not been used for some time, restoring defaults may be necessary. The Temperature calibration can be slightly modified by running a new reference sample while the existing calibration is applied. You can restore default calibration values by selecting the appropriate calibration routine from the Restore menu while in the Calibration window. You can even restore all calibration values by selecting All. This activates the Save and Apply button; click on it and then, in the Save As dialog box, select the calibration file to be used or enter a new file name under which to save the values displayed in the calibration window.


For Temperature and Heat Flow calibrations, run high-purity reference materials (typically indium and zinc) with known temperature and energy transitions. The data obtained from these runs are used in the Pyris software calibration routines to calibrate the Jade DSC. Once the analyzer is calibrated, it will remain calibrated even when the system is turned off, as long as there are no changes in the operating conditions.

Calibration 167



1. From the Calibration dialog box select the Temperature tab. The Temperature page displays.

2. To perform the Jade DSC temperature calibration, complete a scan for each reference material under the same conditions that you use to run your samples.


4. Record the H ( J/ g) and Onset results; you will need the Onset result for Temperature calibration and you can use the H result for Heat Flow calibration.


6. Click on the check box in the “Use” column for each reference that is to be used in the calibration.

7. When all of the information has been entered, click on the Save and Apply button to save the calibration values and apply them. Go on to the next calibration procedure or select Close to close the Calibration window and begin using the new calibration values.




2. To perform the Jade DSC Heat Flow calibration, complete a scan for the reference material under the same conditions that you run your samples or use one of the scans completed for the Temperature calibration.

3. After the run is completed, perform a Peak Area calculation and record the H ( J/ g) result.


5. When all of the information has been entered, click on the Save and Apply button to save the calibration values and apply them. Select Close to close the Calibration window and begin using the new calibration values.

Calibration 169

Pyris 1 DSC Calibration

There are two calibration routines for a Pyris 1 DSC:

• Temperature

• Heat Flow

Once your Pyris 1 DSC is calibrated, it should remain so for a long time, provided there are no major changes in operating conditions. Conditions that could affect the current calibration are:



3. If you change the coolant or coolant accessory, you may need to recalibrate.

4. If the analyzer has been turned off for a long time (that is, weeks or months), it may appear to require recalibration. If so, condition the analyzer by performing several heating and cooling runs with an empty sample holder, then check the calibration by running standard materials.

Before calibrating the Pyris 1 DSC, it is sometimes necessary to restore default calibration values. Typically, it is better to restore defaults when you are changing the temperature range that you are using. If you are changing the purge gas or flow rate, or if the analyzer has not been used for some time, restoring defaults may be necessary. You can restore default calibration values by selecting the appropriate calibration routine from the Restore menu while in the Calibration window. You can even restore all calibration values by selecting All. This activates the Save and Apply button; click it and then, in the Save As dialog box, select the calibration file to be used or enter a new file name under which to save the values displayed in the calibration window.

For Temperature and Heat Flow calibrations, run high-purity reference materials (typically indium and zinc) with known temperature and energy transitions. The data obtained from these runs are used in the Pyris software calibration routines to calibrate the Pyris 1 DSC. Once the analyzer is calibrated, it will remain calibrated even when the system is turned off, as long as there are no changes in the operating conditions.




To perform the Pyris 1 DSC Temperature calibration, complete a scan for each reference material under the same conditions that you run your samples. After each run is completed, perform a Peak Area calculation and include the Onset temperature. Record the H (J/g) and Onset results; you will need the Onset result for Temperature calibration and you can use the H result for Heat Flow calibration.

When all of the reference materials have been run and calculations performed, enter the reference material name, expected onset temperature, measured onset temperature, and calibration method name in the table on the Temperature calibration page. Click the check box in the “Use” column for each reference that is to be used in the calibration.


Calibration 171


Select the Heat Flow tab to display the Heat Flow page of the Calibration window. A Heat Flow calibration uses a single standard. The Heat Flow calibration value can be slightly modified by running a new reference sample while the existing calibration is applied.

To perform the Pyris 1 DSC Heat Flow calibration, complete a scan for the reference material under the same conditions that you run your samples or use one of the scans completed for the Temperature calibration. After the run is completed, perform a Peak Area calculation and record the H (J/g) result.

Enter the reference material name, expected H, the measured H, weight of the reference material, and calibration method name in the Calibration table.


Pyris Software Guide

Running Samples


Running Samples

In Pyris Software, each analyzer’s Instrument Application contains a Method Editor, Control Panel, Instrument Viewer, and Status Panel. To run a sample using any analyzer, each of these parts of the software is used.

Using the Pyris Player feature of Pyris Software, you can create play lists that automate data collection and analysis for an analyzer with an autosampler. Play lists can also be created for analyzers without autosamplers. These lists would automate post-run data analysis on existing data files.

In general, the procedure for a typical experiment includes the following steps:

1. Start the Pyris system.

2. From the Pyris Manager, start the specific analyzer’s Instrument Application.

3. In the Method Editor, select an existing method or create a new method.

4. Load the sample in the analyzer.

5. Start the run from the Control Panel.

6. Monitor the run’s data collection in the Instrument Viewer and using the Status Panel.

7. Save the data.

8. Perform post-run analysis.

A Pyris Player play list for an analyzer with an autosampler can automate steps 3 through 8. All you need to do is prepare the sampler, place samples in the sample tray, set up the play list, and start the run.

Refer to the Hardware Help for guidance on preparing samples.

See how parts of the Pyris software are involved in running samples:

• Instrument Application

• Methods

• Pyris Player

• Control Panel

• Monitoring Data Collection

Running Samples 175

Instrument Applications

Instrument Applications

Each thermal analyzer installed and configured in your Pyris software is represented by a button on the Pyris Manager. Clicking a button opens the Pyris Instrument Application for that analyzer. The analyzer’s name, assigned in the Configuration utility, is displayed in the title bar of the Instrument Application window.

In addition to the standard Windows components (pull-down menus, toolbar, status line, control box, Minimize and Maximize buttons), an Instrument Application screen comprises the following main parts:

Method Editor

The Method Editor is used to create and set up methods for your sample runs. It comprises the following pages — Sample Info, Initial State, Program, and View Program — each indicated by a tab at the top of the Method Editor window. Clicking a tab displays that page.

Instrument Viewer

This window displays a curve representing the real-time signal from the instrument. Depending on what you select from the Curves menu, you can display more than one curve at a time. Appropriate axes labels are automatically added to the display. The display of the real-time signal can be toggled on and off by selecting Monitor from the View menu or the Monitor button from the toolbar.

Data Analysis Window

You can open a Data Analysis window while in an Instrument Application by clicking the Data Analysis button on the toolbar. It can also be opened from the Pyris Task menu seen by clicking the Start Pyris button. When you select Data Analysis, a Select Data File dialog box appears in which you indicate the file you want to open. The selected data file is displayed on which you can perform various calculations, for example, specific heat and purity. You can also display different types of curves from the data file, for example, Heat Flow, Baseline Flow, and Sample Temperature. Also part of the Data Analysis window is access to Remote Monitor with which you can monitor a remote analyzer.

Pyris Player

You can open a Pyris Player window while in an Instrument Application by clicking the Pyris Player button on the toolbar. When you select Pyris Player, the play list last used is displayed in the Edit Play List page. You can create a new play list, open another existing list, or edit the one displayed. The play lists seen here are analyzer-dependent, for example, if you are in the DSC 7 Instrument Application, then the play list files will have a .dsp extension and can be used only with a DSC 7.

Control Panel

This is a dockable panel (that is, it can be moved around the window) containing buttons with which you directly control the analyzer. The default position is the right-hand side of the screen. You can toggle the display of the panel by clicking Control Panel in the View menu. A checkmark is displayed next to that item when the Control Panel is displayed.


Standard Tools Toolbar

This dockable toolbar contains buttons to help you create and edit methods and have access to the other parts of an Instrument Application. Some buttons are grayed out depending on what window is active, for example, the New Method button is unavailable when the Instrument Viewer is the active window. The default position of the toolbar is across the top of the screen below the title bar. You can toggle the display of the toolbar by clicking Toolbar in the View menu. A checkmark is displayed next to that item when the standard toolbar is displayed.

Rescale Tools Toolbar

This is a dockable toolbar that contains buttons to tools that optimize the data displayed in the Data Analysis and Instrument Viewer windows. The default position of the toolbar is across the top of the screen below the standard toolbar and above the Status Panel. You can toggle the display of the toolbar by clicking Rescale Tools in the View menu. A checkmark is displayed next to that item when the Rescale Tools toolbar is displayed.

Status Panel

You can monitor the status of several analyzer parameters in this panel, whose default position is below the toolbars. You can toggle the display of the panel by clicking Status Panel in the View menu. A checkmark is displayed next to that item when the Status Panel is displayed.

Status Panel

The status panel is a dockable panel in an Instrument Application that displays the real-time status of selected parameters of the analyzer.

The panel is resizable so that you can display as many parameter boxes as desired. You can toggle the status panel on and off by selecting Status Panel from the View menu. Each parameter is displayed in a box that contains the parameter name in a drop-down list and the current value.

The parameters available for display depend on the analyzer you are using. To select a parameter to display in the status panel, you can highlight the display field and then type in the first letter of the parameter. This will display the first parameter that begins with that letter. Continue to type that letter to scroll through all parameters that begin with that letter. You can also select a parameter by displaying the drop-down list and highlighting the desired item.

Running Samples 177

DSC 8500 Instrument Application

The main parts of the DSC 8500 Instrument Application are:

• Instrument Viewer

• Method Editor

• Data Analysis

• Pyris Player

• Status Panel

• Control Panel

To move from one part of the Instrument Application to another, you can use the toolbar buttons:

Instrument Viewer

Method Editor

Data Analysis

Pyris Player

Instrument Viewer

The Instrument Viewer is a window that displays the real-time signals from the DSC 8500 as data are collected during a run. You can select the curves (signals) for display from the Curves menu. If there is no run in progress, the Instrument Viewer can be used to monitor the status of the instrument by activating Monitor from the View menu. If you click the Reset Monitor button in the control panel, the display in the Instrument Viewer is cleared and monitoring begins again. The display of the curves can be optimized by using the rescale tools on the Rescale Tools toolbar.

The Instrument Viewer window contains a title bar, control box with the standard Control menu, Minimize and Maximize buttons, and a border that can be used for resizing. The curves displayed in the window can be changed by selecting items on the Calibrate, View, Display, and Curves menus.

Method Editor

The DSC 8500 method is a set of parameters that determine the conditions under which the system will collect data on a sample. Any number of methods can be created and stored so that the parameters can be optimized to handle different analyses. Methods are also used in play lists. The play list can be set up to run many samples using the same method via the sample group. The Method Editor comprises the following pages, each of which contains its own set of parameters:

• Sample Info Page

• Initial State Page

• Program Page

• View Program Page


Another feature of the Method Editor is the Thermal Program Window.

Data Analysis

This application analyzes data collected by any analyzer. This application is not associated with a particular analyzer and can be used to analyze data and edit methods for any instrument attached to your thermal analysis system. More than one Data Analysis Application can be opened at a time.

The Data Analysis window is opened one of two ways:

• From the Start Pyris menu select Data Analysis. The Data Analysis window appears. Use the options on the File menu to display data files collected by different analyzers.

• You can also open the DSC 8500 Data Analysis window while in the Instrument Viewer

or Method Editor by selecting the Data Analysis tool bar icon . From the Open Data File dialog box select the data file you want displayed. Use the items in the File menu to open, add, close, and save a data file or to print the display.

The View, Display, Curves, Math, and Calc menus are used to change the display and the type of curve and to perform calculations on the data for additional information.

The Data Analysis window also contains the standard window items: title bar, control box with Control menu, Minimize and Maximize buttons, and a border that can be used for resizing.

NOTE: For more information on the Data Analysis window, refer to Data Analysis.

Pyris Player

Pyris Player is used to create play lists or sequences of commands that automate data collection and postrun data analysis functions. You can create a play list that prompts you through the steps necessary to run a sample or a series of samples (that is, Load Sample, Start Method, Remove Sample) and then performs a series of analyses on the data files, displays the results, and prints the results. Pyris Player's Sample Group feature, which includes a Sample List and a Data Analysis List, simplifies creation of a play list. For each Sample line in the Sample List, the program will pause in order for you to load or remove the sample since it does not detect an autosampler. The Sample List is a good way to group similar samples together to be analyzed by the same method. The items in the Data Analysis List can take the data file from the current run, preceding play list items, and existing files and perform the same procedures that are available in regular Data Analysis in a play list.

While a play list is running, you can perform other functions on your computer or pause the play list to edit entries below the current line. A complete history file is generated that contains the record of success or failure of each item in the list. If an error occurs, a reason is listed. There also is a sample history page that displays past and current information on the samples in the Sample Lists in the current play list.

See the following topics for more details on the parts of Pyris Player:

• Setup Page

• Edit Play List Page

Running Samples 179

• View List Page

• View Sample List Page

• View History Page

• Sample History Page

• Player Toolbars


DSC 8000 Instrument Application The main parts of the DSC 8000 Instrument Application are:


• Method Editor

• Data Analysis

• Pyris Player

• Status Panel

• Control Panel


Instrument Viewer

Method Editor

Data Analysis

Pyris Player

Instrument Viewer



Method Editor




• Program Page

Running Samples 181



Data Analysis





or Method Editor by clicking the Data Analysis tool bar icon . From the Open Data File dialog box, select the data file you want displayed. Use the items in the File menu to open, add, close, and save a data file or to print the display.



NOTE: For more information on the Data Analysis window, refer to Data Analysis

Pyris Player

Pyris Player is used to create play lists or sequences of commands that automate data collection and postrun data analysis functions. You can create a play list that prompts you through the steps necessary ro run a sample or a series of samples (that is, Load Sample, Start Method, Remove Sample) and then performs a series of analyses on the data files, displays the results, and prints the results. Pyris Player's Sample Group feature, which includes a Sample List and a Data Analysis List, simplifies creation of a play list. For each Sample line in the Sample List, the program will pause in order for you to load or remove the sample since it does not detect an autosampler. The Sample List is a good way to group similar samples together to be analyzed by the same method. The items in the Data Analysis List can take the data file from the current run, preceding play list items, and existing files and perform the same procedures that are available in regular Data Analysis in a play list.


See the following topics for more details on the parts of Pyris Player: Setup Page Edit Play List Page View List Page View Sample List Page View History Page


Sample History Page Player Toolbars

Running Samples 183



• Method Editor

• Data Analysis

• Pyris Player

• Status Panel

• Control Panel


Instrument Viewer

Method Editor

Data Analysis

Pyris Player

Instrument Viewer


The Instrument Viewer window contains a title bar, control box with the standard Control menu, Minimize and Maximize buttons, and a border that can be used for resizing. The curves displayed in the window can be changed by selecting items on the View, Display, and Curves menus.

Method Editor




• Program Page




Data Analysis





or Method Editor by selecting the Data Analysis tool bar icon . From the Open Data File dialog box select the data file you want displayed. Use the items in the File menu to open, add, close, and save a data file or to print the display.



NOTE: For more information on the Data Analysis window refer to Data Analysis.

Pyris Player

Pyris Player is used to create play lists or sequences of commands that automate data collection and postrun data analysis functions. You can create a play list that prompts you through the steps necessary to run a sample or a series of samples (that is, Load Sample, Start Method, Remove Sample) and then performs a series of analyses on the data files, displays the results, and prints the results. Pyris Player's Sample Group feature, which includes a Sample List and a Data Analysis List, simplifies creation of a play list. For each Sample line in the Sample List, the program will pause in order for you to load or remove the sample since if does not detect an autosampler. The Sample List is a good way to group similar samples together to be analyzed by the same method. The items in the Data Analysis List can take the data file from the current run, preceding play list items, and existing files and perform the same procedures that are available in regular Data Analysis in a play list.



• Setup Page


Running Samples 185

• View List Page




• Player Toolbars




• Method Editor

• Data Analysis

• Pyris Player

• Status Panel

• Control Panel


Instrument Viewer

Method Editor

Data Analysis

Pyris Player

Instrument Viewer

The Instrument Viewer is a window that displays the real-time signals from the DSC 4000 as data are collected during a run. You can select the curves (signals) for display from the Curves menu. If there is no run in progress, the Instrument Viewer can be used to monitor the status of the instrument by activating Monitor from the View menu. If you click on the Reset Monitor button in the control panel, the display in the Instrument Viewer is cleared and monitoring begins again. The display of the curves can be optimized by using the rescale tools on the Rescale Tools toolbar.


Method Editor




• Program Page

Running Samples 187



Data Analysis




• You can also open the DSC 4000 Data Analysis window while in the Instrument

Viewer or Method Editor by selecting the Data Analysis tool bar icon . From the Open Data File dialog box select the data file you want displayed. Use the items in the File menu to open, add, close, and save a data file or to print the display.




Pyris Player

Pyris Player is used to create play lists or sequences of commands that automate data collection and postrun data analysis functions. You can create a play list that prompts you through the steps necessary to run a sample or a series of samples (that is, Load Sample, Start Method, Remove Sample) and then performs a series of analyses on the data files, displays the results, and prints the results. Pyris Player's Sample Group feature, which includes a Sample List and a Data Analysis List, simplifies creation of a play list. For each Sample line in the Sample List, the program will pause in order for you to load or remove the sample if it does not detect an autosampler. The Sample List is a good way to group similar samples together to be analyzed by the same method. The items in the Data Analysis List can take the data file from the current run, preceding play list items, and existing files and perform the same procedures that are available in regular Data Analysis in a play list.



• Setup Page



• View List Page




• Player Toolbars

Running Samples 189

Pyris 1 TGA Instrument Application To learn more about the main parts of the Pyris 1 TGA Instrument Application, see each of the topics below:


• Method Editor

• Data Analysis

• Pyris Player

• Status Panel

• Control Panel


Instrument Viewer

Method Editor

Data Analysis

Pyris Player

Instrument Viewer

The Pyris 1 TGA Instrument Viewer is a window that displays the real-time signals from the Pyris 1 TGA as data are collected during a run. You can select the curves (signals) for display from the Curves menu. If there is no run in progress, the Instrument Viewer can be used to monitor the status of the instrument by activating Monitor from the View menu. If you click on the Reset Monitor button in the control panel, the display in the Instrument Viewer is cleared and monitoring begins again. The display of the curves can be optimized by using the rescale tools on the Rescale Tools toolbar.

The Instrument Viewer window contains a title bar, control box with the standard Control menu in the upper-left-hand corner, Minimize and Maximize buttons, and a border that can be used for resizing. The curves displayed in the window can be changed by selecting items on the View, Display, and Curves menus.

Method Editor

The Pyris 1 TGA method is a set of parameters that determine the conditions under which the system will collect data on a sample. Any number of methods can be created and stored so that the parameters can be optimized to handle different analyses. Methods are also used in play lists. The play list can be set up to run many samples using the same method via the sample group. This is especially convenient for use with the autosampler. The Method Editor comprises the following pages, each of which contains its own set of parameters:



• Program Page




Data Analysis

The Data Analysis window is opened one of two ways: First, you can select Data Analysis from the Start Pyris Task menu or from the Pyris Software group in the Program menu. The window displays the last data file displayed there. Use the options on the File menu to display data files collected by different analyzers.

Second, the instrument's Data Analysis window is opened while in the Instrument Viewer or

Method Editor by selecting the Data Analysis button from the toolbar. From the Open Data File dialog box select the data file you want displayed. Use the items in the File menu to open, add, close, and save a data file, or to print the display. The View, Display, Curves, Math, and Calc menus are used to change the display and the type of curve displayed and to perform calculations on the data for additional information.

The Data Analysis window also contains the standard window items: title bar, control box with Control menu in the upper-left-hand corner, Minimize and Maximize buttons, and a border that can be used for resizing.

Pyris Player

The Pyris Player is used to create play lists or sequences of commands that automate data collection and postrun data analysis functions. For a Pyris 1 TGA without an autosampler, you can create a play list that prompts you through the steps necessary to run a sample or a series of samples (that is, Load Sample, Start Method, Remove Sample) and then performs a series of analyses on the data files, displays the results, and prints the results. If your analyzer has an autosampler, Pyris Player can be used to tare all or specific sample pans and weigh all or specific samples in the autosampler tray. Pyris Player's Sample Group feature, which includes a Sample List and a Data Analysis List, automates running samples in the autosampler tray. The Sample List is a good way to group similar samples together to be analyzed by the same method. The Sample List can run the samples in the autosampler in any order. The items in the Data Analysis List can take the data file from the current run, preceding play list items, and existing files and perform the same procedures that are available in regular Data Analysis in a play list.

While a play list is running, you can perform other functions on your computer or pause the play list and edit the entries below the current line. A complete history file is generated that contains the record of success or failure or each item in the list. If an error occurs, a reason is listed. There also is a sample history page that displays past and current information on the samples in the sample groups in the current play list.

The parts of Pyris Player are

• Setup Page


• View List Page



Running Samples 191


• Player Toolbars


TGA 4000 Instrument Application

The main parts of the TGA 4000 Instrument Application are:


• Method Editor

• Data Analysis

• Pyris Player

• Status Panel

• Control Panel


Instrument Viewer

Method Editor

Data Analysis

Pyris Player

Instrument Viewer

The Instrument Viewer is a window that displays the real-time signals from the TGA 4000 as data are collected during a run. You can select the curves (signals) for display from the Curves menu. If there is no run in progress, the Instrument Viewer can be used to monitor the status of the instrument by activating Monitor from the View menu. If you click on the Reset Monitor button in the control panel, the display in the Instrument Viewer is cleared and monitoring begins again. The display of the curves can be optimized by using the rescale tools on the Rescale Tools toolbar.


Method Editor

The TGA 4000 method is a set of parameters that determine the conditions under which the system will collect data on a sample. Any number of methods can be created and stored so that the parameters can be optimized to handle different analyses. Methods are also used in play lists. The play list can be set up to run many samples using the same method via the sample group. The Method Editor comprises the following pages, each of which contains its own set of parameters:



Running Samples 193

• Program Page



Data Analysis

The Data Analysis window is opened one of two ways: First, you can select Data Analysis from the Start Pyris Task menu or from the Pyris Software group in the Programs menu. The window displays the last data file displayed there. Use the options on the File menu to display data files collected by different analyzers.

Second, the instrument's Data Analysis window is opened while in Instrument Viewer or

Method Editor by selecting the Data Analysis button from the toolbar. From the Open Data File dialog box select the data file you want displayed. Use the items in the File menu to open, add, close, and save a data file, or to print the display.

The View, Display, Curves, Math, and Calc menus are used to change the display and the type of curve displayed and to perform calculations on the data for additional information.



Pyris Player

The Pyris Player is used to create play lists or sequences of commands that automate data collection and postrun data analysis functions. You can create a play list that prompts you through the steps necessary to run a sample or a series of samples (that is, Load Sample, Start Method, Remove Sample) and then performs a series of analyses on the data files, displays the results, and prints the results. Pyris Player's Sample Group feature, which includes a Sample List and a Data Analysis List, simplifies creation of a play list. For each Sample line in the Sample List, the program will pause in order for you to load or remove the sample if it does not detect an autosampler. The Sample List is a good way to group similar samples together to be analyzed by the same method. The items in the Data Analysis List can take the data file from the current run, preceding play list items, and existing files and perform the same procedures that are available in regular Data Analysis in a play list.

While a play list is running, you can perform other functions on your computer or pause the play list to edit entries below the current line. A complete history file is generated that contains the record of success or failure of each item in the list. If an error occurs, a reason is listed. There also is a sample history page that displays past and current information on the samples in the Sample Lists in current play list.

The parts of Pyris Player are Setup Page Edit Play List Page View List Page View Sample List Page Sample History Page View History Page Player Toolbars


TGA 8000 Instrument Application

The main parts of the TGA 8000 Instrument Application are:


• Method Editor

• Data Analysis

• Pyris Player

• Status Panel

• Control Panel


Instrument Viewer

Method Editor

Data Analysis

Pyris Player

Instrument Viewer

The Instrument Viewer is a window that displays the real-time signals from the TGA 8000 as data are collected during a run. You can select the curves (signals) for display from the Curves menu. If there is no run in progress, the Instrument Viewer can be used to monitor the status of the instrument by activating Monitor from the View menu. If you click on the Reset Monitor button in the control panel, the display in the Instrument Viewer is cleared and monitoring begins again. The display of the curves can be optimized by using the rescale tools on the Rescale Tools toolbar. The Instrument Viewer window contains a title bar, control box with the standard Control menu, Minimize and Maximize buttons, and a border that can be used for resizing. The curves displayed in the window can be changed by selecting items on the View, Display, and Curves menus.

Running Samples 195

Method Editor

The TGA 8000 method is a set of parameters that determine the conditions under which the system will collect data on a sample. Any number of methods can be created and stored so that the parameters can be optimized to handle different analyses. Methods are also used in play lists. The play list can be set up to run many samples using the same method via the sample group. The Method Editor comprises the following pages, each of which contains its own set of parameters:



• Program Page



Data Analysis



• From the Start Pyris menu select Data Analysis. The Data Analysis window appears.

• Use the options on the File menu to display data files collected by different analyzers.

• You can also open the TGA 8000 Data Analysis window while in the Instrument

Viewer or Method Editor by selecting the Data Analysis tool bar icon . From the Open Data File dialog box select the data file you want displayed.

• Use the items in the File menu to open, add, close, and save a data file or to print the display.



Pyris Player

Pyris Player is used to create play lists or sequences of commands that automate data collection and post run data analysis functions. You can create a play list that prompts you through the steps necessary or run a sample or a series of samples (i.e., Load Sample, Start Method, Remove Sample) and then performs a series of analyses on the data files, displays the results, and prints the results. Pyris Player's Sample Group feature, which includes a Sample List and a Data Analysis List, simplifies creation of a play list. For each Sample line in the Sample List, the program will pause in order for you to load or remove the sample since


it does not detect an autosampler. The Sample List is a good way to group similar samples together to be analyzed by the same method. The items in the Data Analysis List can take the data file from the current run, preceding play list items, and existing files and perform the same procedures that are available in regular Data Analysis in a play list. While a play list is running, you can perform other functions on your computer or pause the play list to edit entries below the current line. A complete history file is generated that contains the record of success or failure of each item in the list. If an error occurs, a reason is listed. There also is a sample history page that displays past and current information on the samples in the Sample Lists in the current play list. See the following topics for more details on the parts of Pyris Player:

• Setup Page


• View List Page




• Player Toolbars

Running Samples 197

STA 8000 Instrument Application The main parts of the STA 8000 Instrument Application are:


• Method Editor

• Data Analysis

• Pyris Player

• Status Panel

• Control Panel To move from one part of the Instrument Application to another, you can use the toolbar buttons:

Instrument Viewer

Method Editor

Data Analysis

Pyris Player

Instrument Viewer The Instrument Viewer is a window that displays the real-time signals from the STA 8000 as data are collected during a run. You can select the curves (signals) for display from the Curves menu. If there is no run in progress, the Instrument Viewer can be used to monitor the status of the instrument by activating Monitor from the View menu. If you click the

Reset Monitor button in the control panel, the display in the Instrument Viewer is cleared and monitoring begins again. The display of the curves can be optimized by using the rescale tools on the Rescale Tools toolbar. The Instrument Viewer window contains a title bar, control box with the standard Control menu, Minimize and Maximize buttons, and a border that can be used for resizing. The curves displayed in the window can be changed by selecting items on the Calibrate, View, Display, and Curves menus.

Method Editor The STA 8000 method is a set of parameters that determine the conditions under which the system will collect data on a sample. Any number of methods can be created and stored so that the parameters can be optimized to handle different analyses. Methods are also used in play lists. The play list can be set up to run many samples using the same method via the sample group. The Method Editor comprises the following pages, each of which contains its own set of parameters:



• Program Page




Data Analysis


The Data Analysis window is opened in one of two ways:


• You can also open the STA 8000 Data Analysis window while in the Instrument Viewer

or Method Editor by clicking the Data Analysis tool bar icon . From the Open Data File dialog box select the data file you want displayed. Use the items in the File menu to open, add, close, and save a data file or to print the display.



NOTE: For more information on the Data Analysis window, refer to Data Analysis.

Pyris Player

Pyris Player is used to create play lists or sequences of commands that automate data collection and postrun data analysis functions. You can create a play list that prompts you through the steps necessary to run a sample or a series of samples (that is, Load Sample, Start Method, Remove Sample) and then performs a series of analyses on the data files, displays the results, and prints the results. Pyris Player's Sample Group feature, which includes a Sample List and a Data Analysis List, simplifies creation of a play list. For each Sample line in the Sample List, the program will pause in order for you to load or remove the sample. The Sample List is a good way to group similar samples together to be analyzed by the same method. The items in the Data Analysis List can take the data file from the current run, preceding play list items, and existing files and perform the same procedures that are available in regular Data Analysis in a play list.



• Setup Page


• View List Page

Running Samples 199




• Player Toolbars


STA 6000 Instrument Application The main parts of the STA 6000 Instrument Application are:


• Method Editor

• Data Analysis

• Pyris Player

• Status Panel

• Control Panel


Instrument Viewer

Method Editor

Data Analysis

Pyris Player

Instrument Viewer

The Instrument Viewer is a window that displays the real-time signals from the STA 6000 as data are collected during a run. You can select the curves (signals) for display from the Curves menu. If there is no run in progress, the Instrument Viewer can be used to monitor the status of the instrument by activating Monitor from the View menu. If you click the Reset Monitor button in the control panel, the display in the Instrument Viewer is cleared and monitoring begins again. The display of the curves can be optimized by using the rescale tools on the Rescale Tools toolbar.


Method Editor

The STA 6000 method is a set of parameters that determine the conditions under which the system will collect data on a sample. Any number of methods can be created and stored so that the parameters can be optimized to handle different analyses. Methods are also used in play lists. The play list can be set up to run many samples using the same method via the sample group. The Method Editor comprises the following pages, each of which contains its own set of parameters:



Running Samples 201

• Program Page



Data Analysis




• You can also open the STA 6000 Data Analysis window while in the Instrument

Viewer or Method Editor by selecting the Data Analysis toolbar icon . From the Open Data File dialog box select the data file you want displayed. Use the items in the File menu to open, add, close, and save a data file or to print the display.




Pyris Player

Pyris Player is used to create play lists or sequences of commands that automate data collection and postrun data analysis functions. You can create a play list that prompts you through the steps necessary to run a sample or a series of samples (that is, Load Sample, Start Method, Remove Sample) and then performs a series of analyses on the data files, displays the results, and prints the results. Pyris Player's Sample Group feature, which includes a Sample List and a Data Analysis List, simplifies creation of a play list. For each Sample line in the Sample List, the program will pause in order for you to load or remove the sample if it does not detect an autosampler. The Sample List is a good way to group similar samples together to be analyzed by the same method. The items in the Data Analysis List can take the data file from the current run, preceding play list items, and existing files and perform the same procedures that are available in regular Data Analysis in a play list.



• Setup Page



• View List Page




• Player Toolbars

Running Samples 203

DMA 8000 Instrument Application

The main parts of the DMA 8000 Instrument Application are


• Method Editor

• Data Analysis

• Pyris Player

• Status Panel

• Control Panel


Instrument Viewer

Method Editor

Data Analysis

Pyris Player

Instrument Viewer

The Instrument Viewer is a window that displays the real-time signals from the DMA 8000 as data are collected during a run. You can select the curves (signals) for display from the Curves menu. If there is no run in progress, the Instrument Viewer can be used to monitor the status of the instrument by activating Monitor from the View menu. If you click on the Reset Monitor button in the control panel, the display in the Instrument Viewer is cleared and monitoring begins again. The display of the curves can be optimized by using the rescale tools on the Rescale Tools toolbar.


Method Editor

The DMA 8000 method is a set of parameters that determine the conditions under which the system will collect data on a sample. Any number of methods can be created and stored so that the parameters can be optimized to handle different analyses. Methods are also used in play lists. The play list can be set up to run many samples using the same method via the sample group. The Method Editor comprises the following pages, each of which contains its own set of parameters:



• Program Page



Another feature of Method Editor is the Thermal Program Window.

Data Analysis


Second, the instrument's Data Analysis window is opened while in the Instrument Viewer or

Method Editor by selecting the Data Analysis button from the toolbar. Use the items in the File menu to open, add, close, and save a data file, or to print the display.


The Data Analysis window also contains the standard window items: title bar, control box with Control menu, Minimize and Maximize buttons, and a border that can be used for sizing.

Pyris Player

The Pyris Player is used to create play lists or sequences of commands that automate data collection and postrun data analysis functions. You can create a play list that prompts you through the steps necessary to run a sample or a series of samples (that is, Load Sample, Start Method, Unload Sample) and then performs a series of analyses on the data files, displays the results, and prints the results. Pyris Player's Sample Group feature, which includes a Sample List and a Data Analysis List, simplifies creation of a play list. For each Sample line in the Sample List, the program will pause in order for you to load or remove the sample since it does not detect an autosampler. The Sample List is a good way to group similar samples together to be analyzed using the same method. The items in the Data Analysis List can take the data file from the current run, preceding play list items, and existing files and perform the same procedures that are available in regular Data Analysis in a play list.



• Setup Page


• View List Page




• Player Toolbars

Running Samples 205

Diamond DSC Instrument Application The main parts of the Diamond DSC Instrument Application are:


• Method Editor

• Data Analysis

• Pyris Player

• Status Panel

• Control Panel


Instrument Viewer

Method Editor

Data Analysis

Pyris Player

Instrument Viewer

The Instrument Viewer is a window that displays the real-time signals from the Diamond DSC as data are collected during a run. You can select the curves (signals) for display from the Curves menu. If there is no run in progress, the Instrument Viewer can be used to monitor the status of the instrument by activating Monitor from the View menu. If you click the Reset Monitor button in the control panel, the display in the Instrument Viewer is cleared and monitoring begins again. The display of the curves can be optimized by using the rescale tools on the Rescale Tools toolbar.



Method Editor

The Diamond DSC method is a set of parameters that determine the conditions under which the system will collect data on a sample. Any number of methods can be created and stored so that the parameters can be optimized to handle different analyses. Methods are also used in play lists. The play list can be set up to run many samples using the same method via the sample group. The Method Editor comprises the following pages, each of which contains its own set of parameters:



• Program Page



Data Analysis

The Data Analysis window is opened one of two ways. First, you can select Data Analysis from the Start Pyris Task menu or from the Pyris Software group in the Programs menu. The window displays the last data file displayed there. Use the options on the File menu to display data files collected by different analyzers.

Second, the Diamond DSC Data Analysis window is opened while in the Instrument Viewer or




Pyris Player

The Pyris Player is used to create play lists or sequences of commands that automate data collection and postrun data analysis functions. For a Diamond DSC without an autosampler, you can create a play list that prompts you through the steps necessary to run a sample or a series of samples (that is, Load Sample, Start Method, Remove Sample) and then performs a series of analyses on the data files, displays the results, and prints the results. If your analyzer has an autosampler, the play list's Sample Group feature, which includes a Sample List and a Data Analysis List, automates running samples in the autosampler's tray. The Sample List is a good way to group similar samples together to be analyzed using the same method. The Sample List can run the samples in the autosampler in any order. The items in the Data Analysis List can take the data file from the current run, preceding play list items, and existing files and perform the same procedures that are available in regular Data Analysis in a play list.

While a play list is running, you can perform other functions on your computer or pause the play list and edit the entries below the current line. A complete history file is generated that

Running Samples 207

contains the record of success or failure or each item in the list. If an error occurs, a reason is listed. There also is a sample history page that displays past and current information on the samples in the sample groups in the current play list.


• Setup Page


• View List Page




• Player Toolbars


Jade DSC Instrument Application The main parts of the Jade DSC Instrument Application are:


• Method Editor

• Data Analysis

• Pyris Player

• Status Panel

• Control Panel


Instrument Viewer

Method Editor

Data Analysis

Pyris Player

Instrument Viewer

The Instrument Viewer is a window that displays the real-time signals from the Jade DSC as data are collected during a run. You can select the curves (signals) for display from the Curves menu. If there is no run in progress, the Instrument Viewer can be used to monitor the status of the instrument by activating Monitor from the View menu. If you click on the Reset Monitor button in the control panel, the display in the Instrument Viewer is cleared and monitoring begins again. The display of the curves can be optimized by using the rescale tools on the Rescale Tools toolbar.


Method Editor

The Jade DSC method is a set of parameters that determine the conditions under which the system will collect data on a sample. Any number of methods can be created and stored so that the parameters can be optimized to handle different analyses. Methods are also used in play lists. The play list can be set up to run many samples using the same method via the sample group. The Method Editor comprises the following pages, each of which contains its own set of parameters:



• Program Page

Running Samples 209



Data Analysis


The Data Analysis window is opened in one of two ways:


• You can also open the Jade DSC Data Analysis window while in the Instrument

Viewer or Method Editor by selecting the Data Analysis tool bar icon . From the Open Data File dialog box select the data file you want displayed. Use the items in the File menu to open, add, close, and save a data file or to print the display.



NOTE: For more information on the Data Analysis window refer to Data Analysis

Pyris Player

Pyris Player is used to create play lists or sequences of commands that automate data collection and postrun data analysis functions. You can create a play list that prompts you through the steps necessary to run a sample or a series of samples (that is, Load Sample, Start Method, Remove Sample) and then performs a series of analyses on the data files, displays the results, and prints the results. Pyris Player's Sample Group feature, which includes a Sample List and a Data Analysis List, simplifies creation of a play list. For each Sample line in the Sample List, the program will pause in order for you to load or remove the sample since it does not detect an autosampler. The Sample List is a good way to group similar samples together to be analyzed by the same method. The items in the Data Analysis List can take the data file from the current run, preceding play list items, and existing files and perform the same procedures that are available in regular Data Analysis in a play list.



• Setup Page



• View List Page




• Player Toolbars

Running Samples 211

Pyris 1 DSC Instrument Application The main parts of the Pyris 1 DSC Instrument Application are:


• Method Editor

• Data Analysis

• Pyris Player

• Status Panel

• Control Panel


Instrument Viewer

Method Editor

Data Analysis

Pyris Player

Instrument Viewer

The Instrument Viewer is a window that displays the real-time signals from the Pyris 1 DSC as data are collected during a run. You can select the curves (signals) for display from the Curves menu. If there is no run in progress, the Instrument Viewer can be used to monitor the status of the instrument by activating Monitor from the View menu. If you click on the Reset Monitor button in the control panel, the display in the Instrument Viewer is cleared and monitoring begins again. The display of the curves can be optimized by using the rescale tools on the Rescale Tools toolbar.



Method Editor

The Pyris 1 DSC method is a set of parameters that determine the conditions under which the system will collect data on a sample. Any number of methods can be created and stored so that the parameters can be optimized to handle different analyses. Methods are also used in play lists. The play list can be set up to run many samples using the same method via the sample group. The Method Editor comprises the following pages, each of which contains its own set of parameters:



• Program Page



Data Analysis


Second, the Pyris 1 DSC Data Analysis window is opened while in the Instrument Viewer or




Pyris Player

The Pyris Player is used to create play lists or sequences of commands that automate data collection and postrun data analysis functions. For a Pyris 1 DSC without an autosampler, you can create a play list that prompts you through the steps necessary to run a sample or a series of samples (that is, Load Sample, Start Method, Remove Sample) and then performs a series of analyses on the data files, displays the results, and prints the results. If your analyzer has an autosampler, the play list's Sample Group feature, which includes a Sample List and a Data Analysis List, automates running samples in the autosampler's tray. The Sample List is a good way to group similar samples together to be analyzed using the same method. The Sample List can run the samples in the autosampler in any order. The items in the Data Analysis List can take the data file from the current run, preceding play list items, and existing files and perform the same procedures that are available in regular Data Analysis in a play list.

While a play list is running, you can perform other functions on your computer or pause the play list and edit the entries below the current line. A complete history file is generated that

Running Samples 213

contains the record of success or failure or each item in the list. If an error occurs, a reason is listed. There also is a sample history page that displays past and current information on the samples in the sample groups in the current play list.


• Setup Page


• View List Page




• Player Toolbars


Methods

A method is a set of parameters that determine how the system will collect data on a given sample. Any number of methods can be generated and stored so that the parameters can be optimized to handle different analyses. A default method is included with Pyris Software. You can edit this method and then save it under a new method name.

Methods are created and managed in the Method Editor. The Method Editor can be opened in both an Instrument Application and the Data Analysis Application by selecting the Method

Editor button in the toolbar ( ). In an Instrument Application, you can edit only those methods that control that instrument. In the Data Analysis Application, you can edit a method for any instrument attached to your system. You can load a method for another instrument type while in Data Analysis by using the Open Method command from the File menu. In the Open Method dialog box, select the instrument type from the List Files Type box and then select a file from the list of available methods.

Methods can also be part of a play list created with Pyris Player. Just as with individual runs, the methods in the list contain the information necessary to run the sample that has been loaded into the sample holder via a Load Sample entry in the play list.

The Method Editor contains different pages in which you enter information needed for the sample run. The parameters displayed on each page depend on the analyzer. The pages of the Method Editor are described below.

Sample Info Page

This page contains information about the sample to be run such as operator ID, sample name, weight (for TGA analyzers), dimensions (for DMA/TMA analyzers), measuring system and geometry of the sample (DMA/TMA analyzers), and location and name of the file in which to save the run's data. If you do not fill a location and file name, Pyris will use the defaults entered in the Save page of Preferences.

Initial State Page

This page contains the settings to be used at the start of the run such as temperature, forces, force controls, purge gas selection, equilibration, and baseline file. By selecting different pre-run actions, you can switch purge gases and flow rates, equilibrate before the run starts, and trigger actions based on signals to or from an external relay box

Program Page

This page is where you set up the temperature and time program and the gas program for your sample run. The main section of this page is Method Steps. You add, insert, or delete individual steps to build the temperature and time program. The method steps are listed in order as you create the program. The page also contains the scan rate and end conditions.

By selecting different actions and events in your method, you can switch purge gases and flow rates, equilibrate during any program step, trigger actions based on signals to or from an external relay box, and time when you want actions to occur during the method. These settings can be edited using the buttons on the right of the page, or by right-clicking a step in the method.

Running Samples 215

View Program Page

This page shows you the selections you made on the Initial State page and Program page in one view. To modify any segment in the program, double-click the item. This will display the appropriate page (Initial State or Program) where you can make editing changes.


Sample Info Page

The Sample Info page appears when you select the Sample Info tab of the Method Editor. This page contains the following sections:

Enter Sample Info Section

Sample ID

Enter a sample name of up to 512 characters. The entry field scrolls horizontally as you type.

Operator ID

Enter the name of the person who will run the experiment; the name can be up to 512 characters. The entry field scrolls horizontally as you type.

Comment

Enter any additional information about the sample or run; the entry can be a maximum of 512 characters. The entry field automatically wraps horizontally and scrolls vertically. Start typing on a new line by pressing Enter.

Enter Sample Weight Section

Weight

Enter the weight of the sample in milligrams. The default value is 1.000 mg.

For TGA and STA methods, you can have the analyzer read the sample weight by using the Sample Weight button in the control panel. The Sample Weight signal button in the control panel will take precedence over the user's entered value.

Zero (DSC 8000 and DSC 8500)

Sets the Heat Flow signal to zero. The Heat Flow Zero value is read directly from the analyzer by selecting the Heat Flow Zero Weight button in the control panel; the value appears in the Zero field. You can also enter a value in the Zero edit field and click away from the Method Editor window or use the tab key to accept the value (click away or tab to lose focus from the edit field box in order to accept the entered value). The Heat Flow Zero Signal button in the control panel will take precedence over the entered value.

Zero (TGA only)

The zero weight value is read directly from the analyzer by selecting the Zero Weight button in the control panel; the value appears in the Zero field. You can also enter a value in the Zero edit field and click away from the Method Editor window or use the tab key to accept the value. The Zero Weight signal button in the control panel will take precedence over the user's entered value. The default value is 0.000 mg. This value is the weight of the empty sample pan either on the hangdown wire for the Pyris 1 TGA or on the sample holder for the TGA 4000. The value is used to tare the weight of the sample pan before loading the sample.

Running Samples 217

DTA Zero (STA only)

Sets the microvolt signal to zero. The DTA Zero value is read directly from the analyzer by clicking the DTA Zero Signal button in the control panel; the value appears in the DTA Zero field. You can also enter a value in the DTA Zero edit field box and click away from the Method Editor window or use the tab key to accept the value. The DTA Zero Signal button in the control panel will take precedence over the user's entered value.

Save Data As Section

File Name

This field is for the name of the file in which the data collected from the run will be saved. You can enter the file name directly in this field or in the Browse dialog box. A Pyris software default file name ( QSAVE.xxD) is used if you do not specify a default file name in the Save Preferences page. The validity of the drive\directory\file name is checked when the data are saved. You can also use incremental file names, for example, if you enter <user-defined file name>### in the File Name field, the data file saved is <user-defined file name> xxx, where xxx starts at 000 and is incremented each time the method is used. This feature is useful when creating a Sample List in the Player Editor. If you do not specify the incremental file name and reuse the method without changing the file name entered, then Pyris Software will append a date – time stamp to the end of the user-defined file name in order to give the data file a unique file name and avoid overwriting an existing file. The format of the file name is <user-defined name>@ YYMMDDHHMMSS.xxD, where YY is the year, MM the month, DD the day, HH the hour (on a 240-hour clock), MM the minutes, and SS the seconds; xx in the extension represents the two-character code for the analyzer and D means data.

Browse

If you want to select a directory other than the default for storing the data file, click on the Browse button to display the Browse dialog box.

Directory

This field displays the drive and directory in which the data are saved after the run. This value reflects the disk\directory chosen in the Browse dialog box. If you do not select a specific directory, the default will be displayed.

Enter Sample Dimensions (DMA 8000 only)

Measuring System/Geometry

From the drop-down list displayed when you click on the down arrow, select the measuring system that you are using in the analyzer and the associated geometry of the sample. The availability of the other fields displayed in this section depends on this selection. Refer to the DMA 8000 Hardware Help for more information on the geometries available.

Height

The sample height (in mm) is entered manually by the user. A default value of 10 mm is shown when the method is opened.

Length

The sample length (in mm) (for an extension measuring system) is entered by the user. A default value of 15 mm is shown when the method is opened.


Thickness

This dimension is the thickness (in mm) of one of the two samples used with a shear measuring system. It is entered by the user. A default value of 3 mm is shown when the method is opened.

Diameter

This diameter (in mm) (for cylindrical or disk-shaped samples) is entered by the user. A default value of 3 mm is shown when the method is opened.

Initial State Page

The Initial State page appears when you select the Initial State tab of the Method Editor. On this page, you specify the initial conditions that are necessary before data is collected. This page is divided into the following sections:

• Pre-Run Actions

• Set Initial Values

• Data Collection

• Baseline File

Pre-Run Actions

In this section, you can select pre-run actions and events. An action defines what will occur during system initialization. For each action, you select one or more events that will cause that action to happen.

Table 1: Actions you can select on the Initial State page:

Action What the action means

Start Run

You can start the run when one or more of the available events has occurred. Your options are to start the run when equilibration conditions have been reached, at a specified time, immediately, or when a signal is received from an external relay box.

Switch Gases You can switch to another purge gas or change the gas flow rate if your system is using a GSA 7, TAGS, or Air Cooling Unit for changing purge gases. On the Initial State page, the gas and flow rate selected are used during system initialization.

NOTE: On the Program page, the purge gas and flow rate can be changed in a gas program. You can also change the purge gas in real time by selecting a different gas in the Purge Gas field in the control panel.

Trigger External Action

This action will trigger a signal to a channel on an external relay box or an X-10 box. (This item is not available for the DMA.)

Running Samples 219

Table 2: Events you can select on the Initial State page:

Event What the event means

A Signal equilibrates In general, when you select an equilibration event, the software will monitor the addressed signal from the analyzer until the peak-to-peak range of the signal is within the specified criterion for 20 seconds (10 consecutive readings, each 2-s intervals)

An External Event occurs

A signal is received from a channel on an external relay box or an X-10 box that triggers the action to occur. (This item is not available for the DMA.)

A Specified Time is reached

The action will occur once a specified time after the program segment starts.

Action occurs Immediately

The action will occur immediately when the program segment starts.

To select pre-run actions and events:

1. Position the mouse cursor in the Pre-Run Actions section and click the right mouse button.

2. A pop-up menu appears. Select Add an Action.

3. A dialog box appears that asks you to select an action. For information on each action, refer to Table 1 above.

4. If you selected the actions of Switch Gases or Trigger an External Action, you will need to specify additional information in the next dialog box that appears.

5. A dialog box appears that asks you to select an event. For information on each event, refer to Table 2 above.

Set Initial Values Section

Temperature

This field displays the initial temperature, that is, the temperature of the thermocouple and the sample’s environment when the run starts. The default value displayed is the Load Temperature value entered in the Instrument page in Preferences. Type a new value or use the spin buttons to increase or decrease the displayed temperature in 5°C steps. This value is used in the first step of the method program on the Program page.

Y Initial

Enter the initial ordinate (Y) value. Type the value or use the spin buttons to increase or decrease the displayed value in 5-mW steps.

Data Collection Section

Sample Rate (Pyris 1 DSC, DSC 8000/8500)

Select the sample rate of Standard or Fast from the drop-down list box. This is the rate at which data are collected throughout the run. The standard data collection rate is 5 points per second; the fast rate is 20 points per second. Proper selection of a sample rate will increase the efficiency of the analysis. Generally, the slower scanning rate improves peak resolution while the fast scanning rate improves the usable sensitivity. The number of points saved in


the date file also depends on the Data Sampling Options in the Step Details section of the Program page.

Baseline File Section

Baseline subtraction performs a linear subtraction of the instrument baseline from a curve to improve the resolution of the transition of interest. Instrument baseline is established by placing empty sample pans in the sample and reference holders and performing a run under similar conditions that you run your samples. The data file saved is a baseline file. One should scan the analyzer under the proposed experimental conditions to check the curvature and noise level of the instrument baseline before analyzing samples. When you are going to run a sample, you can have the software perform a baseline subtraction using a baseline file that you collected. The Baseline File section of the Initial State page contains the following parameters:

Use Baseline Subtraction check box

Click on the check box to activate Baseline Subtraction. The baseline file selected here is subtracted from the data as it is collected to optimize the data. When you select Baseline Subtraction, the Browse button becomes selectable.

Directory

Displays the drive and directory in which the baseline file is stored. You cannot enter the drive/directory directly; you must use the Browse button to find and select the drive/directory.

File Name

Enter the name of the baseline file to be used for the run or select the file from the Browse box.

Browse

Activated when you click on the Baseline Subtraction check box. If you want to select a directory other than the default for storing the data file, click on the Browse button to display the Browse dialog box.

Running Samples 221

Initial State Page for DMA 8000

The Initial State page appears when you select the Initial State tab of the Method Editor. On this page, you specify the initial conditions that are necessary before data is collected. This page is divided into the following sections:

Pre-Run Actions Set Initial Values

Pre-Run Actions

In this section, you can select pre-run actions and events. An action defines what will occur during system initialization. For each action, you select one or more events that will cause that action to happen.

Table 1: Actions you can select on the Initial State page:


Start Run

You can start the run when one or more of the available events has occurred. Your options are to start the run when equilibration conditions have been reached, at a specified time, or immediately.

Switch Gases You can switch to another purge gas or change the gas flow rate if your system is using a GSA 7, TAGS, or Air Cooling Unit for changing purge gases. On the Initial State page, the gas and flow rate selected are used during system initialization.

NOTE: On the Program page, the purge gas and flow rate can be changed in a gas program.

Trigger an External Action

This action will trigger a signal to a channel on an external relay box or an X-10 box.

Table 2: Events you can select on the Initial State page:


A Signal equilibrates In general, when you select an equilibration event, the software will monitor the addressed signal from the analyzer until the peak-to-peak range of the signal is within the specified criterion for 20 seconds (10 consecutive readings, each 2-s intervals).





To select pre-run actions and events:

1. Position the mouse cursor in the Pre-Run Actions section and click the right mouse button.

2. A pop-up menu appears. Select Add an Action.


3. A dialog box appears that asks you to select an action. For information on each action, refer to Table 1 above.


5. A dialog box appears that asks you to select an event. For information on each event, refer to Table 2 above.

Set Initial Values

Temperature

This field displays the initial temperature, that is, the temperature of the thermocouple and the sample’s environment when the run starts. The default value displayed is the Load Temperature value entered in Preferences. Type a new value or use the spin buttons to increase or decrease the displayed temperature in 5°C steps. This value is used in the first step of the method program on the Program page.

Drive Control Mode

This field displays the control mode for the driveshaft of the DMA 8000. Each mode is used for specific types of analysis:

None: Use this mode for bending and shear experiments.

Auto Tension: This is the best choice for tension experiments, because it prevents the sample being stretched to breaking point. Set the Static Force to -1 N to bring the driveshaft forward, and clamp the front fixed clamp with the sample in this position.

Ratio Tension/3pt Bending/Ratio Compression: These modes apply a static force, equal to the dynamic force multiplied by a force multiplier. An additional static force can also be added (set in Preferences).

Static Force (N)

The initial value of the static force applied when no drive control mode is selected.

Dynamic Force (N)

When the DMA 8000 is in Stress mode (as shown by the icon in the Control Panel), you can enter the initial dynamic force to be used in the experiment.

Frequency (Hz)

The initial value of the frequency to be used in the experiment.

Force Multiplier (no effect in auto tension mode)

The factor by which the dynamic force is multiplied to generate the static force applied to the sample in the Ratio Tension/3pt Bending/Ratio Compression modes.

Running Samples 223

Strain (mm)

When the DMA 8000 is in Strain mode (as shown by the icon in the Control Panel), you can enter the initial strain (displacement) to be used in the experiment.

Displacement Meter

Shows the position of the drive shaft in relation to its parked position. Use this to adjust the center knife when using 3-point bending geometry. The knife is adjusted correctly when the displacement marker is in line with the zero point marker, that is, the knife is just touching the sample across its entire width without applying any force.


Program Page

The Program page appears when you select the Program tab of the Method Editor. This page contains the following sections:

Method Steps Section Initial Temperature

Displays the initial temperature entered in the Initial State page. Change the value by typing in the entry field or using the spin buttons. If you change the initial temperature here, the value will be updated on the Initial State page and in the first step in the method program. If you change the Temperature in the Initial State page, the method program is adjusted accordingly.

List of Method Steps

The steps of the method program are listed in the order in which they will occur. If you are creating a new method, a default step is listed initially. The initial temperature entered in the Initial State page is used in the first step. The first step is highlighted upon entering the Program page. Select a step in this list to highlight it for editing. Use the buttons to the right of the list to add, insert, or delete a step. The type of step you add or insert may affect the steps already listed.

Add a Step

Displays the Method Step Options dialog box, in which you select the type of step you wish to append to the program. The types of steps available for selection vary with the type of analyzer you are using.

Insert a Step

Displays the Method Step Options dialog box in which you select the type of step to insert immediately before the highlighted step in the list of method steps.

Delete Item

Deletes the highlighted step, action, or event from the method. If you delete a step, the remaining program must be a continuous temperature program.

Add Action

An action is an item you select that you want the system to execute during the program.

Add Event

For each action, you can select one or more events. An event is an item you select that will cause an action to happen.

End Condition

Displays the Set End Condition box in the Edit Step section of the Program page. Here you specify the end condition for your method.

mk:@MSITStore:C:%5CProgram%20Files%20(x86)%5CPerkinElmer%5CPyris%5CPyris.chm::/pyr00275.htm

mk:@MSITStore:C:%5CProgram%20Files%20(x86)%5CPerkinElmer%5CPyris%5CPyris.chm::/pyr00272.htm#Set_End_Condition_Section

Running Samples 225

Edit Step Section

The Edit Step section displays editable parameters for the highlighted step in the method. The types of steps available for selection depend on the type of analyzer you are using.

Edit TMA Program Step (Diamond TMA only) Edit Temperature Scan Step Edit AutoStepwise Scan Step (TGA only) Edit Variable Rate Scan Step (TGA 8000 only) Edit Isothermal Step Edit Repeat Steps Edit StepScan Scan Iso Step (DSC 6000, Diamond DSC and Pyris 1 DSC only) Display Temperature Graph

Method Actions and Events

You can select actions and events for any program step. An action defines what will occur during system initialization. For each action, you select one or more events that will cause that action to happen.

Table 1: Actions you can select on the Program page


Stop Run You can stop the run when one or more of the available events has occurred. Your options are to stop the run when equilibration conditions have been reached, when a signal crosses a boundary, at a specified time, immediately, or when a signal is received from an external relay box.

Switch Gases You can switch to another purge gas or change the gas flow rate if your system is using a GSA 7, TAGS, or Air Cooling Unit for changing purge gases.


This action will trigger a signal to a channel on an external device. (This item is not available for the DMA or DTA.)

Table 2: Events you can select on the Program page


A Signal equilibrates In general, when you select an equilibration event, the software will monitor the addressed signal from the analyzer until the peak-to-peak range of the signal is within the specified criterion for 20 seconds (10 consecutive readings, each 2-s intervals)

A Signal Crosses a Boundary

In general, when you select a cross-boundary event, the software will monitor the addressed signal from the analyzer and cause the specified action to occur if the signal crosses an upper or lower boundary.

An External Event A signal is received from a channel on an external relay box that triggers the action to occur. (This item is not available for the DMA





mk:@MSITStore:C:%5CProgram%20Files%20(x86)%5CPerkinElmer%5CPyris%5CPyris.chm::/Edit%20StepScan%20Scan%20Iso%20Step.htm

mk:@MSITStore:C:%5CProgram%20Files%20(x86)%5CPerkinElmer%5CPyris%5CPyris.chm::/Meth_Temperature_Graph.htm


occurs or DTA.)

A Specified Temperature is reached

The action will occur once a specified temperature after the program segment starts.





To select method actions and events

1. Click on the Add Action button. Or, position the mouse cursor in the Method Steps section and click the right mouse button. A pop-up menu appears. Select Add an Action.

2. A dialog appears that asks you to select an action. For information on each action, refer to Table 1 above.

3. If you selected the actions of Switch Gases or Trigger an External Action, you will need to specify additional information in the next dialog that appears.

4. A dialog appears that asks you to select an event. For information on each event, refer to Table 2 above.

Set End Condition Section

The Set End Condition parameters are the conditions that the analyzer is to obtain at the end of a run:

Go To Load Temperature

Selects the load temperature entered in Instrument page in Preferences as the end condition for the current method. At the end of the run, the analyzer will be programmed to this temperature.

Hold

At the end of the run, the analyzer will hold at its current temperature.

Go To Temperature

Selects a user-entered temperature as the end condition and enables the Temperature entry field.

Turn Off Cover Heater check box (Pyris 1 DSC, DSC 8000, DSC 8500)

Programs the cover heater to turn off at the end of the current method.

Turn cooler off check box (DSC 8000, DSC 8500)

Programs the cooling device to turn off at the end of the current method.

mk:@MSITStore:C:%5CProgram%20Files%20(x86)%5CPerkinElmer%5CPyris%5CPyris.chm::/pyr00272.htm#T1_PR

mk:@MSITStore:C:%5CProgram%20Files%20(x86)%5CPerkinElmer%5CPyris%5CPyris.chm::/pyr00272.htm#T2_PR

Running Samples 227

Turn Off CryoFill (DSC 6000, Pyris 1 DSC and Jade DSC)

Programs the CryoFill to turn off at the end of the run. When this feature is enabled, a sensor in the LN2 dewar in the analyzer detects the level of the LN2. If it drops below a certain level, the system will automatically bring in LN2 from the supply tank until it reaches the designated level.

Pyris allows extra End Conditions for the Diamond TMA applied force. They are the same for TMA Standard and TMA Hi-Temperature, see Diamond TMA Set End Condition.

Step Info Section

The Step Info section contains the following controls:

Detail

Enter a comment or identification for the highlighted step, up to 40 characters.

Total points in Run

The total number of points in the run, calculated from all steps in the method. This value is automatically updated if you change the data sampling options.

If the method contains a StepScan step, the Total Points in Run value is affected by entries made in 2nd Temp, Rate, Isothermal, and Reps. An increase or decrease of any one of these parameters increases or decreases the total number of points in the run.

Sample Rate

Displays the sample rate (Standard or Fast) selected in the Data Collection section of the Initial State page (if configurable).

Data Sampling Options

For DSC analyzers, this field displays the data sampling option based on the sample rate selected in the Data Collection section of the Initial State page and enables the Select Value entry field. For the Fast sample rate, the only option is Data On. For the Standard sample rate, and for all other analyzers, the options are Seconds Between Points and Number of Points.

Select Value

Depending on the Data Sampling Option, this field displays the seconds between data points collected in the data file or the number of points in the data file. Use the spin buttons to increase or decrease the displayed value. The Total points in Run value, displayed for some analyzers, is adjusted accordingly. The smaller the number of seconds between points, the more data points collected. If the number of points collected is small, you may miss an important event in the run.

If the method contains a StepScan step, the Select Value entry is affected by 2nd Temp, Rate, Isothermal, and Reps, if Data Sampling Options is Number of Points. If you increase or decrease any one of these parameters, the Select Value entry is adjusted accordingly.

End Temperature

This value is displayed for StepScan steps. It is the temperature at the end of the last repetition of scan-iso. It is determined by the Initial Temp, 2nd Temp, and the number of repetitions. If any one of these parameters is changed, the End Temperature value is recalculated and displayed dynamically. The End Temperature cannot exceed the maximum allowed for the instrument, that is, 725 °C for the Pyris 1 DSC.

mk:@MSITStore:C:%5CProgram%20Files%20(x86)%5CPerkinElmer%5CPyris%5CPyris.chm::/Diamond_TMA/Diamond_TMA_Set_End_Condition.htm


Total Time

This value is displayed for StepScan steps. It is the total time is takes to run all of the repetitions of the scan-iso steps. It is determined by the 2nd Temp, Rate, Isothermal, and number of repetitions. If you increase or decrease any one of these parameters, the Total Time is adjusted dynamically.

AutoStepwise Step Info Section

The Step Info section for an AutoStepwise Scan step contains the following fields that define how the method will run:

Detail

Enter an identifying or descriptive comment for this step; a maximum of 40 characters.

Weight

You can specify whether the weight of the sample will increase or decrease during the run by selecting Gain or Loss from the drop-down menu next to Weight. Indicate the amount by which the sample weight is to change in order to have the method switch to the new scan rate by entering a value in the "is more than" field. Select the weight change units to use: mg/min or %/min. The units used for the rate of weight loss in the remainder of this section are determined by this selection. The entry made in this line is called the entrance criterion for the autostepwise scan.

Scan Rate

Select either Scan Rate or Isothermal. If the rate of weight loss is greater than the value you entered in line 1 (the entrance criterion), the analyzer will continue to scan the temperature at the Scan Rate you enter here or hold the temperature constant (by selecting Isotherm). The default value for Isotherm is 10.0 min and for Scan Rate is 2.0 °C/min.

Return to Original Rate

If during this reduced rate segment of the run the rate of weight loss is less than the value entered here, then the analyzer returns to the original scan rate. The entry made in this line is called the exit criterion.

There must be a difference between the entrance and exit criteria in order for the autostepwise scan to be valid: minimum value for

entrance criterion maximum value for entrance criterion

minimum value for exit criterion

maximum value for exit criterion

high balance range (<1300 mg)

0.05 mg/min 9999.9 mg/min 0.05 mg/min 9999.9 mg/min

ultrasensitive balance range (<25 mg)


Low balance range (<130 mg)


minimum value for entrance criterion

maximum value for entrance criterion

minimum value for exit criterion

maximum value for exit criterion

high balance range (<1300 mg)

0.01 %/min 999.9 %/min 0.01 %/min 999.9 %/min

ultrasensitive balance range (<25 mg)

0.01 %/min 999.9 %/min 0.01 %/min 999.9 %/min

Low balance range (<130 mg)

0.01 %/min 999.9 %/min 0.01 %/min 999.9 %/min

For low balance range: 999.99 > entrance criterion > exit criterion ± 0.01 mg/min

Running Samples 229

(entrance criterion – 0.01 mg/min) > exit criterion > 0.01 mg/min For high balance range: 9999.9 > entrance criterion > exit criterion ± 0.01 mg/min (entrance criterion – 0.01 mg/min) > exit criterion > 0.01 mg/min


The options are Seconds Between Points and Number of Points.

Select Value


Variable Rate Scan Step Info Section – TGA 8000 only

The technique of TGA is often used to determine the relative amounts of different components in a mixture based on their relative thermal stability. The underlying problem is that better separation, better resolution of the components, is favored by a slow heating rate, or one that essentially stops at the optimum temperature, to allow the less stable component to decompose while the more stable one does not. So when time is no object one could heat the sample at a very low heating rate, e.g., 1 ºC/min, to get the best possible resolution of the thermal events. (But when is time no object?) If one knew exactly what temperature vs. time program provided the best separation one could enter it into the Pyris Method Editor using a series of different heating rates and isotherms. But finding this out might take a fair amount of trial and error testing, and it likely would be dependent on sample size. AutoStepwise, (1-3) and now Variable Rate programming, provide tools to shortcut this process.

Variable Rate Scan (for TGA 8000) is a choice for a scanning rate (heating only) step. When you add this step to your method you will need to specify a starting temperature, higher ending temperature, initial heating rate, and the maximum rate of weight loss/gain.

The maximum rate of weight loss determines how much slower the heating rate will be in real time, based on the rate of change of the weight signal. For additional details, see How does Variable Rate Analysis work.

The Step Info section for a Variable Rate Scan step contains the following fields that define how the method will run:

Detail

Enter an identifying or descriptive comment for this step; a maximum of 40 characters.

To

Enter the temperature for the end of this step.

Rate

The analyzer will scan the temperature at the Scan Rate you enter here.

Threshold Weight

Select either Loss or Gain.


Threshold Weight Loss or Gain Rate

Enter the maximum rate of weight loss or gain. The value you enter here determines how much slower or faster the heating rate will be in real time, based on the rate of change of the weight signal. Then select a rate of mg/min or %/min.


The options are Seconds Between Points and Number of Points.

Select Value


How Does Variable Rate Analysis Work

Most weight loss processes are exponential in character, that is, they start off slowly, increase exponentially with increasing temperature, and then decay exponentially as the last remnants of material are transformed from solid to gas. The variable rate program takes advantage of this and works inversely; that is, as the weight loss reaction accelerates the heating rate exponentially decelerates to allow more time for that weight loss process to go to completion. Then when the weight loss reaction decelerates the heating rate returns to the original rate in an exponential fashion. Thus a minimum amount of time is wasted at the slow scan rate, and while the sample is losing weight the heating rate can be very slow, tenths of a degree per minute, to allow optimum resolution. This removes the requirement for the user to know a priori at what temperature the reaction starts and ends.

Parameter Selection

There are three parameters that define a variable rate method step: a sensitivity factor which determines how much the heating rate decreases for a given rate of weight loss, a resolution factor that controls how steep the scan rate change is for a change in mass loss, and the initial heating rate, which also becomes the heating rate after the weight loss process completes up until the next step in the method.

For a quick survey scan the user can pick a fast initial scan rate (e.g., 40 or 50 ºC/min) and a moderate sensitivity (e.g., 5% weight loss per minute) and a resolution factor of 5 out of 10. The result is a separation roughly equivalent to what would be obtained at a normal scan rate such as 20 ºC/min but in a shorter period of time. For running a sample with a weight loss step that is a small percentage of the total weight, the sensitivity factor would be selected to be smaller. To effectively lengthen the time which the program spends at a slow scan rate the resolution factor is increased to obtain a separation equivalent to that from a very slow scan rate. When the weight loss event is over, the heating rate resumes, gradually when a low value is selected for the resolution parameter, or quickly in the case of a higher resolution parameter setting. In either case this avoids the unnecessary time taken up by slow scanning in a temperature region where there is little or no weight loss activity.

Running Samples 231

Program Page for DMA 8000

The Program page appears when you select the Program tab of the Method Editor. This page contains the following sections:

Method Steps Section

Initial Temperature

Displays the initial temperature entered in the Initial State page. Change the value by typing in the entry field or using the spin buttons. If you change the initial temperature here, the value will be updated on the Initial State page and in the first step in the method program. If you change the Temperature in the Initial State page, the method program is adjusted accordingly.

List of Method Steps

The steps of the method program are listed in the order in which they will occur. If you are creating a new method, a default step is listed initially. Information entered in the Initial State page is used in the first step. The first step is highlighted upon entering the Program page. Select a step in this list to highlight it for editing. Use the buttons to the right of the list to add, insert, or delete a step. The type of step you add or insert may affect the steps already listed.

Add a Step

Displays the Method Step Options dialog box, in which you select the type of step you wish to append to the end of the program. The types of steps available for selection vary with the type of analyzer you are using.

Insert a Step

Displays the Method Step Options dialog box in which you select the type of step to insert immediately before the highlighted step in the list of method steps.

Delete this Step

Deletes the highlighted step from the method. To delete a step, the remaining program must be a continuous temperature program.

End Condition

Displays the Set End Condition box in the Edit Step section of the Program page. Here you specify the end condition for your method.

Edit Step Section The Edit Step section displays editable parameters for the highlighted step in the method. The parameters displayed depend on the scan used in the step.

Edit Temperature Scan Step Edit Isothermal Step Edit Frequency Multiplex Step Edit Strain Multiplex Step Edit Creep/Recovery Step Edit Stress/Strain Step Edit Stress/Relax Step



You can select actions and events for any program step. An action defines what will occur during system initialization. For each action, you select one or more events that will cause that action to happen.

Table 1: Actions you can select on the Program page:


Switch Gases You can switch to another purge gas or change the gas flow rate if your system is using a GSA 7 or a TAGS for changing purge gases.

Stop Run You can stop the run when one or more of the available events has occurred. Your options are to start the run when equilibration conditions have been reached, at a specified time, or immediately.

Trigger External Action This action will trigger a signal to a channel on an external relay box or an X-10 box.

Table 2: Events you can select on the Program page:




A Specified Temperature is reached

The action will occur at the specified temperature.



To select method actions and events:

1. Click the Add Action button. OR Position the mouse cursor in the Method Steps section and click the right mouse button. A pop-up menu appears.

2. Select Add an Action. A dialog box appears that asks you to select an action. For information on each action, refer to Table 1 above.

3. Select the Action you want to occur and click OK. A dialog box appears that allows you to set the details for the action.

4. Click OK. A dialog box appears that asks you to select an event. For information on each event, refer to Table 2 above.

5. Select the event you want to occur and click OK. A dialog box appears that allows you to set the details of the event.

6. Click OK.

Running Samples 233

Set End Condition

The Set End Condition parameters for the DMA 8000 appear at the bottom of the Program page when you select the End Condition button. These are the conditions that the analyzer is to obtain at the end of a run. The Set End Condition section contains the following controls:

Temperature

Go To Load Temperature

Selects the load temperature entered in Preferences as the end condition. At the end of the run, the analyzer will be programmed to this temperature.

Hold at Current

Selects the current temperature as the end condition temperature.

Go To

Selecting Go To activates the Temperature entry field and indicates that a user-entered temperature is the end condition temperature. Enter the temperature to which the analyzer will return at the end of the run.

Frequency

Go To Load

Selects the load frequency entered in Preferences as the end condition for the frequency. At the end of the run, the analyzer will be programmed to this frequency.

Hold at Current

Selects the current frequency as the end condition frequency.

Go To

Selecting Go To activates the Frequency entry field and indicates that a user-entered frequency is the end condition. Enter the frequency to which the analyzer will return at the end of the run.

Strain

Go To Load

Selects the load strain entered in Preferences as the end condition for strain. At the end of the run, the analyzer will be programmed to this strain.

Hold at Current

Selects the current static strain as the end condition strain.

Go To

Selecting Go To indicates that a user-entered strain is the end condition. Enter the static strain to which the analyzer will return at the end of the run.

When you have finished setting the end condition, click Done to return to the Set End Condition dialog box.


Step Info Section

The Step Info parameters are displayed when the Step Info button on the Program page is selected. The Step Info section for most of the scan types contains the following controls:

Detail

Enter a comment or identification for the highlighted step, up to 40 characters.


The only data sampling option with the DMA 8000 is Seconds Between Points.

Select Value

Displays the seconds between data points collected. Use the spin buttons to increase or decrease the displayed value. The smaller the number of seconds between points, the more data points are collected. If the number of points collected is small, you may miss an important event in the run.

Frequency MultiPlex and Creep/Recovery steps also display the number of Repetitions, that is, how many different temperature stages are included in the method where data will be collected.

DMA 8000 Method Steps The Method Step options for the DMA 8000 are:

• Temperature Scan

• Isothermal

• Frequency Multiplex

• Strain Multiplex

• Creep/Recovery

• Stress/Strain

• Stress/Relax

Method Step Settings Temperature Scan

This is the most widely used method in DMA. The sample is heated between two temperatures at a specific heating rate. The experiment can be performed with frequency or strain control, for single or multiple values.

• From - the value in the Initial Temp field next to the Add a step button.

• To - the final temperature in the scan.

• Rate - the heating rate for the temperature scan.

The frequency or strain settings shown can be edited by clicking Setting.

Running Samples 235

Isothermal

This method is used to characterize fatigue behavior, curing, degradation, etc. The sample is heated at a set temperature for a specific time. The experiment can be performed with frequency or strain control, for single or multiple values.

Time - the duration for the sample to be heated at the initial temperature.

The frequency or strain settings shown can be edited by clicking Setting.

Frequency Multiplex

This method measures a material's properties over a wide range of applied frequency.

• Log or Linear - the distribution used to calculate the frequency values.

• From - the initial frequency used in each scan.

• To - the final frequency used in each scan.

• Points per decade - the number of interim values for every ten-fold increase in frequency

• Temperature Rate - the heating rate when moving between temperature values.

• Increment - the interval between temperature readings at which the frequencies are scanned.

• Iso - the time period for which the temperature is maintained before data are collected, to allow the sample to reach thermal equilibrium.

• End - the final temperature value at which frequencies are applied.

• Strain - the strain to be applied during all the measurements at different frequencies.

Strain Multiplex

This method assesses the strain dependence of a material by measuring the force required to achieve a specific displacement at a number of different temperatures.

Settings are as for Frequency Multiplex except that the frequency is held constant at the value specified during the measurements at different strains.

Creep/Recovery

This method measures the displacement caused by applying a static load at a number of different temperatures. Plot the Static Strain Corrected against time to view the how the material behaves once the applied force is removed, and whether there is any permanent deformation.

• Force Settings Load - the load to be applied during the experiment. Rate (N/min) - the rate at which the load is applied. Mid-point Recovery - check the checkbox to remove the load halfway through the isotherm and monitor the recovery of the sample.

• Temperature Settings Rate - the ramp rate for the temperature changes between isotherms.


Incr - the incremental increase in temperature between each isotherm. Iso - the dwell time at each temperature isotherm. End - the final temperature isotherm (the initial isotherm is the value in the Initial Temp box).

• Ramp Data - check the checkbox to continue collecting data while the temperature is changing.

Stress/Strain

This method applies a range of static forces (stresses) to the material at a specific temperature. Plot Static Strain Corrected against Static Stress to view the results and calculate the modulus from the initial slope.

• Force Settings Load - the load to be applied during the experiment. Rate - the rate at which the load is applied.

• Time Settings Pre - the duration of the pre-equilibration step before the experiment begins (if required). Iso - the duration of the experiment.

Stress/Relax

This method assesses the behavior of a material under a constant applied strain over a temperature range. Plot the Total Applied Static Force or the Static Force Corrected against time to see how the force needed to maintain the applied strain changes.

• Load - the load to be applied initially to hold the sample in place.

• Strain - the strain (in mm) applied to the sample at the start of the experiment.

• Time (Iso) - the dwell time at each temperature isotherm.

• Ramp Data - check the checkbox to continue collecting data while the temperature is changing.

Using the Settings dialog box

1. Select the type of experiment from the following options: Single - a scan using a single frequency or strain value. Freq - a scan using multiple frequency values. Strain - a scan using multiple strain values.

2. Select the initial values of frequency and strain to be used.

3. For experiments using multiple frequencies or strains, select the number of different values to be used. For each frequency or strain, set a value in the appropriate box. The initial value counts as the first value. For an experiment with three values, you have to set levels for two more values.

4. Click OK to close the Settings dialog box.

Running Samples 237

The settings selected in the Settings dialog box are automatically applied to all the steps in the method.


By selecting different actions and events in your method, you can switch purge gases and flow rates, equilibrate before the run starts or during any program step, trigger actions based on signals to or from an external relay box, and time when you want actions to occur during the method.

Gas Switch Actions To switch purge gases or flow rates in your method:

1. Display the Initial State page of the method if you want to switch purge gases or flow rates before the run begins. Or, display the Program page of the method if you want the gas switch action to occur during one of the program steps.

2. Right-click to display the pop-up menu and select Add Action. Select Switch Gases.

3. In the Gas Switch action dialog box, select the following parameters. The values displayed here are the default gas and flow rate selected in Preferences.

Parameter Description

Purge Gas Click the arrow to display the drop-down list of available gases. For a TAGS, the choices in the drop-down list are all available gases plus the option Gas Off. The gases selected in Preferences are marked with an asterisk and appear at the top of the list. For a GSA 7, the choices in the drop-down list are the two gases specified in Preferences (when editing a method in Data Analysis application, the choice of gases is the entire list). The gases selected in Preferences are marked with an asterisk and appear at the top of the list. If there is no gas accessory attached, then the name of the gas used at the start of the run is displayed in gray. Only the Air Cooling Unit is available for Diamond TG/DTA, Diamond TMA Standard Temperature, and Diamond TMA High Temperature.

Flow Rate The default purge gas flow rate displayed was entered in Preferences. This field is read only for a GSA 7 and no gas switching accessory. For a TAGS, increase or decrease the flow rate by entering a new value or using the spin buttons.

4. Select the event that you want to trigger the gas switch action to occur. For more information on these events, see Table 2.

Equilibration Events

The parameters in this dialog box depend on the analyzer. In general, when you select an equilibration event, Pyris will monitor the addressed signal from the analyzer until it fluctuates within the specified criterion for 20 seconds (10 consecutive readings, each 2-s intervals).

NOTE: You can select one or more equilibration events. Use AND statements to specify that all events must occur before the run begins. Use OR statements to specify that only one of the events must occur before the run begins. For more information on using these statements, see Combining Events with AND/OR Statements.

To specify an equilibration event in your method:


1. Display the Initial State page of the method if you want to specify the equilibration event before the run begins. Or, display the Program page of the method if you want to specify the event during one of the program steps.

2. Right-click to display the pop-up menu and select Add Action. Select the action that will be triggered when the equilibration event occurs. The choices of actions are Start Run (Initial State only), Stop Run (Program page only), Switch Gases, and Trigger an External Action.


4. When the dialog box appears that asks you to select an event, click A Signal Equilibrates.

5. In the Equilibration Event dialog box, select the signal that needs to be equilibrated. The signals that appear in this dialog box depend on the analyzer. The different signals are described in the table below.

Signal Analyzer Description

Sample Temperature all analyzers This is the temperature of the thermocouple and the sample's environment in degrees Celsius.

Temperature all analyzers This is the temperature you specify for the program in degrees Celsius.

Heat Flow DSC analyzers For DSC analyzers, the Y signal is Heat Flow. Units are in milliwatts (mW).

Normalized Heat Flow DSC analyzers This is the heat flow signal divided by the sample weight. Units are in Weight/grams (W/ g).

Weight TGA analyzers For TGA analyzers, the Y signal is weight in milligrams (mg).

Unsubtracted Delta T DTA 7 For the DTA 7, this is the Delta T signal before baseline subtraction is performed. Delta T is the difference in temperature between the sample and an inert reference material.

Probe Position Diamond TMA, TMA 7

This is the average position of the probe tip (in millimeters) during the run.

Height% Diamond TMA, TMA 7

The amount by which the height measured by the analyzer can fluctuate from the Height value measured and entered by the user.

6. Select a Criterion value. This is a plus or minus value that represents the amount the signal can fluctuate up or down when equilibration occurs.

7. If desired, you can use a Setpoint by checking the box and entering a value. A setpoint defines a target value for equilibration. For example, if you select a Setpoint at a

Running Samples 239

temperature of 50 °C and the criterion is 0.1, the equilibration event will only occur if the signal equilibrates between the range of 49.9 to 50.1 °C. If the signal equilibrates at a different temperature, for example 40 °C, the equilibration event will not occur because it is not at the specified setpoint.

8. Select whether you want the signal to be monitored at the beginning of the segment or at a specified time into the segment and enter the time in minutes.

Cross-Boundary Events

In general, when you select a cross-boundary event, the software will monitor the addressed signal from the analyzer and cause the specified action to occur if the signal crosses an upper or lower boundary.

To specify a cross-boundary event in your method:

1. Display the Initial State page of the method if you want to specify the cross-boundary event before the run begins. Or, display the Program page of the method if you want to specify the event during one of the program steps.

2. Right-click to display the pop-up menu and select Add Action. Select the action that will be triggered when the cross-boundary event occurs. The choices of actions are Start Run (Initial State only), Stop Run (Program page only), Switch Gases, and Trigger an External Action.


4. When the dialog box appears that asks you to select an event, click on A Signal Crosses a Boundary.

5. In the Cross-Boundary Event dialog box, select the signal that needs to be monitored. The signals that appear in this dialog box depend on the analyzer. The different signals are described in the table below.

Signal Analyzer Description

Sample Temperature all analyzers This is the temperature of the thermocouple and the sample's environment in degrees Celsius.

Temperature all analyzers This is the temperature you specify for the program in degrees Celsius.

Heat Flow DSC analyzers For DSC analyzers, the Y signal is Heat Flow in milliwatts (mW).

Normalized Heat Flow DSC analyzers This is the heat flow signal divided by the sample weight. Units are in Weight/grams ( W/ g).

Weight TGA analyzers For TGA analyzers, the Y signal is weight in milligrams (mg).

Probe Position Diamond TMA This is the average position of the probe tip (in millimeters) during the run.

Height% Diamond TMA The amount by which the height measured by the analyzer can fluctuate from the Height value measured and entered by the user.


6. You can specify both an upper boundary and lower boundary, or just one boundary. Check the appropriate boxes and enter a value. The action you specified will only occur if the signal crosses the specified boundaries.

7. Select whether you want the signal to be monitored at the beginning of the segment or at a specified time into the segment and enter the time in minutes.

External Relay Actions and Events

One of the advanced features of the software is operation of your system and accessories in conjunction with an external relay box. The software is capable of both sending and receiving signals from the external relay box. You can specify an external relay action, which will trigger an action to occur by switching a channel on the external relay on or off before the run or during any program step. Or, you can specify an external relay event, which means that an action associated with a program step will only occur if the software receives a signal from the external relay box.

NOTE: External Relay actions and events are not available for the DMA or DTA.

To specify an external relay ACTION in your method:

1. Display the Initial State page of the method if you want to specify the external relay before the run begins. Or, display the Program page of the method to specify the external relay during one of the program steps.

2. Right-click to display the pop-up menu and select Add Action. Select Trigger an External Action.

3. Select the event that you want to trigger the external relay action to occur.

4. In the External Trigger Action dialog box, click on the drop-down list to select the channel on the external relay box to switch on or off.

To specify an external relay EVENT in your method:

1. Display the Initial State page of the method if you want to specify the external relay before the run begins. Or, display the Program page of the method to specify the external relay during one of the program steps.

2. Right-click to display the pop-up menu and select Add Action. Select the action that will be triggered when the external relay event occurs. The choices of actions are Start Run (Initial State only), Stop Run (Program page only), Switch Gases, and Trigger an External Action.

NOTE: For advanced applications, the software allows you to specify that both an external relay action should switch one channel on or off and that this action should occur based on an external relay event from another channel.


4. When the dialog box appears that asks you to select an event, click An External Event occurs.

5. In the External Trigger Event dialog box, click on the drop-down list to select the channel on the external relay box to switch on or off.

Running Samples 241

Timed Events

When you select a timed event, the action will occur when a specified time is reached after a program segment starts. You have the option of timing any of the following actions: Start Run (Initial State only), Stop Run (Program page only), Switch Gases, and Trigger an External Event.

To specify timed events in your method

1. Display the Initial State page of the method if you want to specify the timed event before the run begins. Or, display the Program page of the method to specify the timed event during one of the program steps.

2. Right-click to display the pop-up menu and select Add Action. Select the action that will be triggered when the specified time is reached. The choices of actions are Start Run (Initial State only), Stop Run (Program page only), Switch Gases, and Trigger an External Action.


4. When the dialog box appears that asks you to select an event, click A Specified Time is reached.

5. In the Timed Event dialog box, specify the amount of time to wait in the program segment before the action occurs.

Combining events with AND/OR statements

To select one event AND another event for a given action

In some cases, you may want an action to occur when more than one condition is met. For example, you can switch gases when an external event occurs and a specified time is reached. Both of these events must occur before the action takes place.

This example would read as follows: Switch the Gas to Nitrogen at 20.0 ml/min

...and the Time is >=2.000 min

...and the External Channel 1 is On

1. Click the action to highlight it, then click the right mouse button.

2. A pop-up menu appears. Select Add an Event.

3. In the next dialog box that appears, select an additional event.

To select one event OR another event for a given action

In some cases, you may want an action to occur when only one of multiple events takes place. For example, you may want to start the run either when the desired signal is equilibrated or when a specified time is reached. In this case, you need to duplicate the action by selecting it again, each time with a different event selection. The example would read as follows:

Start the Run


...if the Temperature Equilibrates Within +/ -1.000e-002

Start the Run

...if the Time is >=1.000 min

Modifying Actions and Events

To modify actions and events

1. Position the mouse cursor in the white program box and click the right mouse button.

2. A pop-up menu appears. Select one of the following commands:

Use this command in the pop-up menu... To do this...

Edit an Item To change the conditions associated with an action or event

Delete an Item To delete an action or event

Change an Item To select a different action or event

Temperature Events

When you select a Temperature event, the action will occur when a specified temperature is reached after a program segment starts. You have the option of selecting temperature with any of the following actions: Stop Run (Program page only), Switch Gases, and Trigger an External Event.

To specify temperature events in your method

1. Display the Program page of the method to specify the temperature event during one of the program steps.

2. Right-click to display the pop-up menu and select Add Action. Select the action that will be triggered when the specified temperature is reached. The choices of actions are Stop Run (Program page only), Switch Gases, and Trigger an External Action.


4. When the dialog box appears that asks you to select an event, click A Specified Temperature is reached.

5. In the Temperature Event dialog box, specify the temperature to reach in the program segment before the action occurs.

Running Samples 243

Control Panel

Each Instrument Application window contains a control panel on the right side. This panel is dockable and its display can be toggled on and off from the View menu. It contains buttons that directly control parameters specific to the analyzer. Some parameters can be set in both the Method Editor and the control panel. A change in one place is reflected in the other. Use the control panel to start and stop a run, change the furnace temperature, change the purge gas, zero the weight, zero the height, apply forces, hold the probe, or hold the temperature.

See the topics below to learn about the control panel for each analyzer:

DSC 8500 Control Panel




Pyris 1 TGA Control Panel

TGA 4000 Control Panel

STA 8000 Control Panel


DMA 8000 Control Panel

Diamond DSC Control Panel

Pyris 1 DSC Control Panel

Jade DSC Control Panel


DSC 8500 Control Panel The DSC 8500 control panel contains the following controls:

Start Method Button Stop Method Button

The Start Method button has the red vertical line on the left side. Click on the button to start the run using the method loaded in the Method Editor. When the run starts, the Instrument Viewer becomes the active window, the run begins, and the button changes to the Stop Method button. The Stop Method button has the red vertical line on the right side. When you click on the Stop Method button, the method’s end condition is executed, the data are saved, the curve(s) is redrawn in the Instrument Viewer (if Auto-Rescale was selected in the Display menu), and the button changes back to Start Method.

Go To Temperature Button

Programs the analyzer to the temperature specified in the Go To Temperature entry field. If a run is in progress when you select this button, the run ends immediately.

Go To Temperature

Enter the temperature in °C to which the analyzer will be programmed when the Go To Temperature button is selected.

Go To Load Button

Programs the analyzer to the load temperature specified on the Instrument page in Preferences. If a run is in progress when you select this button, the run ends immediately.

Hold Temperature Button

Holds the analyzer at the current temperature. If a run is in progress when you select this button, the run ends immediately.

Clean Furnace Button

Executes the Clean furnace procedure. This button is disabled during a run.

WARNING: Before cleaning the furnaces, remove all samples and pans.

Performing the DSC Clean Furnace Procedure NOTE: You must open the sample holder cover and expose the furnaces to air so all organic

materials are removed during the cleaning process.


Running Samples 245

When the Clean button is selected in the control panel, the clean furnace procedure begins automatically. A dialog box appears with a message. If you select Continue, the run begins. If you select Cancel, no further action takes place and the DSC goes to the load temperature. During the Clean procedure, the Status line displays the Cleaning status.

The Clean procedure heats the DSC sample holder to 600 °C and holds it there for several minutes. This temperature is high enough to burn off any organic residue that may have been deposited in the sample holder. When the clean furnace button is selected on the Pyris Control Panel, the sample covers will remain open throughout the cleaning procedure to expose the furnaces to the air. As part of the cleaning procedure, you will be able to set the temperature at which the system will hold for a specific duration in order to clean the system. By default the cleaning procedure will heat the DSC sample holder to 600 °C and hold it there for several minutes. This temperature is high enough to burn off any organic residue that may have been deposited in the sample holder.

To clean the furnaces:

1. Click on the Clean Furnace button. The covers automatically open. A pop up window displays a message stating:

2. If you click Cancel the cleaning procedure is canceled. OR If you click OK, a second pop up message appears:

3. Click Yes to start the clean cycle, or click No to cancel the clean cycle.

4. You can check the Maximum Purge check box to have the full purge feature of the mass flow controller enabled during the furnace cleaning procedure. T


5. You can stop a clean cycle by clicking on the Clean Furnace button a second time.

6. After the cleaning procedure is complete a pop up message appears that states:

7. Click OK to close this message. When the clean furnace procedure is complete, the cover remains open and you must use the Close Cover button to close the cover.

Autosampler Control Button

Displays the Autosampler Control dialog box if an autosampler is installed on the DSC 8500. You can use the commands in the dialog box to control certain movements of the autosampler to handle an individual sample. If no autosampler is present, the button is grayed out.

Cover Heater Button

Turns the heater in the sliding sample holder enclosure cover on or off. When the cover heater is on, the housing of the sampler holder is heated to provide condensation-free and frost-free operation.

AirShield Plus Button

Activates or deactivates the AirShield feature. If the AirShield is activated, then when the sliding sample holder enclosure cover is moved back to expose the sample holders, the AirShield automatically turns on. When the cover is returned to its closed position, the AirShield feature turns off. You can also turn the AirShield feature on or off by using the adjustable control panel.

Zero Heat Flow Signal

Reads and saves current Heat Flow signal. It subtract from all successive values. Sets The Heat Flow signal to zero.

Running Samples 247

Reset Monitor Button

Clears the display in the Instrument Viewer window and restarts the monitor. When there is no run in progress, the monitor displays the baseline signals from the analyzer. When a run is in progress, the monitor displays the real time signals as the data are collected.

Set Balance and Slope

Displays a dialog box that allows you to perform real-time adjustment of the balance and slope while a baseline is running via the Method Editor. The graphical display will show the real-time changes "on-the-fly."

Open/Close Cover Button

This button opens and closes the sample cover. This button is disabled during a run.

Cooling Device Button

Activates or deactivates the cooling device that is configured with your analyzer.

Purge Gas

Use the drop-down list to switch the purge gas. The gases available are entered in the Purge Gases page of Preferences. Click the Apply button to implement the change of purge gas immediately.

Smart Scan

This is an information display and informs you whether or not SmartScan has been applied.



The DSC 8000 Control Panel contains the following controls:





Go To Temperature


Go To Load Button







Performing the DSC Clean Furnace Procedure. NOTE: You must open the sample holder cover and expose the furnaces to air so all organic

materials are removed during the cleaning process.


Running Samples 249

When the Clean button is selected in the control panel, the clean furnace procedure begins automatically. A dialog box appears with a message. If you click Continue, the run begins. If you click Cancel, no further action takes place and the DSC goes to the load temperature. During the Clean procedure, the Status line displays the Cleaning status.

The Clean procedure heats the DSC sample holder to 600°C and holds it there for several minutes. This temperature is high enough to burn off any organic residue that may have been deposited in the sample holder. When the clean furnace button is selected on the Pyris Control Panel, the sample covers will remain open throughout the cleaning procedure to expose the furnaces to the air. As part of the cleaning procedure, you will be able to set the temperature at which the system will hold for a specific duration in order to clean the system. By default the cleaning procedure will heat the DSC sample holder to 600 °C and hold it there for several minutes. This temperature is high enough to burn off any organic residue that may have been deposited in the sample holder.

To clean the furnaces:

1. Click on the Clean Furnace button. The covers automatically open. A pop up window displays a message stating:

2. If you click Cancel the cleaning procedure is canceled. OR If you click OK, a second pop up message appears:

3. Click Yes to have the clean cycle begin, or click No to cancel the clean cycle.

4. You can check the Maximum Purge check box to have the full purge feature of the mass flow controller enabled during the furnace cleaning procedure. T


5. You can stop a clean cycle by clicking on the Clean Furnace button a second time.

6. After the cleaning procedure is complete a pop up message appears that states:

7. Click OK to close this message. When the clean furnace procedure is complete, the cover remains open and you must use the Close Cover button to close the cover.


Displays the Autosampler Control dialog box if an autosampler is installed on the DSC 8000. You can use the commands in the dialog box to control certain movements of the autosampler to handle an individual sample. If no autosampler is present, the button is dimmed.

Cover Heater Button

Turns on or off the heater in the sliding sample holder enclosure cover. When the cover heater is on, the housing of the sampler holder is heated to provide condensation-free and frost-free operation.

AirShield Plus Button


Zero Heat Flow Signal

Reads and saves current Heat Flow signal. This is subtracted from all successive values, which sets the Heat Flow signal to zero.

Running Samples 251



Set Balance and Slope

Displays a dialog box that allows you to perform real-time adjustment of the balance and slope while a baseline is running via the Method Editor. The graphical display will show the real-time changes "on-the-fly."

Open/Close Cover Button

This button opens and closes the sample cover. This button is disabled during a run.

Cooling Device Button

Activates or deactivates the cooling device that is configured with your analyzer.

Purge Gas

Use the drop-down list to switch the purge gas. The gases available are entered in the Purge Gases page of Preferences. Click on the Apply button to implement the change of purge gas immediately.

Smart Scan

This is an information display and informs you whether or not SmartScan has been applied.







Programs the analyzer to the temperature specified in the Go To Temperature entry field. If a sample run is in progress when you select this button, the run ends immediately.

Go To Temperature

Enter the temperature in °C to which the analyzer will be programmed when the Go To Temperature button is clicked. You can enter a temperature ranging from –180 °C to 445 °C.

Go To Load Button





Clears the display in the Instrument Viewer window and restarts the monitor. When there is no run in progress, the monitor displays the baseline signals from the analyzer. When a run is in progress, the monitor displays the real-time signals as the data are collected.


Displays the Autosampler Control dialog box if an autosampler is installed on the DSC 6000. You can use the commands in the dialog box to control certain movements of the

Running Samples 253

autosampler to handle an individual sample. You can also access the gripper alignment wizard which is used to realign the gripper after removing and replacing the autosampler for installing a reference pan. If no autosampler is present, the button is dimmed.

Purge Gas

Use the drop-down list to switch the purge gas. The gases available are entered in the Purge Gases page of Preferences. Click the Apply button to implement the change of purge immediately.

CryoFill Button

Activates or deactivates the CryoFill Liquid Nitrogen Filling System. When this feature is on, a sensor in the LN2 dewar in the DSC 6000 detects the level of the LN2. If it drops below a certain level, the system will automatically bring in LN2 from the supply tank until it reaches the designated level.

NOTE: You must turn the CryoFill off when you are going to disconnect the supply in order to refill the supply tank.








Go To Temperature


Go To Load Button







Displays the Autosampler Control dialog box if an autosampler is installed on the DSC 4000. You can use the commands in the dialog box to control certain movements of the autosampler to handle an individual sample. You can also access the gripper alignment

Running Samples 255

wizard which is used to realign the gripper after removing and replacing the autosampler for installing a reference pan. If no autosampler is present, the button is grayed out.

Purge Gas

Use the drop-down list to switch the purge gas. The gases available are entered in the Purge Gases page of Preferences. Click on the Apply button to implement the change of purge immediately.


Pyris 1 TGA Control Panel

The Pyris 1 TGA control panel contains the following controls:


The Start Method button has the red vertical line on the left side. Click on the button to start the run using the method loaded in the Method Editor. When the run starts, the Instrument Viewer becomes the active window, the run begins, and the button changes to the Stop Method button. The Stop Method button has the red vertical line on the right side. When you click on the Stop Method button, the method's end condition is executed, the data are saved, the curve(s) is redrawn in the Instrument Viewer (if Auto-Rescale was selected in the Display menu), and the button changes to Start Method.



Go To Temperature


Go To Load Button





Displays the Autosampler Control dialog box if an autosampler is installed on the Pyris 1 TGA. You can use the commands in the dialog box to control certain movements of the autosampler to handle an individual sample. If no autosampler is present, the button is grayed out.

Running Samples 257


Executes the Clean furnace procedure for the Pyris 1 TGA. If a run is in progress when you select this button, the run ends immediately.

Sample Weight Button

Tells the analyzer to read the weight of the sample in the sample pan and display it in the Weight field in the Sample Info page in the Method Editor. This button is disabled during a run.

Zero Weight Button

Tells the analyzer to read the weight of the empty sample pan; this is the offset weight which is subtracted from the total weight to obtain the weight of the sample in the pan. The weight is displayed in the Zero field in Sample Info page in the Method Editor. This button is disabled during a run.

Raise Furnace Button

Moves the furnace to the Raised or Run position. If a run is in progress when you select this button, the run continues.

Lower Furnace Button

Moves the furnace to the Lowered position. If a run is in progress when you select this button, the run ends immediately.

Cool Furnace Button

Moves the furnace to the Cooling position. If a run is in progress when you select this button, the run ends immediately.



Antistatic Device Button

Controls the state of the static shield. Pyris 1 TGA's static shield creates an invisible curtain of charged particles that prevent static cling between the sample pan and furnace wall. The device can be On, Off, Auto-Enabled, or Auto-Disabled. The status is displayed in the status panel. When the status is On, the device is on. When the status is Off, the device is always off. When the status is Auto-Enabled, the device is on when the furnace is stationary in the lower position, traveling between the lower position and the raised position. Auto-Disabled is the same as Off, that is, the device is always off. This control panel button can toggle the status of the antistatic device. It can also be controlled from the instrument's panel.


Upper Fan Button

The upper fan of the Pyris 1 TGA is used to create a gradient for the furnace to help it attain ambient temperature. The temperature gradient is needed in order for the motor to stay on and the furnace to run. The fan blows on the outside of the furnace tube when it is in the raised position. The upper fan is controllable from the control panel. There are two states: Auto and Off. The status is displayed in the status panel.

Purge Gas

Use the drop-down list to switch the sample purge gas. This is available when you have a GSA 7 or a TAGS accessory attached to your analyzer and configured in the system. The gases available are entered in the Purge Gases page of Preferences. Click the Apply button to implement the change of purge gas immediately.

Running Samples 259


The TGA 4000 Control Panel contains the following controls:





Go To Temperature


Go To Load Button





Reads the weight of the sample in the sample pan and displays it in the Weight field in the Sample Info page in the Method Editor. This button is disabled during a run.

Zero Weight Button

Reads the weight of the empty sample pan; this is the offset weight which is subtracted from the total weight to obtain the weight of the sample in the pan. It is displayed in the Zero field in Sample Info page in the Method Editor. This button is disabled during a run.


Cooling Air Button

Enables/disables the small internal air pump which produces forced air that cools down the furnace. If a run is in progress when you select this button, the run ends immediately.


Displays the Autosampler Control dialog box if an autosampler is installed on the TGA 4000. You can use the commands in the dialog box to control certain movements of the autosampler to handle an individual sample. You can also access the gripper alignment wizard which is used to realign the gripper after removing and replacing the autosampler in order to install a new sample thermocouple. If no autosampler is present, the button is grayed out.



Purge Gas

Use the drop-down list to switch the purge gas. The gases available are entered in the Purge Gases page of Preferences. Click on the Apply button to implement the change of purge gas immediately.

Running Samples 261


The TGA 8000 control panel contains the following controls:

Start Method/Stop Method

The Start Method button has the red vertical line on the left side. Click on the button to start the run using the method loaded in the Method Editor. When the run starts, the Instrument Viewer becomes the active window, the run begins, and the button changes to the Stop Method button. The Stop Method button has the red vertical line on the right side. When you click on the Stop Method button, the method's end condition is executed, the data are saved, the curve(s) is redrawn in the Instrument Viewer (if Auto-Rescale was selected in the Display menu), and the button changes to Start Method.



Go To Temperature


Go To Load Button





Displays the Autosampler Control dialog box if an autosampler is installed on the Pyris 1 TGA. You can use the commands in the dialog box to control certain movements of the autosampler to handle an individual sample. If no autosampler is present, the button is grayed out.


Executes the Clean furnace procedure for the TGA 8000. If a run is in progress when you select this button, the run ends immediately.

mk:@MSITStore:C:%5CUsers%5CGarrisER%5CDocuments%5CTGA8K%20Help%5CPyris%2011.0%20Software%20Help%5Cpyris.chm::/p1tpref.htm

mk:@MSITStore:C:%5CUsers%5CGarrisER%5CDocuments%5CTGA8K%20Help%5CPyris%2011.0%20Software%20Help%5Cpyris.chm::/p1tasdia.htm

javascript:void(0);



Tells the analyzer to read the weight of the sample in the sample pan and display it in the Weight field in the Sample Info page in the Method Editor. This button is disabled during a run.

Zero Weight Button

Tells the analyzer to read the weight of the empty sample pan; this is the offset weight which is subtracted from the total weight to obtain the weight of the sample in the pan. The weight is displayed in the Zero field in Sample Info page in the Method Editor. This button is disabled during a run.

Raise Furnace Button

Moves the furnace to the Raised or Run position. If a run is in progress when you select this button, the run continues.

Lower Furnace Button

Moves the furnace to the Lowered position. If a run is in progress when you select this button, the run ends immediately.

Enable/Disable Furnace Cover

The furnace cover is used to control the heat convection generated by the furnace. When the cover is enabled, it will be closed when the furnace is heating or holding isothermally and during all run conditions. When the cover is disabled, the cover will be open at all times



Antistatic Device Button

Controls the state of the static shield. The TGA 8000’s static shield creates an invisible curtain of charged particles that prevent static cling between the sample pan and furnace wall. The device can be On, Off, Auto-Enabled, or Auto-Disabled. The status is displayed in the status panel. When the status is On, the device is on. When the status is Off, the device is always off. When the status is Auto-Enabled, the device is on when the furnace is stationary in the lower position, traveling between the lower position and the raised position. Auto-Disabled is the same as Off, that is, the device is always off. This control panel button can toggle the status of the antistatic device. It can also be controlled from the instrument's panel.

Running Samples 263

Fan Button

The fan of the TGA 8000 is used to create a gradient for the furnace to help it attain ambient temperature. The temperature gradient is needed in order for the motor to stay on and the furnace to run. The fan blows on the outside of the furnace tube when it is in the raised position. The upper fan is controllable from the control panel. There are two states: Auto and Off. The status is displayed in the status panel.

Purge Gas

Use the drop-down list to switch the sample purge gas. The gases available are entered in the Purge Gases page of Preferences. Click the Apply button to implement the change of purge gas immediately.

mk:@MSITStore:C:%5CUsers%5CGarrisER%5CDocuments%5CTGA8K%20Help%5CPyris%2011.0%20Software%20Help%5Cpyris.chm::/Purge_Gas_Preferences_page.htm



The STA 8000 control panel contains the following controls:


The Start Method button has the red vertical line on the left side. Click the button to start the run using the method loaded in the Method Editor. When the run starts, the Instrument Viewer becomes the active window, the run begins, and the button changes to the Stop Method button. The Stop Method button has the red vertical line on the right side. When you click the Stop Method button, the method’s end condition is executed, the data are saved, the curve(s) is redrawn in the Instrument Viewer (if Auto-Rescale was selected in the Display menu), and the button changes back to the Start Method button.



Go To Temperature


Go To Load Button


Cooling Air Button

Activates a built-in air pump for additional cooling of the furnace. This button is disabled during a run.

When activated, the button changes to this symbol:



Running Samples 265


Reads the weight of the sample in the sample pan and displays it in the Weight field of the Sample Info page in the Method Editor. This button is disabled during a run.

Zero Weight Button

Reads the weight of the empty sample pan; this is the offset weight which is subtracted from the total weight to obtain the weight of the sample in the pan. It is displayed in the Zero field of the Sample Info page in the Method Editor. This button is disabled during a run.

Pause Temperature Control Button

Holds the power to the furnace constant while samples are being loaded or unloaded from the sensor. This prevents problems with temperature control when the furnace tries to compensate for rapid changes in heat capacity. The button is only available when the instrument's status is At Temp and the furnace temperature is below 100 °C.

When activated, the button changes to this symbol and the analyzer beeps every four seconds. Click the button to deactivate the function once the sample is loaded and the furnace lid is replaced. If a run is started by pressing the Start Method button while the temperature control is paused, the function is deactivated automatically and the button is disabled while the run is in progress.



Purge Gas

Use the drop-down list to switch the purge gas. The gases available are entered in the Purge Gases page of Preferences. Click the Apply button to implement the change of purge gas immediately. You can check the purge gas properties at any time using the Status Panel.

NOTE: During an experiment, the purge gas setting on the control panel is overruled by the method being used. The default new method automatically includes a purge of 20 ml/min of nitrogen, unless changed by the user.



The STA 6000 Control Panel contains the following controls:





Go To Temperature


Go To Load Button


Cooling Air Button

Activates a built-in air pump for additional cooling of the furnace. This button is disabled during a run.

When activated, the button changes to this symbol: .



Running Samples 267


Reads the weight of the sample in the sample pan and displays it in the Weight field in the Sample Info page in the Method Editor. This button is disabled during a run.

Zero Weight Button

Reads the weight of the empty sample pan; this is the offset weight which is subtracted from the total weight to obtain the weight of the sample in the pan. It is displayed in the Zero field in Sample Info page in the Method Editor. This button is disabled during a run.


Displays the Autosampler Control dialog box if an autosampler is installed on the STA 6000. You can use the commands in the dialog box to control certain movements of the autosampler to handle an individual sample. If no autosampler is present, the button is disabled.



Purge Gas

Use the drop-down list to switch the purge gas. The gases available are entered in the Purge Gases page of Preferences. Click the Apply button to implement the change of purge gas immediately. You can check the purge gas properties at any time using the Status Panel.

NOTE: During an experiment, the purge gas setting on the Control Panel is overruled by the method being used. The default new method automatically includes a purge of 20 ml/min of nitrogen, unless changed by the user.


DMA 8000 Control Panel

The DMA 8000 Control Panel contains the following controls:


The Start Method button has the red vertical line on the left side. Click the button to start the run using the method loaded in the Method Editor. When the run starts, the Instrument Viewer becomes the active window, the run begins, and the button changes to the Stop Method button. The Stop Method button has the red vertical line on the right side. When you click the Stop Method button, the method’s end condition is executed, the data are saved, the curve(s) is redrawn in the Instrument Viewer (if Auto-Rescale was selected in the Display menu), and the button changes back to Start Method.



Go To Load Button




Balance Zero

Runs the Balance Zero calibration. The analyzer reads the weight of the probe when zero force is applied. This zeros the weight of the probe so it is not included in the run of the sample. You must tare the probe when you change the measuring system and before mounting a sample.



Running Samples 269

Apply Force

The forces that are set up in the method are applied by the motor to the sample, allowing you to see the effect on your sample when you are designing an experiment. If a run is in progress, this button has no effect since the forces are already applied.

Zero Force

Sets the static and dynamic forces applied by the motor to 0 mN, turns the Static and Dynamic Controls to Force, and sets the frequency to 1 Hz.

Apply Static Force

Activates the static force control set in the Set Controls dialog box in the Initial State page. When the control is on, the button is lit, that is, has a white background.

Apply Dynamic Force

Activates the dynamic force control set in the Set Controls dialog box in the Initial State page. When the control is on, the button is lit, that is, has a white background.

Heater Control

Activates instrument control of the heater in the environmental chamber of the DMA 8000.

When the control is on, the button changes to .

Cryo Control

Activates instrument control of the cryogenic valve that regulates the flow of coolant from the Liquid Nitrogen Dewar to the DMA 8000. The valve will open and close at the temperatures set in the Instrument Page in Preferences. When the control is on, the button

changes to .

Drive Control

Controls the static forces that are applied to the sample during the experiment. When the

control is on, the button changes to . The available control modes are selected in the Initial State page.

Rebalance Control

Activates the rebalancing function, which balances out the forces so that the net force applied to the clamping fixture is zero. It should be used before loading your sample to hold


the head in a neutral position before the experiment begins. When the control is on, the

button changes to .

Park Mode

This button indicates if the instrument is in Park mode. Park mode shuts down all controls to the DMA 8000 while still remaining in communication with the instrument. When the

instrument is not in Park mode, the button changes to .

Stress/Strain Mode

This button indicates that the instrument is in Strain mode, where it attempts to apply defined displacements to the sample during the experiment. To change to Stress mode,

where defined forces are applied instead, click this button. It then changes to . Click the button again to change back to Strain mode.

Purge Gas

The purge gas box displays the gas selected in Preferences. It is for information only. The Apply button does not change the gas flow rate.

Running Samples 271

Diamond DSC Control Panel

The Diamond DSC control panel contains the following controls:





Go To Temperature


Go To Load Button





Displays the Autosampler Control dialog box if an autosampler is installed on the Diamond DSC. You can use the commands in the dialog box to control certain movements of the autosampler to handle an individual sample. If no autosampler is present, the button is grayed out.




Cover Heater Button

Turns on or off the heater in the sliding sample holder enclosure cover. This is a toggle button. When the cover heater is on, the housing of the sample holder is heated to provide condensation-free and frost-free operation. This should be turned on only when subambient temperatures are in use. You can also turn the cover heater on or off by using the adjustable control panel on the Diamond DSC.

AirShield Button


CryoFill Button

Activates or deactivates the CryoFill Liquid Nitrogen Filling System. When this feature is on, a sensor in the LN2 dewar in the Diamond DSC detects the level of the LN2. If it drops below a certain level, the system will automatically bring in LN2 from the supply tank until it reaches the designated level. You must turn the CryoFill off when you are going to disconnect the supply in order to refill the supply tank. You can also turn CryoFill on or off by using the adjustable control panel.



Purge Gas

Use the drop-down list to switch the purge gas. This is available when you have a GSA 7 or a TAGS accessory attached to your analyzer and configured in the system. The gases available are entered in the Purge Gases page of Preferences. Click on the Apply button to implement the change of purge gas immediately.

Running Samples 273

Pyris 1 DSC Control Panel

The Pyris 1 DSC control panel contains the following controls:





Go To Temperature


Go To Load Button





Displays the Autosampler Control dialog box if an autosampler is installed on the Pyris 1 DSC. You can use the commands in the dialog box to control certain movements of the autosampler to handle an individual sample. If no autosampler is present, the button is grayed out.




Cover Heater Button

Turns on or off the heater in the sliding sample holder enclosure cover. This is a toggle button. When the cover heater is on, the housing of the sample holder is heated to provide condensation-free and frost-free operation. This should be turned on only when subambient temperatures are in use. You can also turn the cover heater on or off by using the adjustable control panel on the Pyris 1 DSC.

AirShield Button


CryoFill Button

Activates or deactivates the CryoFill Liquid Nitrogen Filling System. When this feature is on, a sensor in the LN2 dewar in the Pyris 1 DSC detects the level of the LN2. If it drops below a certain level, the system will automatically bring in LN2 from the supply tank until it reaches the designated level. You must turn the CryoFill off when you are going to disconnect the supply in order to refill the supply tank. You can also turn CryoFill on or off by using the adjustable control panel.



Purge Gas

Use the drop-down list to switch the purge gas. This is available when you have a GSA 7 or a TAGS accessory attached to your analyzer and configured in the system. The gases available are entered in the Purge Gases page of Preferences. Click on the Apply button to implement the change of purge gas immediately.

Running Samples 275

Jade DSC Control Panel

The Jade DSC Control Panel contains the following controls:





Go To Temperature

Enter the temperature in °C to which the analyzer will be programmed when the Go To Temperature button is selected. You can enter a temperature ranging from –180°C to 450°C.

Go To Load Button







Displays the Autosampler Control dialog box if an autosampler is installed on the Jade DSC. You can use the commands in the dialog box to control certain movements of the autosampler to handle an individual sample. You can also access the gripper alignment wizard which is used to realign the gripper after removing and replacing the autosampler for installing a reference pan. If no autosampler is present, the button is grayed out.


Purge Gas

Use the drop-down list to switch the purge gas. The gases available are entered in the Purge Gases page of Preferences. Click on the Apply button to implement the change of purge immediately.

CryoFill Button

Activates or deactivates the CryoFill Liquid Nitrogen Filling System. When this feature is on, a sensor in the LN2 dewar in the Jade DSC detects the level of the LN2. If it drops below a certain level, the system will automatically bring in LN2 from the supply tank until it reaches the designated level.

NOTE: You must turn the CryoFill off when you are going to disconnect the supply in order to refill the supply tank.

Running Samples 277

Monitoring Data Collection

While a method is running, the data collected is presented in graphical form in the Instrument Viewer. You can also see the status of selected instrument parameters or signals as curves if Monitor is activated. The status of the instrument’s parameters is seen as well in the Status Panel. If you have multiple analyzers running, you can use the instrument buttons on the Pyris Manager to monitor the status of each analyzer while you do other work.

Instrument Viewer

The Instrument Viewer is a graphical window that displays the collected data in real-time during the run, as well as the status of selected analyzer signals in graphical form. For example, for a DMA 7e, you can display the Probe Position, Sample Temperature, Dynamic Force, and other parameters as a function of time. When a method is not running, the Instrument Viewer can display real-time baseline signals from the analyzer. You select what signals to display from the Curves menu. You can remove a curve from the display by selecting the curve and then pressing the Shift + Delete keys simultaneously. Stop the display of all selected curves in the Instrument Viewer by selecting Monitor in the View menu or the Reset Monitor button on the control panel. You can change the color, line style, and plot type of the curve by right-clicking on the curve and selecting the appropriate option from the popup menu displayed. You can change the axes labels and titles by right-clicking near the X or Y axis and selecting the option from the popup menu. You can toggle the grid lines on and off by right-clicking within the Instrument Viewer and selecting the option.

You can use the rescaling tools on the Rescale Tools toolbar or the rescaling options in the Display menu to redisplay the selected analyzer information and the real-time data.

Status Panel

The Status Panel is a dockable panel that appears in each Instrument Application window and Data Analysis window. It is made up of boxes each of which displays a parameter and its current value, for example, Probe Position for a DMA 7e. Select the parameter to be displayed in the box from a drop-down list of parameters. As soon as you select a parameter, its current value is displayed. You can also highlight the display field and type in the first letter of a parameter. For example, if you using a DTA 7 and type in “f” in a Status Panel box, one possible parameter that can be displayed is Furnace Lock. Type “f” again and Furnace Cover or Furnace Status will be displayed.

The Status Panel must contain at least one parameter box. To resize the Status Panel, that is, to eliminate or add a parameter box, first detach the Status Panel from the window frame (click it and drag it away from the window frame), then click and drag the Status Panel border to include or exclude a box.

You can hide the Status Panel to allow more room for other windows that are displayed beneath the Status Panel, for example, the Initial State page in the Method Editor. Select Status Panel from the View menu to toggle the panel off.

Click here to see an example of the Status Panel while a run is in progress.

Using the Monitor

You can monitor the status of an analyzer in the Instrument Viewer before the start of a run by selecting the Monitor command in the View menu. The Monitor command toggles the monitoring feature on and off. A checkmark appears next to the command in the View menu when the Monitor is on.


You can select what to monitor in the Instrument Viewer by selecting an item from the Curves menu. For example, for the DMA 7e you can display curves for probe position, static and dynamic forces, frequency, sample and program temperatures, amplitude, and phase angle. You can remove a curve from the monitor by selecting it and pressing Shift + Delete simultaneously. The Y-axis label is also removed.

Select Auto-Rescale in the Display menu to have Pyris scale the curve automatically. If you want to rescale the curve, use the Rescale Tools toolbar or the items in the View menu.

To clear the data in the Instrument Viewer, select the Reset Monitor button in the Control Panel. The Instrument Viewer will clear and the Monitor will restart.

Pyris Manager

You can use the Pyris Manager to monitor the status of multiple analyzers. Go to the Pyris Manager and display the Pyris Manager popup menu by placing the cursor in the background area of the bar and clicking with the right mouse button. Select Always On Top to keep the Pyris Manager bar displayed on top of all open windows. Reposition the Pyris Manager to a more convenient place on the screen by clicking and dragging.

Each analyzer button on the Pyris Manager has two status lines. The default items for display are temperature and analyzer status. When there is no run in progress, the first status line displays “Offline.” You can change the items displayed in these lines by using the Change Status Information dialog box.

The color of the LED in the upper-right-hand corner of each button indicates the status of the analyzer as follows:

Green: analyzer is on but no method is running Red: analyzer is heating (method is running) Yellow: analyzer is holding (method is running) Blue: analyzer is cooling (method is running) Dark Gray: analyzer is off

Running Samples 279

Remote Monitor

A powerful feature of the Pyris Software is that it can expand to a broad network of users. You can monitor the real-time status of and stop a run on an analyzer on a remote computer via a network connection. In the remote computer’s Remote Access page in Preferences, you must select the amount of access to your analyzer(s) that a remote user is allowed. You can open a Remote Monitor window for each analyzer configured on the remote computer. In order to use the Remote Monitor feature, you need an Advanced Instrument Control key. The Remote Monitor option appears in the Tools menu.

Remote Monitor is part of the Data Analysis application. There is one Remote Monitor window per Data Analysis application.

Starting the Remote Monitor

To start the Remote Monitor for a Pyris analyzer: 1. Open a Data Analysis Application

At your Pyris computer, open a Data Analysis application either by selecting Data Analysis from the Start Pyris Task menu, by clicking the Data Analysis icon on the toolbar, or by selecting it from the Pyris Software group in the Programs menu displayed from the Start button. At the Open Data File dialog box select any data file in order to open the Data Analysis application.

2. Open the Remote Monitor Click the Remote Monitor command in the Tools menu. The Select PC dialog box is displayed.

3. Select a Computer to Monitor With the PC tab selected, display the drop-down list of names of computers on the network that you can monitor. The first time you open the Remote Monitor, the name of only your computer is listed. This is the name you assigned when you installed Windows. Add a computer to the list by typing its name in the Name field. The next time you open the Remote Monitor, the computer name you entered will be displayed in the drop-down list. After entering the PC, click Connect.

4. Select an Instrument to Monitor After you select a computer to monitor, select the Instrument tab. All Pyris analyzers configured on the selected computer are listed in the drop-down list. Select the analyzer you want to monitor, then click OK. Only analyzers that are connected and running can be selected. Analyzers that are configured but not running are grayed out and cannot be selected.

Viewing the Instrument Monitor and Status Panel

After selecting and connecting to the remote analyzer that you want to monitor, the Status Panel for that analyzer appears and the Instrument Viewer displays the remote analyzer’s real-time curve. The Status Panel on your computer screen is exactly the same as what you see on the screen of the computer to which the monitored analyzer is attached. In addition, the Status Panel contains a Stop Run button at the left-hand side. If you have permission, you can stop a run on the remote analyzer by clicking Stop Run. Permission is set in the Remote Access page of Preferences.

The Status Panel is dockable. The current values of several analyzer parameters, read from the analyzer, are displayed in the Status Panel. You can customize the Status Panel to display different parameters.


Display in the Instrument Monitor

1. If Remote Monitor is activated when the monitored analyzer is running, the curve(s) displayed will include data starting from the beginning of the run.

2. If Remote Monitor is activated when the monitored analyzer is not running, the curve(s) displayed will include data only from the time the remote connection is made.

3. If Remote Monitor is already on when a run begins on the monitored analyzer, the data is cleared and data from the beginning of a run is displayed.

Turning the Instrument Monitor and Status Panel Off

1. When both the Status Panel and the Instrument Monitor are on and then the Status Panel is toggled off, the remote connection is maintained. The Status Panel can be redisplayed by clicking Status Panel in the View menu.

2. When both the Status Panel and the Instrument Monitor are on and then the Instrument Monitor is toggled off, the remote connection is maintained. The Instrument Monitor can be redisplayed by clicking Monitor in the View menu.

3. When the Status Panel is displayed and the Instrument Monitor is off and then the Status Panel is toggled off, the connection to the remote analyzer is lost. The connection can be reestablished by using Remote Monitor in the Tools menu.

4. When the Instrument Monitor is displayed and the Status Panel is off and the Instrument Monitor is toggled off, the connection to the remote analyzer is lost. The connection can be reestablished by using Remote Monitor in the Tools menu.

Stopping a Run in the Remote Monitor

Select the Stop Run button in the Remote Monitor Status Panel to stop the sample run you are monitoring. When you select this button, a confirmation message appears; select No if you change your mind and do not want to stop the run.

The Stop Run button may be inhibited by the permission setting on the PC that is running the analyzer. Permission is set in the Remote Access page in Preferences. Permission settings are (1) no access to the analyzer, (2) status monitoring only (no ability to stop a run remotely), and (3) status monitoring and ability to stop a run.

Running Samples 281

Pyris Player

The Pyris Player is used to create a play list of steps that control an analyzer with an autosampler. In general, a play list’s steps tell the analyzer/autosampler to load a specific sample from the sample tray, start a method, unload the sample, and perform postrun analyses and display specified curves. Pyris Player can also be used with an instrument that does not have an autosampler. Play lists can be created that automate post-run activities.

The Pyris Player features are:

• The ability to perform other tasks while a play list is being run.

• The ability to edit the currently running play list.

• Complete history files generated to record the success or failure of each item in a list.

• The ability to create a list of samples that is to be analyzed with the same method and then have the data files analyzed using the same data analysis list.

The Pyris Player is accessed in Instrument Application or Data Analysis by clicking the Pyris

Player button on the standard Pyris toolbar. The Pyris Player consists of six tabbed pages: Setup, Edit Play List, View List, View Sample List, View History, and View Sample History.

Setup Page

If you open Pyris Player while in Data Analysis, the Setup page allows you to select which instrument you would like to control with the player. If you open Pyris Player while in Instrument Application, the Player is used for the current instrument only.

Edit Play List Page

This page is where you create and edit play lists. The list is displayed in a format like that used in Windows Explorer. The folders are Prepare Sample, Sample Group, File Group, and Data Analysis. These folders contain items such as Load Sample, Start Method, Pause, or Display Curve. Sample Group contains two sections: sample list and data analysis list. File Group consists of File List and Data Analysis list.

Sample Group allows the instrument to run and analyze a set of samples identically. There may be more than one Sample Group in a Play List. You may choose any of the available commands for Data Analysis. The File Group allows you to analyze several data files in the same manner as Sample Group but without using an instrument run.

If a folder item has a plus sign next to it, click the plus sign to display the folder’s contents; the plus sign changes to a minus sign. Click the minus sign and the item folds up its list. An item’s relation to a folder and the folder’s relation to the entire list are shown by dotted lines. Use the Add a step, Insert a step, and Delete this step buttons to create and edit the play list.

View List Page

This page displays the play list in a manner similar to that shown in the Edit Play List page, that is, use the "+" and "–" signs to open and close parts of the list. Since the page does not have the Edit Steps section, there is more room for displaying the play list. The View List Page is for viewing purposes only.


View Sample List

This page displays in spreadsheet format the list of samples in a sample group in the current play list. The columns in the spreadsheet are sample ID, file name, method used, carousel location of the sample, and the sample's weight.

View History Page

This page displays the history of the playback of the play list. Each time the play list is run, the system records the success or failure of each step. The play list is displayed in the same format as in the Edit Play List and View Play List pages except that the "+" and the "–" signs are replaced with other symbols that indicate if the item was completed successfully. A history file can be deleted from the list.

Sample History Page

This page is the same spreadsheet as seen in View Sample List except for the additional column before Sample ID. This column contains a code that indicates the status of the sample's run: O = OK, S = Skip, and X = Error.

When you enter the Pyris Player, the standard toolbar is replaced by the Pyris Player standard toolbar and a control bar.

Pyris Player Toolbars

When you enter Pyris Player, the standard toolbar seen in Instrument Viewer, Method Editor, and Data Analysis is replaced by a smaller toolbar and an additional toolbar whose buttons control the playback of the play list. These toolbars can be moved to other positions at the top of the screen. It is convenient to have them next to each other directly beneath the menu bar.

Pyris Player Standard Toolbar

The Pyris Player standard toolbar is as follows; click on each button to see a description of its function:

Pyris Player Control Bar

The Pyris Player control bar appears below the standard toolbar when you open Pyris Player. This bar controls the playback of the play list. Click on each button for a description of its function:

Pyris Player Setup Page

If you select Pyris Player while in an Instrument Application, the Player opened is for that instrument alone. You can open Pyris Player from another Instrument Application for another instrument on your system. For example, if you have a Pyris 1 DSC with an autosampler and a DSC 7 Robotic System as your Thermal Analysis system, you can have a play list for each instrument operating simultaneously.

If you are in Data Analysis Application when you select Pyris Player, use the Setup page to select with which instrument you would like Player to be associated. Analyzer Type

Running Samples 283

If you are in the Data Analysis Application when you click the Pyris Player button on the toolbar, then the drop-down list for Analyzer Type will display all available instruments from which to select the desired instrument. When you go to the Edit Play List page, the last play list displayed for that instrument is seen. If you are in an Instrument Application, the only instrument listed in the drop-down list is that particular instrument.

NOTE: If you are running Pyris version 9 with your analyzer, all older play lists of the same type (the same file extension) are usually compatible. However, play lists that you create for an analyzer in version 9 may not operate with an older instrument with software older than version 9. The exception to this is any Sample List that has the speed improvement.

Lot ID

If your laboratory groups samples into lots, this field is where you can record the lot number of the samples you are going to run with the play list. This is particularly useful for runs on an autosampler. Comment

You can enter free-form text describing what the play list does in the Comment field. There is no limit to how long the comment can be.

Pyris Player Edit Play List Page

The Edit Play List page is where you can create and save play lists or open existing lists to edit or run. The Player Steps area shows the steps of the list as you add, insert, or delete steps using the buttons to the right. The area underneath the Player Steps area, the Edit Step area, contains fields in which you enter values to be used in the play list. Enter the values and then click the step in the list in order for the new values to be displayed in the Player Steps area.

Levels

There are four main levels in a play list: Prepare Sample, Sample Group, File Group, and Data Analysis. These main levels contain second-level entries. Your play list does not have to have all four. A typical play list may contain a Prepare Sample section and a Data Analysis section. Another list may be just Data Analysis procedures.

Sample Group is used to run several samples with the same method. A Sample Group comprises a Sample List and a Data Analysis list. The samples in a Sample List are similar and are run using the same method. The data are then analyzed using the same data analysis commands. Sample Groups are particularly useful with an autosampler. The steps that you would have to enter into a regular play list are added automatically when a Sample List is run. A Sample Group can be embedded within a regular play list or it can stand alone. A play list can contain many Sample Groups.

A Sample Group can be used with an analyzer without an autosampler. Automatic Pause dialog boxes are displayed at the appropriate points by the program, to allow you to remove or load a sample at these points.

File Group can be used to analyze groups of data after they were collected. File Group comprises a File List and Data Analysis List. The File List contains one or more File List Items. The Data Analysis List contains zero or more data analysis items. File Group is designed in much the same way that Sample Group is designed. A major difference is in the File List as compared with the Sample List. A Sample List contains, in addition to the list of sample items, method information that is used to run each of the sample items in the list. A File List contains only the list of File items.


The Edit Play List page contains the following items: Player Steps box

Displays the steps of the play list as you add, insert, or delete them using the buttons to the right. The play list is initially displayed in expanded mode as it is created. You can compress parts of the play list by clicking on the minus signs next to the main-level items Prepare Sample, Sample Group, File Group, and Data Analysis. The second-level steps beneath will disappear and the minus sign will be replaced by a plus sign. You can see the play list alone and in its own window by clicking the View Play List tab.

Add a step button

Use this button to start creating a play list or to add a step to the end of an existing play list. The Player Step Options dialog box is displayed when you click Add a step. The items available to add to an existing play list will depend on the type of analyzer and what is already in the play list. A play list always starts out with Prepare Sample, Sample Group, File Group or Data Analysis.

Insert a step button

As soon as one step is in the Player Steps area, the Insert a step button becomes selectable. When you insert a step, it appears above the step that was highlighted when you

Running Samples 285

selected Insert a step. The items that appear in the Player Step Options dialog box for insertion depend on the main-level item immediately above the insertion point.

Delete this step button

Highlight the step you want to remove from the play list and click Delete this step. If other steps in the play list are dependent on this step, a Dependencies List dialog box is displayed. For example, if you try to delete a Display Curve step, you may be reminded that an Add Curve step below it depends on that step.

Edit Step Section

Whenever an item is added or inserted into the play list, an item-sensitive Edit Step section appears below the Player Steps section. The step number and item name are shown. Parameters specific to the play list item are displayed for editing.

Creating and Running a Play List Creating and Editing a Play List

When creating a play list for any analyzer, the items in the Player Step Options dialog box consists of Prepare Sample, Data Analysis, File Group and Sample Group. The list of items in the Player Step Options dialog box when adding a line to or inserting a line into the play list depends on the analyzer and the highlighted step at the time.

• When you click Add a step, the new step is always appended to the end of the play list, no matter which play list item is highlighted.

• When you click Insert a step, the new step is inserted above the highlighted step.

• The choices displayed in the Player Step Options dialog box depend on what main-level item the added or inserted item will appear beneath: Prepare Sample, Data Analysis, or Sample Group. For example, if you are adding or inserting a line beneath a Display Curve entry, which would appear under Data Analysis, the Player Step Options dialog box contains the same selections that appear in the Math, Calc, and Display menus.

• As you add or insert steps into the play list, the Edit Step area below the Player Steps box displays information and fields specific to that step.

The main-level items in a regular play list are numbered 1, 2, 3, etc. The second-level items are numbered x.1, x.2, x.3, etc., where x is the number of the main level item directly above. These items are indented. Dotted lines connect the main-level items to their second-level items. Since the area in which a play list's steps are displayed is small in the Edit Play List page, use the View Play List page to get a better picture of the structure of the play list.

Saving a Play List

When Pyris Player is running, the Save options under the File menu and on the toolbar will save the play list file.

Running a Play List

Click the Pyris Player start button on the control bar to start a playback of the play list at the top of the list, that is, from the first entry.

NOTE: Once a player file is started, do not choose a furnace or balance command outside player. Doing so will halt the player.


Pyris Player View Play List Page The Pyris Player View Play List page shows the current play list only. This view is useful for displaying the play list in compressed or expanded form. Since there are no buttons or an Edit Step area, the play list has more room for display. This makes it easier to read and to get a better overview of what the play list is doing. Use the “+” and the “–“ symbols to the left of the first-level items (numbered 1, 2, 3, etc.) to expand or compress the list beneath that item. Prepare Sample, Sample Group, File Group, and Data Analysis are like folders that contain additional folders and/or steps.

Running Samples 287

Pyris Player View Sample List

The View Sample List page is a more compact display of the samples to be run in your play list. You can edit the information about a sample or samples in this list rather than on the Edit Play List page. Data in every column can be edited except for the Method Used column for samples in a Sample List as part of a Sample Group. Since the method used applies to all the samples in the Sample List, you cannot change the method for a particular sample. You would need to change the method for the Sample List in the Edit Play List page.

A play list in the Edit Play List page and its associated View Sample List page are shown below:


Place the cursor in a field on any sample line and that value is displayed in the display field above the sample list. There you can change the value. When in the Sample File Name or Method Used field, a Browse button appears next to the display field. If you want to change the directory in which the data file will be saved, click on the Browse button to display the Save in dialog box to change the path. For a method, when you click on the Browse button, the Look in dialog box is displayed in which you can look for and select another method to use.

To print data with grid and column lines:

1. Set the cursor to the beginning of the first column to print the entire table.

2. From the edit menu, select Copy Sample Grid. The control Copy Sample Grid is disabled when the table is empty.

NOTE: To make the information more visible, drag the vertical column separator all the way to the right of the margin for each cell. The Pyris Player does have column widths limitations. Users can also use the Copy Sample Grid command to export data into Microsoft Excel.

Pyris Player View History Page

The View History page of Pyris Player lists the history of the playback of the play list. It is also a real-time update list so as a play list is in playback mode, the history list is dynamically revised to reflect the status of a play list step. There is a history entry, indicated by the symbol , for each time the play list is run, with the date and time of the run displayed. Click on the “+” to the left of History entry to “open up” the history folder; this displays the main-level entries of the play list: Prepare Sample, Sample Group, File Group, and Data Analysis. Click on the “+” next to those entries to open the folders and display the

Running Samples 289

second-level steps in the folders. If there is a green checkmark before the step, the operation was performed successfully. If appears in front of a step, the operation failed. Double click on the “+” to the left of the to display an additional Error line that explains why the playback of the play list entry failed. A blue down arrow indicates that the step was skipped. A Pause is indicated by a blue flag .

More Detail

Click on this button with a history entry highlighted to display a dialog box showing the date and the time that the entry was executed. Some entries' More Detail dialog boxes will contain additional information. For example, for a Start Method entry, the following dialog box is seen:

Delete History

You can delete a history entry by clicking this button. The focused line must be a History line when you select this feature. You are warned that the entire block (that is, all the entries associated with that run) will be deleted. You can cancel the deletion request by clicking the Cancel button.

Delete All

This button will delete all of the history entries in the View History page. You are warned that the entire History List will be deleted and are given the chance to cancel the request.


Expand All/Collapse All

These buttons toggle the display of the History List between full view and collapsed view. The sample History List above is expanded; all entries for all History files are displayed. The same History List collapsed is as follows:

Pyris Player Sample History Page

The history of the samples run by the current play list can be displayed in the Sample History page. This page can also be used to dynamically display the current run's history. To select which History file to display, click on the down arrow in the display field above the sample listing to show all of the History files for the play list.

• To show the current run's history, check the Current History check box.

Running Samples 291

The first column in the Sample History page displays the item number in the play list that generated the data file. The second column displays the status code for the sample in the History file. If the sample ran with no errors, an O is displayed. If the sample was skipped for any reason, for example, there was no sample pan in the designated autosampler location, an S is displayed. If there was an error running the sample, for example, there was a problem with the selected method, an X is displayed.

The remaining columns are similar to those in the View Sample List page: the data file name, method used, location (relevant for autosamplers), and Detail Description. If there was an error, this field displays the error message generated. If the run was OK, this field displays the sample weight. These fields cannot be edited.

To print data with grid and column lines. Set the cursor to the beginning of the first column to print the entire table. From the edit menu, select Copy Sample Grid. The control Copy Sample Grid is disabled when the table is empty.

NOTE: To make the information more visible, drag the vertical column separator all the way to the right of the margin for each cell. The Pyris Player does have column widths limitations. Users can also use the Copy Sample Grid command to export data into Microsoft Excel.


Valet

Valet runs outside of a method and can be used for any of the following tasks:

• Trigger events at a certain time of day

• Switch on/off power to instruments and accessories, such as chillers

• Trigger an external device using the X10 Relay switch

Starting Valet

1. Click on the Instrument Viewer window.

2. Click on in the Toolbar. The Pyris Valet window appears. An example of how you can use Valet is shown below.

Using Valet

Valet is controlled by actions and events. This means that you define one or more specific events that must occur before any given action take place. For example, you can specify that you want to trigger an external event when a certain time of day is reached.

Table 1: Actions you can select using Valet:


Start a Play List

You can start a play list when one or more of the available events have occurred. Your options are to start a play list at a specified

Running Samples 293

time, immediately, or when a signal is received from an external relay box.


This action will trigger a signal to a channel on an external device.

Table 2: Events you can select using Valet:


A Time of day is reached

The action will occur once a specified time is reached.

An External Event occurs

A signal is received from a channel on an external relay box that triggers the action to occur.


The action will occur immediately when the action starts.

To select an action and event:

1. Click on the Add Action button.

2. A dialog box appears that asks you to select an action. For information on each action, refer to the table above.

3. If you selected the action of Trigger an External Action, you will need to select the external channel in the next dialog box that appears.

4. A dialog box appears that asks you to select an event. For information on each event, refer to the table above.

5. Select one of the events listed in the dialog box, then click on OK.

To modify actions and events:

1. Position the mouse cursor in the white box and click the right mouse button.

2. A pop-up menu appears. Select one of the following commands:

Use this command in the pop-up menu... To do this...

Edit an Item To change the conditions associated with an action or event

Delete an Item To delete an action or event

Change an Item To select a different action or event

To cause an action to start immediately:

1. After starting Valet, select the action (highlight it).

2. Right-click and select Do Action Now in the pop-up menu.


To repeat the events listed in the dialog box

1. Select the Loop checkbox.

2. Click Start Valet. The actions listed in the dialog box will be repeated until Pyris Valet is paused or stopped.

Analyzing Data


Data Analysis

The Data Analysis Application can be accessed by selecting Pyris Data Analysis either from the Pyris Software menu in the Programs menu or from the Pyris Manager Task menu displayed by clicking the Start Pyris button in the Pyris Manager panel. When you access Data Analysis either of these ways, you have access to all data files, that is, data from all attached analyzers. You can also access the analyzer-specific Data Analysis application by

clicking the Data Analysis button on the toolbar while in an Instrument Application. However, the only data files you can call up for analysis are those associated with the current instrument.

Pyris Software lets you analyze data collected from any thermal analyzer. Data are saved to the file that you specified in the Sample Info page in the Method Editor, to the file specified in a play list, or to the default file name specified in Preferences. You can open multiple Data Analysis Applications from the Pyris Manager as well as open Data Analysis windows inside an Instrument Application. You can switch from one Data Analysis window to another by clicking on the appropriate Data Analysis button in the Pyris Manager. As each Data Analysis window is opened, it is indicated by an additional button in the Pyris Manager bar, in addition to the instrument buttons.

In Data Analysis, you can perform many functions on a data file to manipulate the data. The menus available while in Data Analysis indicate the possibilities. The items in these menus can be used to rescale the displayed curves, display different types of curves for the data, perform calculations with the data, and other functions.

Analyzing Data 297

Display Curves

In order to analyze your data that has been collected in a run and saved to a data file, you must first display it in a Data Analysis window. More than one curve can be displayed in a window and more than one Data Analysis window can be open at the same time.

Select the Data Analysis Application

After a run, click the Data Analysis button on the toolbar to open Data Analysis. This Data Analysis Application is associated with the particular Instrument Application you are using. You can also open a Data Analysis Application for another analyzer by selecting Data Analysis from the Pyris Manager Task menu.

Select the Data File

In the Open Data File dialog box, select a data file for display. The curve is displayed as it was last displayed before closing the file. The default settings for displaying curves can be adjusted in the Preferences window.

Use the Menus

Use the items in the View menu, Display menu, and Rescale Tools toolbar to change the display of the data. Use items in the Curves, Math, and Calc menus to display different curves and manipulate the data. Use the File menu items to add a curve to the display, open another window, or close the window.


Optimizing the Data Display

A curve displayed in the Instrument Viewer and the Data Analysis windows can be optimized a number of ways, mainly by using the rescale tools on the Rescale Tools toolbar. Some of those tools are also on menus.

Rescaling

You can optimize the display of the data file by rescaling the X- and Y-axes of the Instrument Viewer or the Data Analysis window, thereby displaying only a portion of the curve(s) in the window. There are three ways to rescale:

1. Create a box around the portion of the curve you want to display by clicking on the mouse and dragging it. While dragging, a box is created. Once the box is around the desired area, double click inside the box. Both X- and Y-axes of the active curve are automatically rescaled. If the Radar window also is displayed while rescaling, its box is redrawn to reflect the new scaling.

2. This action rescales the X-axis for all curves and the Y-axis of the active curve. All curves using the same Y-axis as the active curve are also displayed on the new Y scale. All other curves are rescaled in the X direction only.

3. You can resize the existing box in the Radar window. The curve in the Data Analysis window will be rescaled accordingly.

4. Use the commands on the Display menu or the buttons in the Rescale Tools toolbar to rescale: Rescale X Axis, Rescale Y Axis, Full X Scale, Full Y Scale, Full Scale, and Previous Scale.

Shift Curves

You can shift any heat flow, baseline heat flow, or unsubtracted heat flow curve vertically

along the Y-axis using the Shift Curve button on the Rescale Tools toolbar. This button is gray until a heat flow curve is displayed. Shifting a curve vertically makes it easier to see differences between curves that are overlapping. When you shift a curve, only the curve moves; the axes and scales do not change.

Select the curve you want to shift by making it the active curve, then select the Shift Curve button in the Rescale Tools toolbar. The Shift Curve dialog box appears and an X appears on the active curve.

Analyzing Data 299

The shift along the Y axis is defined by two points: the Shift From point and the Shift To point. The point at which the X intersects the active curve is the Shift From point. The Shift To point is the Y-axis value to which you want to move the Shift From point. Use the mouse to drag the X to the desired Shift From and Shift To points or type the values directly in the dialog box.

If you select the Align All check box, all curves in the active Data Analysis window that share the same Y-axis will shift to the point on the Y-axis defined by the X. This is a quick way to shift more than one curve.

Change the Curve's Slope

You can change the slope of any heat flow, baseline heat flow, or unsubtracted heat flow

curve using the Change Slope button on the Rescale Tools toolbar. When you change the slope of a curve, only the active curve is affected; the axes and scales do not change.

Select the curve whose slope you want to change, then select the Change Slope button on the Rescale Tools toolbar. The Change Slope dialog box appears:

A line representing the slope is placed on the curve. The left end of the line is the pivot point and is identified by a small box. The right end of the line is the slope point and is identified by an X. Use the mouse to drag the pivot point and the slope point to the desired coordinates on the curve or type the X coordinates for each point directly in the Change Slope dialog box. The values in the dialog box update automatically when you move the pivot and slope point markers with the mouse. If you type the coordinates in the dialog box, the slope line on the curve does not update until you click OK. The pivot point must always be to the left of the slope point.

Align Endpoints automatically assigns the slope point and the pivot point to the same Y value, forcing the slope line to be horizontal and the slope to be 0.

Annotate Curves

Another way to optimize the data curve display is to add informative and descriptive text

labels. Either click on the Annotate button on the Rescale Tools toolbar or select Annotate from the Display menu to display the Annotations dialog box. The labels you add can be saved with the data or used for display only. You can create multiple labels for each curve. You can reposition, edit (for example, change its font, color, and orientation), and delete an annotation.


DMA 8000 (TTS) Time-Temperature Superposition

Time-Temperature Superposition (TTS) Optimizing the Data Display analysis allows modelling of material behaviour at low and high frequencies collected using the DMA 8000 (0.001 Hz to 600 Hz), which may be more representative of “real world” applications. At the low frequency end of the frequency spectrum, “creep” measurements may be carried over many months or even years, however modelled data from DMA using TTS can give an indication of long-term behavior in a very short time. Similarly, higher frequencies such as those which represent “impact”, typically in the kHz range, can be investigated quickly and easily using DMA in a way which allows meaningful comparisons between different sample treatments or modifications to be assessed.

It should be stressed that TTS is a modelling technique and results may be incorrect and misleading or wildly inaccurate in the worst cases. It is up to the scientist carrying out the measurements to make an assessment of the validity of the data and this will usually involve a correlation with other forms of measurement. A full treatment of the technique and its theory is outside the scope of this topic.

How Does TTS Work

The data required for TTS is collected using a series of frequency scans collected at isothermal temperatures in a range which passes across the glass transition of the material being tested. When correctly chosen the start temperature, end temperature and the temperature steps produce a set of data called a “frequency dispersion”, and an example taken from a PET film in tension mode is shown below.

The data shows the classical series of scans which start off at the highest modulus of the sample when the temperature is below its glass transition then, as the sample starts to enter the glass transition, the lowest frequencies show the “below Tg” modulus while the higher frequencies still show the “above Tg” modulus – this is related to the shift in glass transition due to frequency and these are seen in the PET sample below. This data was collected at 1 Hz, 2 Hz, 5 Hz, 10 Hz and 20 Hz and scanned at a rate of 3 °C/min and demonstrates the measured shifts to higher temperatures as the frequency increases. This frequency-dependant shifting is the behavior which allows us to create the classic frequency dispersion curves shown below.

Analyzing Data 301

Will TTS Work on my Sample?

Before TTS can be used, suitable data must be collected. The first stage is to assess whether the material itself is suitable for TTS analysis. To do this, a simple temperature scan at 1 Hz eg. at 3 °C/min must be run.

How to Use Time-Temperature Superposition

1. Open a dm8d file and remove all the curves.


2. Select the ordinate(s). Ensure that you checked the Display each step as a separate curve in the Step Select dialog.

3. Set Frequency as the x-axis.

4. Click Time/Temp Superposition in the Calc menu to start TTS.

Analyzing Data 303

The TTS dialog the TTS Wicket Curves and TTS Master Curves view display.

In the Time/Temp Superposition dialog you can use Auto-Shift or manual shift.

5. Click Finish to end TTS. Three views display for TTS data: TTS Master Curves, TTS Shift Factor Curves, and TTS Wicket Curves.


6. Select the Data Analysis view, where you can Save the data and close the files. If you click Save, TTS data will be saved into dm8d file. or Click Export TTS Data… in the File menu to export TTS data to CSV file.

7. Reopen the dm8d file. In the Curves menu, click TTS then select All Curves.

Analyzing Data 305

Three TTS views will be displayed.


Math, Calc, and Curves Menus

Math, Calc, and Curves Menus

You can display additional curves based on the data represented by the active curve in a Data Analysis window by using the items in the Curves, Math, and Calc menus. The new curve is added to the active Data Analysis window. You can also display other curves in the Instrument Viewer.

The data saved from a run includes analyzer signals pertaining to certain parameters. For example, the sample and program temperatures are saved for all analyzers. The heat flow is saved for DSC analyzers. Weight and weight % are saved for the TGA analyzers. Probe position, static and dynamic forces, frequency, amplitude, and phase angle are saved by the DMA analyzers. In addition, for the DMA /TMA analyzers, other parameters such as expansion coefficient, volumetric expansion, and modulus are also saved and can be displayed as curves in the Data Analysis window. These analyzer signal curves are on the Curves menu.

In the Data Analysis application for all analyzers, you can display curves that are calculated using the data in the active curve by selecting a command from the Math or Calc menu. The calculated curve is added to the window and becomes the active curve. You can perform such calculations as obtaining the derivative, adding curves together, subtracting, averaging, smoothing, peak area, glass transition etc. You can also smooth and normalize the focused curve.

You can display data from one or more method steps rather than all of the data in the active curve by selecting the Step Select command in the Curves menu. When you select this command, a checkmark appears next to the command in the menu. As long the checkmark is displayed, Step Select is "on." Each time you select a command in the Curves menu to display a different curve, the Step Select dialog box appears. Click the Select All button to highlight and select all of the steps.

Math Menu

The Math menu is available only for Data Analysis windows. The Math menu for all analyzers contains the following commands:

• Derivative

• Subtract

• Add

• Average

• Smooth

Analyzing Data 307

Calc Menu

The Calc menu is available on the menu bar in Data Analysis. It contains the following commands, some of which are analyzer-dependent:

• Peak Area

• Peak Search

• Tg Calculation (DSC only)

• Step

• Heat Flow

• Crystallinity (DSC only)

• Onset

• Delta Y

• Delta X

• Event Mark

• Trigger

• Slope

• Oxidative Induction

• Response Ratio

• Specific Heat

• Purity

• Kinetics

Curves Menus

The Curves menu is available when either the Data Analysis window or the Instrument Viewer is displayed. In Instrument Viewer, the Curves menu allows various curves to be displayed during data acquisition. The contents of the Curves menu in Data Analysis depends on the analyzer used to collect the data file displayed.


Viewing Methods and Results

After displaying, optimizing, and performing calculations on the data curves, you can view and print out those results in several ways.

View Results

When you perform calculations, the results are not saved unless you save the data file. When a data file with calculations is recalled, the results are not automatically displayed on the screen. Use the Results command in the View menu to display the calculation results. When you select this command, the View Results dialog box appears. All of the calculation results saved with the active curve or performed during the current session and which can be displayed are listed. Select one or more results, then select the View Results button. The calculations whose results cannot be displayed on the current axes are listed separately.

Use the Delete Results button in the View Results dialog box to delete calculation results from the active curve’s data file or results obtained during the current session, for example, the Van’t Hoff curve for purity. The results deleted from the dialog box list will be deleted from the data file only when you save the file.

Printing Curves

Use the Print command or the Print button on the toolbar to print the active Data Analysis window. Before printing you can use Print Setup in the File menu to set up the page(s) on which the output will be printed. The Page Setup dialog box contains three tabbed pages in which you define a title, margins, and header and a footer for your printout. To see what your printout will look like before printing it, select the Print Preview

command in the File menu or the Print Preview button on the toolbar.

When you select the Print command, the Print dialog box appears. Select the printer and the number of copies to print, or select the Properties button to display the Print Properties dialog box. In the Print Properties dialog box, you can access a number of different print options, including whether to print in Landscape or Portrait mode.

View Methods

You can view information about the method used to collect the data displayed in the Data Analysis window. Make the desired data curve the active curve, then select the Method Used command in the View menu. The View Method Properties window appears. This window comprises six pages which display the following information:

Sample information Initial conditions Equilibration parameters Method step information Validation Information Calibration information

You can change such parameters as the Sample ID, Operator ID, and Comment for your data file. The other information is for display only; it cannot be changed.

Using the Create button on any of the pages, you can save the method as an ASCII file with the same file name as the method but with a .TXT extension.

Analyzing Data 309

Print Methods

There are two ways to print a method:

• With the Method Editor as the active window, use the Print command or the Print

button on the toolbar to print the method currently displayed in the Method Editor.

• With a Data Analysis window as the active window, select the Method Used command in the View menu. Click the Print button on any of the six pages of the View Method Properties window.

To see what your printout will look like before printing it, select the Print Preview

command in the File menu or the Print Preview button on the toolbar.

Copy Methods

You can export your methods from Pyris Software by copying them to an ASCII file and then using the file in third-party software. Use the Method Used command in the Data Analysis window View menu to perform this function. When you select this command, the View Method Properties window appears. Select the Create button to create the ASCII text file. The file has the same file name as the method but has a . TXT extension. It is saved in the same directory as the method.

Include the data points collected in the run and/or the Calibration Information by selecting the appropriate check box before creating the ASCII file. The data points are saved as an ASCII table of values.


Saving Processed Data

To save what is displayed in the Data Analysis window, select the Save button in the toolbar or Save Data from the File menu. The derived curves currently displayed in the Data Analysis window along with the calculation results stored with these curves and the original data and method are saved. When you open the data file again, the data will be displayed as you saved it. Use Save Data As from the File menu to save the data under a different file name. The original data file still exists.

If you delete a curve from the display and then save the data, the curve and all results calculated on that curve are not retrievable.

NOTE: If you are using Pyris Enhanced Security when you select the save command the file is saved automatically, and a copy of this file is placed in the History directory with a version number attached to the file name. This prevents older versions of data files from being overwritten.

Sharing Data


Sharing Data

There are several ways you can share data using Pyris. Click on the links below for more information: Create a report Export the data Import and convert data from other instruments

Sharing Data 313

Report Manager

Report Manager

The Pyris Report Manager gives you the capability of exporting a Pyris data file to a document in Microsoft Word or HTML (Hypertext Markup Language) format. The software lets you create a report template in order to specify the design of the report and the information that the report contains. This template can be used over again to facilitate the creation of new reports.

Starting Report Manager

1. Start the Data Analysis application.

2. Open the data file that you want to use to create the report.

3. In the Tools menu, select Report Manager.

4. The Report Manager dialog box appears (see illustration below).

Using the Report Manager See the following topics for more information: Select a Stored Template or Create a New Template Select the Output File Specify Items in Report and Template Design Create the Report


Select a Stored Template or Create a New Template

To create a new report template

1. In the Report Manager dialog box, click on the button. The Select Report File dialog box appears.

2. Type a new filename in the File Name box, then click on Open. The software creates a filename with the extension “.rpp”. This is the filename where the template information will be stored.

To select a stored template

If you have already saved a template, you can select this template and use it as is, or modify it. If you choose to modify it, you can use it as the starting point for a new template and save it under a new name.

Click on the button to select a previously stored report template file. In the dialog box, select a different directory if necessary and select the file. The default location for templates is the Data directory.

Select the Output File

The Output File is the report that the software creates in Microsoft Word or HTML format.

Enter a name for the Output File. If you do not specify an extension for the file name, the software will automatically add the extension “doc” and will use Microsoft Word format (for example, “ABC Labs report.doc”). If you want to have the report created in HTML format, use the extension of “.htm” or “.html”, for example “ABC Labs report.htm” or “ABC Labs report.html”.

The default location for the Output File is the Data directory. Click on the button to select a different directory.

As in the naming of data files, you can use one or more “#” signs in the Output filename to automatically number the files in sequential order. For example, if you use the name ABCLabs##, the software will generate a series of reports with the following names: ABCLabs01, ABCLabs02, ABCLabs03, etc.

If you do not use a “#” sign in the filename, each time you specify the same Output File, new reports will be appended to the end of the file.

TIP: If you are using the same Output File each time you generate a report and appending information to the end of the file, specify a New Page at the end of your template. By doing this, each new report will start on a new page.

Sharing Data 315

Specify Items in Report

Template Description: This box shows a descriptive name for the template. You can edit this name if desired.

NOTE: If you change the name, the actual filename for the template will not change.

Orientation: Click on Orientation in the Report Output box to select the orientation of the printed page. Landscape is a wider format and will fit more columns on one page. The Orientation is always listed as part of the final template.

Portrait Landscape

Header/Footer: A Header appears in the top line of the report on each page. A Footer appears in the bottom line on each page. A Header/Footer is useful for automatically inserting the filename of the report, page numbers, the date the report was printed, or other information. The Header/Footer is always listed as part of the final template, even if you choose not to use a header or footer.

To specify the Header/Footer:

1. Click on Header/Footer in the Report Output box.

2. To type in your own Header or Footer, you first must remove the checkmark from the Use Autotext box. Then, type the desired text in the Header or Footer box.

3. OR

4. Select Use Autotext and select either Filename or Date Printed in the drop-down list. The Filename is the name of the Output File. The Date Printed is the date that you actually print the report (not necessarily the date that the report is created).

You can include page numbers in the Header or the Footer by selecting the Include Page Number box. The page number will appear on each page of the report.

An example of how you can fill out the Headers & Footers dialog box is shown below.


To select the items that you want to include in the report:

The Report Options box on the left shows a list of items that you can choose from to include in the report template. The Report Output box on the right shows the list of items that have been selected. The order of items in the box on the right is the order in which the information will be printed in the report.

TIP: Select New Paragraph between each item to place a line space between items in the report. Select New Page at the end of the report to start reports appended to the same file on a new page.

To add items:

Click on an item in the box on the left. Click on Add ==>. The item appears as the next item listed in the box on the right.

To remove items:

Click on an item in the box on the right. Click on <==Remove. The item is removed from the box and will not be included in the report.

NOTE: Orientation and Header/Footer cannot be removed from the list.

Sharing Data 317

To edit items:

You use the Edit button to change the information specified for one of the items. First, click on the item you want to modify, then click on Edit…

An example of how you might specify a template is shown below.

The different items that you can include in the report are described below.

Sample Info

Sample Information can include the filename of the data file, the Sample ID, the Operator ID, Comments in the data file, Sample Dimensions (Weight, Height, etc.), and Collection Date and Time.

Method

Method information is for the method used to generate the data and can include the Method filename, the Instrument Type, Instrument Name, Instrument Serial Number, and Software Version Number.

Calibration

Calibration information can include the Calibration File Name, and the Calibration Date and Time.

New Paragraph

This is used to insert a blank line between sections of the report.

Graph Image

This will place a picture of the most recent plot and curve shown in Data Analysis in the report.

Results

You can display either the most recent result or all of the results from the currently focused curve.

Data Table

The Data Table is a representation of the currently focused curve in a table format. The increment you select on the x-axis will determine the amount of data in the table. Select the increment carefully, since the same increment will be used regardless of the X-axis units currently in use.


Text

You can type in any text you want to appear in your report. For example, you can include headings, descriptive information about the analysis, or notes.

New Page

This will add a page break in the report. Select New Page at the end of the report to start reports appended to the same file on a new page.

Bitmap File

Select the bitmap that you want to include in the report. For example, you can include a bitmap with your logo at the beginning of the report by selecting Bitmap as the first item in the template.

Sharing Data 319

Create the Report

The Report Manager gives you the following options:

• Generate the Report

• Print the Report

• Preview the Report

To generate the report:

Click on Create Report to generate the report according to the specification in the Report Manager. You can then open the report in Microsoft Word. The report is stored in the directory specified for the Output File. The default location is the Program Files (x86)/PerkinElmer/Pyris/Data directory.

To see a preview of the report:

You can see how the report will look before you print it, then make any modifications desired, and later print the report.

1. Click on Create Report to generate the report.

2. Click on the Preview button. The report is shown in Microsoft Word.

3. Use the Page Down key or scroll bar to view all the pages in the report.

NOTE: Disregard the filename shown in Word. A temporary filename is displayed in the preview, not the filename you have assigned for the report.

4. Close the preview window to return to Pyris. (You cannot use Pyris until the file is closed.)

To print the report

To print all the pages in the report, check the Print All Pages box. To print only a portion of the report, remove the checkmark from the Print All Pages box and specify a start page and end page. For example, to print only page 1, select 1 for both the start page and end page. Click on Print Report to start printing.

NOTE: To cancel printing, select Start > Settings > Printers from the Windows task bar. Double-click on the name of the printer. In the Printer menu, select Purge Print Documents.


Printing

Print dialog box

The standard Windows Print dialog box appears when you select the Print command in the

File menu throughout Pyris Software or the Print button on the toolbar. It is the same dialog box you see when you print in other applications on your computer. The options in this dialog box allow you to specify how the data, method, calibration file, or play list should be printed.

Name

This is the name of the active printer. Select the drop-down arrow to display additional printers available to you. The four fields – Status, Type, Where, Comment – are informational only. They cannot be changed.

Print to file

Click in this checkbox to print the information to a file rather than directing it to the printer. You will be prompted to specify a file name and location.

Properties

Click on this button to set up options for the selected printer. The options available depend on the printer.

Print Range

Specify the pages you want to print:

• All prints the entire document.

• Pages prints the range of pages you specify in the from and to boxes.

• Selection prints the currently selected text.

Copies

Specify the number of copies you want to print for the specified page range.

Collate

When more than one copy is to be printed, the Collate button is activated. Prints copies in page number order instead of separated multiple copies of each page.

Print Setup dialog box

The Print Setup dialog box appears when you select the Print Setup command in the File menu in Calibrate and Pyris Player. It also is displayed when you click on the Setup button in the Page Setup dialog box which is displayed first when you select Print Setup in the File menu in Instrument Viewer and Data Analysis. It is the standard Windows Setup dialog box you see in other applications on your computer. It contains the following fields:

Sharing Data 321

Name

Select the printer you want to use from the list of printers available to you. The default printer of your system is the default. Click on the down arrow to see additional printers. You install printers and configure ports for your system using the Control Panel.

Properties

Click this button to access the dialog box in which you set up options for the printer. The options available depend on the features of the printer.

Size

Select the size of paper on which the document is to be printed.

Source

Some printers offer multiple trays for different paper sources. Specify the tray here.

Orientation

Choose Portrait or Landscape.

Network...

Choose this button to create a connection to a network printer. You must have the proper printer driver available.


Exporting Data

Data collected by Pyris can be exported as a data text file in the ASCII format.

1. Select File>Export Data>ASCII format.... The Create Text File dialog box is displayed.

2. Choose the content of the text file. The header information from the Pyris data file is exported by default. Select Include Data Points to add the data for the program performed by the instrument. You can add the calibration information current at the time of the scan by selecting Include Calibration Information. The filename and location are displayed in the dialog box but cannot be changed.

3. Click OK. The text file is created and can be used in other software such as Microsoft Excel.

Sharing Data 323

Importing and Converting Data

The Import Data command is available in the File menu in Data Analysis only. Use this command to import the following types of data files and convert them to data files that Pyris can use.

• ANF files

• PC Series files

• External Data

• X-Y Data

ANF Files

Use this command to convert an ANF file to a data file that Pyris can use. ANF files are the result of converting data files from Series 7 UNIX instruments as well as from other analyzers by using the data file conversion software provided with Pyris Software. When you select this command, the Convert ANF Data Files dialog box is displayed. Select the file to be converted. Click Open and the file is converted automatically. Pyris gives it the extension associated with the analyzer that collected the data and it is saved in the same directory as the ANF file. Retrieve the file using Add Data or Open Data in the File menu. For more information, see Converting ANF Files to Pyris data files.

PC Series

Use this command to convert a PC Series data file to a data file that Pyris can use. PC Series files are in ASCII format. When you select this command, the Convert PC Series Data Files dialog box is displayed. Select the file to be converted. [Available file types are DSC 7 Temp (.D7), DSC 7 Iso (.I7), DSC 7 SpHeat (.C7), TGA 7 (.G7), TMA 7 (.T7).] Click Open and conversion is performed automatically. The converted file has the Pyris extension associated with the instrument that collected the data, for example, dsd for a DSC 7 data file, and it is saved on the same directory as the PC Series file. Retrieve the file using Open Data or Add Data from the File menu. For more information, see PC Series Data File Conversion.

External Data

Use this command to convert external data files (created by certain non-Pyris instruments) to a data file that Pyris can use.

X-Y Data

Use this command to import a data file that is in ASCII format. The Import Data dialog box is displayed from which you select the .txt file you want to import. This command can be used to import a data file from another instrument whose file format is incompatible with Thermal Analysis analyzers' data file formats. If you can save the data file in .txt format then you can import it into Pyris Software.

NOTE: (1) The text file must consist of two tab-delimited columns. (2) The first item in each column is the data description for that column (for example, Heat Flow Endo Up, Specific Heat). This text will appear in the axis label. (3) The first column is the X-axis data and the second column is the Y-axis data.


Index

A

About Pyris ...................................... 6 Access to Pyris functions .................. 4 Accessories ................................... 36 Add a step button ........................ 294 Add Analyzer dialog box ................. 38 Administration Audit Trail ............... 21 Advanced Instrument Control key ..... 4 Always on top.................................. 6 Analyzers ........................... 36, 38, 69

adding ....................................... 38 calibrating ................................ 112 editing ....................................... 36 removing ................................... 36 status ...................................... 182

ANF files ..................................... 335 Apply Current Force button .......... 279 Apply Zero Force button ............... 279 ASCII files ................................... 335 Audit Trail Viewer .......................... 24 Auto Tension ............................... 230 Autohide ......................................... 6 Automatic save ........................ 29, 77 Auto-rescale .................................. 77 Autosampler Preferences Page ....... 80

B

Baseline File Section .................... 228 Baseline optimization ................... 114 Baseline subtraction ..................... 228

C

Calibrate ..................................... 112 Calibration ............................ 112, 170

Diamond DSC ........................... 170 DMA 8000 ................................ 166 DSC 4000 ................................ 141 DSC 6000 ................................ 138 Jade DSC ................................. 172 Pyris 1 DSC .............................. 175 Pyris 1 TGA .............................. 144 Pyris Diamond DSC ................... 170

STA 6000 ................................. 162 STA 8000 ................................. 158 TGA 4000 ................................ 146

Calibration files ............................ 332 print ........................................ 332

Calibration Jade DSC .................... 172 Cancelling Printing ....................... 331 Cascade .......................................... 6 Collapse All.................................. 301 Color Preferences Page .................. 76 Compliance ................................... 30 Configuration ........................... 36, 38

Diamond DSC ............................. 65 DMA 8000 .................................. 63 DSC 4000 .................................. 49 DSC 6000 .................................. 47 DSC 8000 .................................. 44 DSC 8500 .................................. 41 Jade DSC ................................... 67 Pyris 1 DSC ................................ 69 Pyris 1 TGA ................................ 51 STA 6000 ................................... 61 STA 8000 ................................... 59

Control panel Diamond DSC ........................... 282 DMA 8000 ................................ 279 DSC 4000 ................................ 265 DSC 6000 ................................ 263 DSC 8000 ................................ 258 DSC 8500 ................................ 253 Jade DSC ................................. 286 Pyris 1 DSC .............................. 284 Pyris 1 TGA .............................. 267 STA 6000 ................................. 277 STA 8000 ................................. 275

Convert ANF File .......................... 335 Convert PC Series File .................. 335 Cooling devices ............................ 108 Cover Open/Close button ...... 253, 258 Create Playlist ............................. 297 Creating a Template

Report Manager ....................... 326 Creating the Report ..................... 331

Index 327

Creep/Recovery Scan Step ............ 244 Curves ................................. 309, 310

changing slope ......................... 310 color ......................................... 76 display data of, in third-party software

............................................ 334 display in Data Analysis Application309 menus ...................................... 319 optimizing ................................ 310 rescaling .................................. 310 saving .......................... 29, 77, 322

Customizing Pyris .......................... 10

D

Data ............................................ 180 analyzing .................................. 308 monitoring ........................ 182, 288 saving ...................................... 322

Data Analysis ............................... 308 Data Analysis application .............. 308

how to open ............................. 309 Data Analysis button

on Pyris Manager ...................... 308 Data Analysis Curves .................... 319 Data Analysis window

Diamond DSC ........................... 214 display curves in ....................... 309 DMA 8000 ................................ 211 DSC 4000 ................................. 193 DSC 6000 ................................. 190 DSC 8000 ................................. 211 DSC 8500 ................................. 184 Jade DSC.................................. 217 Pyris 1 DSC .............................. 220 Pyris 1 TGA .............................. 196 TGA 4000 ................................. 199

Data collection ..................... 180, 288 Data Collection Section ................. 228 Data files ....................29, 32, 77, 332

default name ........................ 29, 77 display curves of ....................... 309 display in third-party software ... 334 save as .................................... 225

Data range ............................ 92, 108 Data sampling .............................. 228 Database Report ........................... 23 Default calibration values .............. 112

Default data file name .............. 29, 77 Default directory paths ............. 29, 77 Default instrument values . 71, 92, 108 Delete All .....................................301 Delete History ..............................301 Delete this step button .................294 Diamond DSC Preferences Page ....103 DMA 8000

calibration ................................166 configuration ............................. 63 control panel ............................279 instrument application ...............210 methods ................... 229, 239, 242 preferences ..............................100

DMA Reports ................................. 74 Dockable panels ..................... 10, 182 Dockable toolbars .......................... 10 DSC 8000

configuration ............................. 44 control panel ............................258 instrument application ...............186 preferences ............................... 86

DSC 8500 configuration ............................. 41 control panel ............................253 instrument application ...............183 preferences ............................... 83

E

Edit Creep/Recovery Step .............244 Edit Frequency Multiplex Step .......243 Edit Play List page ................ 294, 297 Edit Strain Multiplex Step ..............243 Edit Stress/Strain Step ..................244 Electronic Signatures ..................... 27 Emergency Repair Disk .................. 32 Enter Sample Info section .............224 Enter Sample Weight Section ........224 Equilibration constant ...................108 Expand All ...................................301 External data ...............................335 External Event Trigger

X10 ........................................... 74

F

File integrity .................................. 28 File name, increment


long ........................................... 32 File versioning ............................... 28 Fonts ............................................ 77 Frequency Multiplex Scan Step ..... 243 Frequency Scan Step ................... 242

G

General Preferences Page .............. 74 Getting started ...................... 2, 6, 36 Go To Temperature rate ........ 92, 108 Graph Preferences Page ................. 77 Groups .......................................... 16 GSA 7 ......................................... 245

I

Import command ......................... 335 Initial Temperature field ............... 227 Insert a step button ..................... 294 Instrument Application ................. 181

Diamond DSC ........................... 213 DMA 8000 ................................ 210 DSC 4000 ................................ 192 DSC 6000 ................................ 189 DSC 8000 ................................ 186 DSC 8500 ................................ 183 Jade DSC ................................. 216 Pyris 1 DSC .............................. 219 Pyris 1 TGA .............................. 195 STA 6000 ................................. 207 STA 8000 ................................. 204 TGA 4000 ................................ 198

Instrument communication ............. 32 Instrument Control key .................... 4 Instrument monitor ..................... 290 Instrument Page ............................ 71

Diamond DSC ........................... 103 DMA 8000 ................................ 100 DSC 4000 .................................. 90 DSC 6000 .................................. 88 DSC 8000 .................................. 86 DSC 8500 .................................. 83 Jade DSC ................................. 106 Pyris 1 DSC .............................. 108 Pyris 1 TGA ................................ 92 TGA 4000 .................................. 94

Instrument Preferences Page . 92, 108

J

Jade DSC calibration ................................ 172 configuration .............................. 67 control panel ............................ 286 instrument application .............. 216 preferences .............................. 106

L

Lag compensation ........................ 108 Line types ..................................... 74 Load temperature .................. 92, 108 Locking out users .......................... 19 Login history ................................. 22 Long file names ............................. 32

M

Math menu .................................. 318 Maximize All .................................... 6 Maximum temperature ................. 108 Menus ............................................. 9 Method ................................. 30, 320

Creep/Recovery ........................ 244 DMA Temperature Scan ............ 242 Frequency Scan ........................ 242 Isothermal Scan ....................... 242 Stress/Relax Scan ..................... 244 Stress/Strain Scan .................... 244

Method Actions and Events .......... 245 Method Editor .............................. 224 Method files ............................ 29, 77 Method steps

Creep/recovery......................... 244 DMA isothermal ........................ 243 Frequency multiplex ................. 243 Frequency scan ........................ 242 Stress/Relax ............................. 244 Stress/Strain scan..................... 244

Method used ........................ 299, 320 Minimize All ..................................... 6 Monitor ....................................... 288 More Detail ................................. 301

Index 329

O

Ordinate filter factor ..................... 108 Output File

Report Manager ........................ 326

P

Passwords .................................... 20 PC Series files .............................. 335 Permissions .................................. 16 Play list

create ...................................... 297 Play lists .................................. 29, 77

create ...................................... 297 edit .................................. 294, 297

Poisson's ratio .............................. 100 Preferences29, 71, 74, 76, 77, 79, 80, 92,

98, 99, 108 Diamond DSC Preferences Page . 103

Previewing the Report .................. 331 Print dialog box ............................ 332 Print Setup dialog box .................. 333 Printing the Report ....................... 331 Purge Gas Preferences Page .......... 80 Purge gases .................................. 69 Pyris 1 DSC ................................... 69

calibration ................................ 175 configuration ............................. 69 control panel ............................ 284 instrument application ............... 219 preferences .............................. 108 Pyris Player ...................... 220, 297

Pyris 1 TGA calibration ................................ 144 configuration ............................. 51 Control Panel ............................ 267 instrument application ............... 195 preferences ............................... 92

Pyris Configuration ............. 36, 38, 69 Pyris Manager ................................. 6 Pyris Player

play lists ........................... 294, 297 toolbars .................................... 293

Pyris Player Control Bar ................ 293 Pyris Player Edit Play List page ...... 294 Pyris Player Sample History Page .. 302 Pyris Player Setup Page ................ 293 Pyris Player View History Page ...... 301

Pyris Player View Play List page ....297 Pyris Player View Sample List page 299 Pyris software .................... 2, 6, 9, 10

R

Real-Time Curves Preferences Page 79 Remote Access Preferences Page ... 79 Remote Monitor ...........................290 Repair Disk Utility .......................... 32 Report Manager .... 325, 326, 327, 331 Rescale tools ................................310 Right click menus ............................ 6

S

Sample History page ....................302 Sample Info Page .........................224 Sample List ..................................299

view .........................................299 Sample rate .................................228 Samples .......................................180

analyzing ..................................180 Save Data As Section ....................225 Save Preferences Page ............. 29, 77 Set Force .....................................230 Set Initial Values Section ..............227 Set Length ...................................230 Setting up groups .......................... 16 Setup page, Pyris Player ...............293 STA 6000

calibration ................................162 configuration ............................. 61 control panel ............................277 instrument application ...............207 preferences ............................... 99

STA 8000 calibration ................................158 configuration ............................. 59 control panel ............................275 instrument application ...............204 preferences ............................... 98

Standard toolbar Pyris Player...............................293

Start Pyris button ............................ 6 Start Pyris Task menu ...................... 6 Static Force Control ......................230 Status Panel ............ 11, 182, 288, 290 Stop Run, in Remote Monitor ........291


System warning level ..................... 74

T

Taring and Weighing Samples on the TGA ........................................ 267, 270

Temperature go to ................................. 92, 108 initial ....................................... 227 load ................................... 92, 108

Temperature Events .................... 245 Temperature field ........................ 227 Temperature PID settings ............ 169 Temperature setpoint .................... 80 Templates

Report Manager ................ 326, 327 TGA 4000

calibration ................................ 146 configuration .............................. 53 control panel ............................ 270 instrument application .............. 198 preferences ................................ 94

Toolbars ................................ 10, 293 Tooltips ......................................... 74 Trigger External Event

X10 settings ............................... 74 Troubleshooting ............................ 32 TTS - Time-Temperature Superposition

............................................... 313

U

Uninstaller ....................................... 2

Update Flash EPROM ..................... 69 USB keys ......................................... 4 Users ............................................ 14

V

Valet ........................................... 304 Validate Method............................. 30 View History Page ........................ 301 View List Page ............................. 297 View methods .............................. 320 View results ................................. 320 View Sample List Page ................. 299

W

Weight calibration ........................ 145 Weight Calibration, TGA ........ 145, 147 Weight field ................................. 224

X

X10 ............................................... 74 X-Y data ...................................... 335

Y

Y Data range ................................. 92 Y Initial field ................................ 227

Z

Zero field .................................... 224 Zero Force................................... 279 Zero Weight ................................ 224

Index 331

Pyris Software Guide

Documents

Transcript of Pyris Software Guide