Installing and Understanding Your GC-AED ChemStation. Agilent GC-AED ChemStation

Transcription

1 Installing and Understanding Your GC-AED ChemStation Agilent GC-AED ChemStation

2 Copyright Agilent Technologies 2000 All Rights Reserved. Reproduction, adaptation, or translation without permission is prohibited, except as allowed under the copyright laws. Part No. G Replaces G First edition, JUN 2000 Printed in USA Microsoft is a U.S. registered trademark and Windows NT is a trademark of Microsoft Corporation. Agilent Technologies 2850 Centerville Road Wilmington, DE

3 Contents Part 1: Installation of the GC-AED ChemStation Chapter 1 Introduction GC-AED ChemStation overview... 5 Software installation overview... 5 What you need... 6 Software compatibility... 7 Documentation supplied... 8 Bundled packages also include:... 8 Contents of ChemStation CD-ROM... 9 Installation Qualification Utility... 9 ChemStation Software Status Bulletin... 9 ChemStation Revision History... 9 User-Contributed Library Chemical Analysis Group Supplemental Information Online help system Accessing online help Help searching utilities Logbook Chapter 2 Installing the Hardware Hardware installation overview Installing the GPIB interface board GPIB cabling Configuring the or GPIB board Chapter 3 Installing the Software Overview Installation procedures Configuring the 5890 GC Configuring the 6890 GC Installing the Control Charts reports Installing the AED Control Module software i

4 Contents Chapter 4 Validating and Starting the ChemStation ChemStation Installation Qualification Overview Installation Qualification ChemStation Installation Qualification utility execution ChemStation IQ utility results Generating an Installation Qualification reference file on a customized installation Starting the ChemStation Part 2: Understanding the GC-AED ChemStation Chapter 5 General Description General description GC-AED About the GC-AED ChemStation software Instrument control Data analysis Online help System suitability reports The GC-AED ChemStation directory structure Chapter 6 Methods Multiple injections Default method AED checkout method Checkout test for the 5921A AED Chapter 7 Selectivity and Sensitivity Interferences Improving sensitivity with matched filters Improving selectivity with background correction The recipe sum of all the improvements ii

5 Contents Chapter 8 Data Acquisition Data files Online monitors Online signal monitor Online spectra monitor Chapter 9 Data Analysis Data analysis Back Amount Spectral displays Select spectrum Select peak apex spectrum Select average spectrum Select range of spectra Select peak spectra Select reference spectrum 1 and Isoabsorbance plot Spectra preferences Isoplot preferences D Plot AED-CIC Appendix Startup Problems and Causes Software startup problems and possible causes Agilent Response Center Support Services resolves problems and maximizes performance Calling the Agilent Analytical Response Center Computer hardware checklist Computer configuration checklist iii

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7 Part 1: Installation of the GC-AED ChemStation

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9 1 Introduction

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11 Introduction GC-AED ChemStation overview GC-AED ChemStation overview The ChemStation can fully control and automate many features of the GC and other instruments including an extensive range of sampler, column, and detector options. One of these detector options is the AED. The ChemStation and AED control module run in tandem with the GC instrument to acquire, process, and report chromatography data. The functions of these modules are: ChemStation Core General data analysis and reporting functions, common to all instruments and detectors. GC Instrument control for 5890 or 6890 gas chromatographs. AED Control, data acquisition, and data analysis functions that are specific to the atomic emission detector. Monitor ChemStation CD-ROM AED Software Module CD-ROM Keyboard Mouse Software installation overview Read chapter 1 for an overview of the GC-AED ChemStation software and documentation. Chapter 2 explains how to set up your hardware and software drivers for your PC. In chapter 3, the installation of the GC-AED ChemStation is explained. Chapter 4 describes how to validate and start your newly installed ChemStation. 5

12 Introduction What you need What you need The minimum software and hardware requirements your system needs to run the ChemStation software are: Microsoft Windows NT 4.0, updated with Microsoft s Service Pack 6 (SP6). Personal computer with an Intel Pentium processor (166 MHz or greater). 48 MB RAM minimum. 3.5 inch floppy disk drive. Agilent 82341C/82341D/82350A GPIB interface card. 1.2 GB hard disk drive. Super VGA or ultra VGA monitor and interface. The screen resolution must be at least to take advantage of the ChemStation graphical user interface. CD-ROM driv e. Windows-supported mouse or other pointing device. Windows-supported printer. GPIB cables that are two meters long or less. A Pentium II 400 mhz PC with 128 MB RAM is recommended. This booklet assumes that you are familiar with Microsoft Windows NT. It is essential that you are comfortable using Windows before attempting to use the ChemStation. 6

13 Introduction Software compatibility Software compatibility GC data acquired on previous versions of the ChemStation can be processed with the new version. Sequences developed for GCs on previous Agilent 3365 versions of the ChemStation will run on the new version for the purposes of reprocessing only. GC Methods developed on previous 3365 versions of ChemStation can be converted to run on the new version provided that they don't include macros, and that both the previously developed and converted methods are for the same instrument model (for example, a 5890 GC). Macros written on previous 3365 versions of the ChemStation will need to be rewritten to run on the new version. Pre and post run programs may need to be modified or rewritten. Screen saver software should not be used with the ChemStation. Screen savers can cause undue loading on the CPU that may result in the loss of data from the GC during high data collection periods. Methods, sequences, and macros created on a Pascal AED workstation cannot be converted for use with the GC-AED ChemStation. Data files collected with a Pascal AED workstation can be converted for use with the GC-AED ChemStation by a user-contributed program, which is included on your ChemStation s CD-ROM. 7

14 Introduction Documentation supplied Documentation supplied Section 1 of this handbook describes how to prepare your ChemStation for operation by installing the necessary hardware and software. The Understanding Your Agilent ChemStation handbook provides a discussion of ChemStation concepts to increase your understanding of how the ChemStation works. Section 2 of this handbook describes those features of the AED that are not covered in the Understanding Your Agilent ChemStation handbook. An online Macro Programming guide describes how to work with the powerful command set to customize and expand the capabilities of your ChemStation. Select Commands from the Help menu to access this online guide. A README file contains information on items such as added new features, known work-arounds, and corrections that could not be included in this manual at the time of printing. To access the readme.txt file from the Start menu in the Task Bar, select Programs/ChemStations/readme.txt. Bundled packages also include: Microsoft Windows NT online help and handbooks. Hardware handbooks for each instrument, including the PC. 8

15 Introduction Contents of ChemStation CD-ROM Contents of ChemStation CD-ROM This CD-ROM contains the executable files, utilities, and documentation for the ChemStation. In order to install the ChemStation, you must supply a valid license registration number. The license registration number is included with the original product and is your proof of license. The AED software module CD-ROM contains the software needed to operate the AED with the ChemStation. A license registration number is also included with the AED software module. Installation Qualification Utility The ChemStation comes with a utility that qualifies and documents the completeness and integrity of a new installation. The Installation Qualification Utility is installed automatically on the hard drive during software installation. ChemStation Software Status Bulletin The Software Status Bulletin is a document reflecting the results of Agilent Technologies defect logging, tracking, and repair methodology by publishing the current status of ChemStation application software products (known defects, available fixes, and additional information). The SSB is located in the Support\SSB directory of the HP ChemStation CD-ROM. If you have a software contract, you will receive the HP ChemStation Software Status Bulletin on a regular basis. ChemStation Revision History The Revision History is targeted towards users who may have to consider revalidating their analytical data system after upgrading to a new revision of the 9

16 Introduction Contents of ChemStation CD-ROM application software. The Revision History contains the revision history of all products that are part of the ChemStation product family. The history files are located in the Support\History directory of the ChemStation CD-ROM. User-Contributed Library The contents of this library are intended to help users develop and customize the installations for their specific needs to get the most out of their investment. The content of the library comes from both Agilent internal and user-contributed sources. Each contribution is checked for functionality but does not necessarily go through the same level of formal testing procedures as the actual product. Therefore, Agilent Technologies does not guarantee the correctness of the contributions. The User-Contributed Library comprises utilities and macros. Each contribution is delivered with a specific README.TXT file which can be viewed using any ASCII text editor. The UCL is located in the \UCL directory of the ChemStation CD-ROM. Chemical Analysis Group Supplemental Information The Chemical Analysis Group Supplemental Information contains additional media, graphics drivers, and printer drivers for bundled packages shipped after the ChemStation software release. Please refer to the documentation supplied with the CAG Supplemental Information for further details on the specific drivers and how to install them. The Chemical Analysis Group Supplemental Information is available with the ChemStation Vectra bundle on flexible disk. 10

17 Introduction Online help system Online help system An extensive online help system provides reference material, step-by-step instructions, and a completely cross-referenced commands set for your ChemStation. There are two ways to access help and three searching utilities in the Help system. Accessing online help Click the Help button in any dialog box (or press the <F1> key) to access context-sensitive reference material. Online reference material explains what each ChemStation function does and defines the entries necessary to accomplish it. Select Help from the main menu to access Help Topics, Commands, and Tutorial. 11

18 Introduction Online help system Select Help Topics from the Help menu to display a list of categories for the ChemStation system. Click the appropriate category, then click the topic you want to view. For your information, a description of new features is available when you start the program for the first time. See page 53. These topics provide online step-by-step instructions and instrument specific help. Online step-by-step instructions include the most frequently performed ChemStation tasks, such as how to Run a Method, Integrate a Data File, Annotate a Chromatogram, Generate a Report, and more. The instrument specific help provides help for each instrument. This information can be printed from the online help screens. Select Commands from the Help menu to display command categories for your ChemStation and the online Macro Programming guide. Click the appropriate category, then click the command you want to view. The commands online help includes extensive information for each command, such as the name, group, syntax, parameters, discussion, return value, and 12

19 Introduction Online help system examples (where possible). The Macro Programming guide describes how to work with the command set to customize your ChemStation. To access the tutorial, select Tutorial from the Help menu. A list of available tasks for the current ChemStation View is displayed. An integrated tutorial is provided as part of your ChemStation software. This self-paced, hands-on introduction will help you learn how to use selected features. If you are a new user, start by going through this training. The Tutorial guides you through each task with step-by-step instructions that you may either choose to perform yourself by selecting the Start Task button, or have a list of steps provided by selecting the Show Me button. If you select the Show Me button, the ChemStation performs the first step for you and provides you with a list of additional steps to complete the task. You can use these step-by-step instructions on your own data files, methods, and sequences, or on the sample files specified in the help text. 13

20 Introduction Online help system Help searching utilities There are three searching utilities in the Help system: Contents lists help topics by category. Click Contents and follow the system prompts. Index lists all help topics alphabetically. Click Index and follow the system prompts. Find enables you to perform a full text search for on specific words or phrases. The first time you use the find utility, Windows will create a database of all the words in your help system. To create the database, click Find and follow the system prompts. Once the database is created, you will need to perform this process again. To perform full text searches, click Find and follow the system prompts. Logbook An automatically updated Logbook contains any error conditions discovered during operation and corrective actions (if required). To access, choose Logbook from the View menu, then double-click the entries. The most recent entries are at the top of the list. 14

21 2 Installing the Hardware

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23 Installing the Hardware Hardware installation overview Hardware installation overview The hardware for your AED-GC system must be installed before installing the ChemStation software. Your gas chromatograph, AED module, PC and printer are supplied with documentation explaining their installation. This chapter describes: Installation of the or GPIB board into the ChemStation s PC. Installation of the GPIB board Windows NT drivers. Attachment of cables between the ChemStation s PC, the GC and the AED. If you purchased a bundled package that included a PC from Agilent Technologies, your GPIB interface boards and GC-AED ChemStation software are factory installed in your PC. See the sections on configuring your GC and AED software module in the next chapter if you need to change your configuration. 17

24 Installing the Hardware Installing the GPIB interface board Installing the GPIB interface board Since the GPIB or the 82341C GPIB boards can be installed in several different computers, the following instructions are general. If you have difficulty during the installation, consult your computer manual or dealer. The GPIB board: This board requires a free (E)ISA slot in your PC. This board requires the user to install the Standard Interface Control Library (SICL) after installation of the board. See Configuring the GPIB board upon completion of GPIB cabling. Because this board has partial plug-and-play capabilities, it is not necessary to set the switches. The PCI High-Performance GPIB Interface Card: This board requires a free PCI slot in your PC. To install it, follow the instructions provided with the board or the instructions for installing an board below. Place the board in any free PCI slot. After installation, install the I/O Libraries and configure the board as described later. WARNING Disconnect your computer and all attached electrical devices before removing any covers. Be sure to wear the antistatic strap when installing the boards. 1. Turn off and unplug your computer, then remove the computer s cover(s). 2. Select any empty slot; however, it is best not to place the GPIB board next to a video board. 3. Write down the slot number you will use and store it for later use. (Some EISA computers require slot number and board type information after installation. For computers that require this information, refer to the appropriate installation documentation.) 4. Loosen the mounting screw and remove the selected empty slot s rear plate. 5. Holding the board by its edges, insert the board into its slot. Make certain that the board s edge connector is fully seated. Lock the board into place with the mounting screw. 18

25 Installing the Hardware GPIB cabling 6. Replace the computer s cover(s). Plug in, and restart the computer. GPIB cabling When connecting GPIB devices together, there are several basic rules that should be observed. 1. Turn off and unplug the computer and all attached devices before the GPIB cables are installed. 2. Before connecting any analytical instrument to an GPIB cable, consult the documentation supplied with each device and determine its GPIB address. No two devices connected to the ChemStation may have the same address. Alter their addresses as necessary to avoid any duplication. Write down each GPIB address. This information will be needed later. 3. Where possible, use GPIB cables that are two meters long or less. GPIB cable (0.5 m) (10833D) GPIB cable (1.0 m) (10833A) GPIB cable (2.0 m) (10833B) GPIB cable (4.0 m) (10833C) The ChemStation does not support GPIB extenders. 4. Attach one end of an GPIB cable to the computer s GPIB connector. Properly tighten all GPIB connectors. A poor connection causes errors which are difficult to diagnose. 5. Connect GPIB devices in a chain. A chain occurs when an GPIB device is connected to the next GPIB device, and it is, in turn, connected to the next, and so on. Try to avoid star configurations (connecting all of the devices to a central point). 19

26 Installing the Hardware GPIB cabling See the following examples. Sampler control GPIB cable Tray cable Tray Tower cable Tower 5890 GC GPIB cable Remote start cable G2350A AED GPIB cable Computer Printer Parallel cable Remote start cable 5890 Series GC 20

27 Installing the Hardware GPIB cabling Sampler control Tray Tower cable RS-232 cable Remote start cable GPIB cable Tower GPIB cable Tray 6890 GC Remote start cable G2350A AED Computer Printer Parallel cable 6890 GC Tray GPIB cable Tray Tower Tower GPIB cable Remote start cable Computer Parallel cable 6890 GC G2350A AED Printer 6890 Plus GC 21

28 Installing the Hardware Configuring the or GPIB board Configuring the or GPIB board After installing the GPIB board in the computer, it is necessary to install the SICL to complete the communication link from your GC to your ChemStation. 1. Start Windows and insert the ChemStation CD-ROM into the CD-ROM drive. 2. From the Start menu in the Task Bar, select Start/Run. 3. At the command line, type drive:\gpib\hpiolibs, then click OK. 4. The I/O Libraries InstallShield self-extracting EXE screen appears. To continue the installation, click Yes. 22

29 Installing the Hardware Configuring the or GPIB board 5. Once the InstallShield extracts the I/O Libraries, the following screen appears. If other Windows programs are in use, you will be prompted to close them. To continue the I/O Libraries setup program, click Next. To quit the Setup, select Cancel. 6. Once you have chosen to continue, the following screen appears. Make sure the checkbox is clear, as shown. Click Next. 23

30 Installing the Hardware Configuring the or GPIB board 7. Next, the Select Destination Directories screen appears. To remain with the default directories, click Next. To select a different directory, edit the SICL and Visa fields, and click Next. 8. The Ready To Start Copying Files screen appears. To confirm your settings and copy the I/O Libraries to your PC, click Next. 24

31 Installing the Hardware Configuring the or GPIB board 9. After installing the or GPIB board and I/O Libraries software, you must configure your interfaces before you can use the I/O Libraries. The I/O Libraries Setup program automatically sends you to the View Readme and Configure interfaces screen, shown below. To configure an or GPIB board, click Next. If you later require access to the I/O Libraries configuration utility from outside of the Setup program, you can select it from the Windows Start menu. 25

32 Installing the Hardware Configuring the or GPIB board 10. You will be asked if you would like to configure your interfaces automatically or manually. Select Configure interfaces manually. Click Next. 11. From the Available Interface Types list, select the GPIB board installed, and click Configure to continue. 26

33 Installing the Hardware Configuring the or GPIB board The configuration utility detects the selected GPIB board and assigns the correct resources to the board. 12. After completing the Interface Configuration Application for your GPIB board, the board configuration screen appears. 13. Enter the settings shown below. a. For both the and GPIB boards, set the SICL Interface Name to hp82341 (hp must be lowercase). b. Set the Bus Address to 30. c. Click System Controller GPIB GPIB 27

34 Installing the Hardware Configuring the or GPIB board 14. Click OK to continue. The Interface Configuration Application screen should now reflect the correct settings for the or GPIB board GPIB GPIB To complete the procedure and exit the Setup program, click OK. Note Even if you installed an GPIB board, the SICL name is "hp82341". 28

35 3 Installing the Software

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37 Installing the Software Overview Overview This chapter explains how to: Install the ChemStation and GC instrument software as a dedicated system or as a Client/Server on a network Configure the ChemStations GC Instrument Install and configure the AED control module software Installation procedures You must install a GPIB board in your computer before installing the ChemStation software. The software drivers for this board must be installed and running under Windows NT. See chapter 2 for these procedures. If you are upgrading from the 3365 ChemStation, back up your data and method files and then remove the existing ChemStation software from your PC before running this installation. You must also remove the [PCS] section from your Win.ini file if another ChemStation was previously installed on your PC. If you do not know about the Microsoft Windows Win.ini file and how it is sectioned, please contact Agilent Technologies for assistance. Use the following procedure to install or upgrade the ChemStation. Installing a bundled package If you purchased a bundled package from Agilent Technologies, your GPIB interface board, instrument module, and ChemStation are already installed. Go directly to Configuring the 5890 GC on page 36 or Configuring the 6890 GC on page 38 to configure your new ChemStation. 31

38 Installing the Software Installation procedures Initial installation and upgrade 1. Start Windows. 2. Insert the ChemStation CD-ROM into the CD-ROM drive. 3. From the Start menu in the Task Bar, select Start/Run. 4. At the command line, type drive:\setup (e.g., D:\Setup), then click OK. Select the drive where your CD-ROM resides. 5. If you are performing an initial installation, skip to step 7. If you are upgrading existing ChemStation software, after a few seconds the Setup program will display the following prompt. Click Yes to have the Setup program update the ChemStation software on your PC. 32

39 Installing the Software Installation procedures 6. After your upgrade is complete, the Setup program prompts you to add any new instrument control modules. To complete the installation procedure and exit the Setup program Click No and skip to step 11. You may use the Configuration Editor at a later time to complete the instrument configuration. 7. To install your ChemStation on a different drive, change the default drive letter in the ChemStation directory field. It is recommended that you use \HPChem for the installation directory on this drive. Select instrument number 1 and click Add/Change. 33

40 Installing the Software Installation procedures 8. Select the G2070AA GC ChemStation from the list in the Available Products box and click Add. 9. Enter the License Registration Number for the selected module in the New License Number field and click Add. The applicable license numbers are printed on your Software Certificate and Registration Packet. 34

41 Installing the Software Installation procedures 10. Click OK return to the previous screen. The following screen appears: 11. Complete the setup process of the ChemStation by clicking Install. 12. If you are performing an initial installation, the Setup program installs your ChemStation and instruments, then displays an information dialog box reminding you to exit Windows and reboot your system before starting your ChemStation (click OK). The program will automatically send you to the Configuration Editor. If you are upgrading your ChemStation, the Setup program upgrades your ChemStation and instrument software, then prompts you to configure your instruments. To access the Configuration Editor and configure your ChemStation and instruments, click Yes. 35

42 Installing the Software Configuring the 5890 GC Configuring the 5890 GC This section explains how to configure the ChemStation when attached to a 5890 GC. If your installation is for a 6890 GC, skip to the next section. 1. At the Configuration Editor s opening screen, highlight the title bar of the Instrument 1 box and select Configure/Instruments. 2. Select the 5890 GC instrument. 3. Accept the instrument name, or type a new one in the Instrument Name field. 36

43 Installing the Software Configuring the 5890 GC 4. Select the Initial Screen Window Size. Normal fills most of the screen Minimized is an Icon Full screen fills the entire screen. 5. To accept the setting and display the Device Configuration dialog box, click OK. 6. Select a GPIB address. The GC controlled by your ChemStation must have a unique GPIB address. If you are unsure of how to obtain this address, refer to your 5890 GC instrument s manual. If you change the GPIB address shown here in order to prevent duplication, complete this configuration, then turn the instrument off and reboot your system so the change goes into effect. 7. To configure your 5890 GC with a sampler, select the sampler from the Options group box. Select a GPIB address for this sampler and click Add. 8. Press OK to return to the Select Instrument dialog box. Skip to step 8 in the next section titled Installing the AED Control Module software. 37

44 Installing the Software Configuring the 6890 GC Configuring the 6890 GC 1. At the Configuration Editor s opening screen, highlight the title bar of the Instrument 1 box and select Configure/Instruments. 2. Select the 6890 GC instrument. 3. Accept the instrument name, or type a new one in the Instrument Name field. 38

45 Installing the Software Configuring the 6890 GC 4. Select the Initial Screen Window Size. Normal fills most of the screen Minimized is an Icon Full screen fills the entire screen. 5. To accept the setting and display the Device Configuration dialog box, click OK. 6. Configure the GC s interface card. GPIB based instrument Select GPIB as the interface type and then select a GPIB address. Each instrument controlled by your ChemStation must have a unique GPIB address. If you are unsure of how to obtain this address, refer to your 6890 GC instrument s manual. If you change the GPIB address shown here in order to prevent duplication, complete this configuration, then turn the instrument off and reboot your system so the change goes into effect. 7. Return to the Select Instrument dialog box by clicking Ok. 8. To exit the Select Instrument dialog box and return to the Agilent Configuration Editor main menu, click OK. 9. Select File/Save from the Configuration Editor s menu. File Save Print Exit 10. Select File/Exit to return to Windows. 39

46 Installing the Software Installing the Control Charts reports 11. Exit Windows and reboot your system before starting the ChemStation so the changes go into effect. Remember: If you changed the 5890/6890 instrument s GPIB address in step 6, then turn the GC off and on again so that the change goes into effect. Store your CD-ROM and license numbers in a safe place. These will be required if you have to reinstall your software or for future upgrades. Installing the Control Charts reports In order to use this feature you must have Microsoft Excel 97 installed. After you have installed your ChemStation and rebooted your PC system, you are ready to install the ChemStation Control Charts feature. 1. Start the ChemStation. 2. At the ChemStation command line, type MACRO STARTCHT.MAC, GO then press Enter. 3. A dialog box providing information about the installation appears. 4. Select Help from this dialog box for information about using Control Charts with your ChemStation. 5. Select OK to install Control Chart feature to your ChemStation. This process adds "Control Charts" to your reports menu. Installing the AED Control Module software 1. Insert the AED Control Module CD-ROM in your CD-ROM drive. 2. From the Windows NT Start menu, select Start/Run. 3. At the command line, enter drive:\setup (e.g., E:\Setup). After a time (minutes) during which the AED software is installed, the following License Registration screen will appear. 40

47 Installing the Software Installing the AED Control Module software 4. Enter the license number of your AED module, click Add, and then OK. The system displays a GC Module prompt asking if you want to run the Agilent Configuration Editor to set up your instruments. 5. To access the Configuration Editor, click Yes. 6. Highlight the title bar of the Instrument 1 box and select Configure/ Instrument from the Configuration Editor s menu. This displays the Select Instrument dialog box. 41

48 Installing the Software Installing the AED Control Module software 7. Select the 5890 GC or 6890 GC instrument option depending on which GC model you are using. 8. Select the 5921 AED or the G2350A AED in the Options group box, and enter the AED instrument s GPIB address. The default value is 15. To process your selection, click ADD, then click OK. 9. Select File/Save to save the new instrument configuration(s). File Save Print Exit 10. Select File/Exit to return to Windows. 11. Exit Windows and reboot your system before starting the ChemStation so the changes go into effect. If you changed the AED instrument s GPIB address, power the AED off and on again so that the change goes into effect. 42

49 Installing the Software Installing the AED Control Module software Store your CD-ROM and license numbers in a safe place. These will be required if you have to reinstall your software or for future upgrades. 43

50 Installing the Software Installing the AED Control Module software 44

51 4 Validating and Starting the ChemStation

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53 Validating and Starting the ChemStation ChemStation Installation Qualification ChemStation Installation Qualification Overview After installing the ChemStation system software on your computer and configuring the instruments, you may evaluate the correctness, and completeness of the installation and verify that the analytical system is fully operational. Installation Qualification The ChemStation Installation Qualification utility uses factory delivered installation reference files to verify the existence, correctness, and integrity of the required ChemStation system files (executable program files, binary register files, macro files, initialization files, help files, and customized report templates). This process is called Installation Qualification (IQ). File integrity is verified by comparing the installed file with the original file recorded on Agilent s installation master. The file details of the installation master are delivered on so-called reference files. Modified or corrupted files are detected by the IQ utility. The integrity of the reference files themselves is also tracked. In case the installation qualification utility is supplied with a reference file that was modified after its generation, this will be flagged in the report under the optional qualification section marked invalid reference files. In addition, the IQ utility checks the version code of the ChemStation executable system files (*.EXE, *.DLL). The appropriate ChemStation IQ icon is added to your ChemStation drop box. 47

54 Validating and Starting the ChemStation ChemStation Installation Qualification ChemStation Installation Qualification utility execution The calculations for all ChemStation system files may take several minutes. A dialog box indicates the name of the system file that is currently being analyzed. ChemStation IQ utility results The ChemStation Installation Qualification utility displays the qualification results on the screen and can optionally generate a report of its findings. On a complete and consistent installation, the installation qualification runs without any error messages and no files are reported missing or modified. If the qualification report lists files as missing or modified, the installation qualification utility displays the error message Installation Qualification completed with error(s) in the message line. 48

55 Validating and Starting the ChemStation ChemStation Installation Qualification The ChemStation Installation Qualification reports the following file categories: File Categories reported by ChemStation Installation Qualifications File Category Explanation Required Action Identical files Required files exist and passed the version and integrity check. No action required. Missing files Modified files Invalid reference file Files are missing that are required to run the ChemStation. Files have been corrupted or modified. The original reference file is corrupt or has been modified after creation. Reinstall the ChemStation. Reinstall unless you have intentionally customized or updated ChemStation files, then generate a new installation qualification reference file for customized or updated ChemStation installations. Reinstall the original reference file. 49

56 Validating and Starting the ChemStation ChemStation Installation Qualification The printed report contains the license registration numbers used on the system that was checked. It also lists the reference files (name and date code) that were used for the installation qualification. Example report: 50

57 Validating and Starting the ChemStation ChemStation Installation Qualification Generating an Installation Qualification reference file on a customized installation The ChemStation has an open system that allows knowledgeable users to add their own customizing code. In regulated environments, such adaptations, additions, or modifications are generally documented. For your own tracking purposes, you can use the ChemStation Installation Qualification utility to generate a reference file listing for the customized system. You can use this reference file to qualify the completeness and integrity of the customized ChemStation and use it as a tracking document for future modifications. The program scans for files with the extensions *.dlc, *.dll, *.drv, *.enu, *.exe, *.hlp, *.ini, *.mac, *.mcx. For example, in order to create the file contents list along with the corresponding file checksums for your existing installation: Check your GC ChemStation installation before running this reference file. From the Windows Start menu, select Run. Execute the Agilent Installation Qualification utility with the following command line options: C:\HPCHEM\SYS\HPVERI00.EXE -a -f sys\*.ref -n. core sys ce gc lc ms drivers language helpenu Add the resulting reference file to your project documentation. To automatically run an installation qualification test using the new reference file, set up an icon with the following command line specification in its properties: C:\HPCHEM\SYS\HPVERI00.EXE -a -r sys\*.ref -n. core sys ce gc lc ms drivers language helpenu For a complete description of the command line syntax of the Installation Qualification utility, refer to its help file (C:\HPCHEM\SYS\HPVERI.HLP). See the Installation Qualification help system for a complete description of the Installation Qualification utility s command line options. The Installation Qualification does not check method files, sequence files, or data files. These 51

58 Validating and Starting the ChemStation Starting the ChemStation files are stored in Agilent Technologies proprietary, unalterable binary formats and are checked for integrity when loaded into the ChemStation. Starting the ChemStation After installing and configuring the ChemStation software, and rebooting your system, you may start an online instrument session of the ChemStation. 1. From the Start menu in the Task Bar, select Start/Programs/ ChemStations/ and select the appropriate instrument. 52

59 Validating and Starting the ChemStation Starting the ChemStation The opening screen you will see is similar to the one shown below. Look in What s New for an overview of new features with this revision of the ChemStation. Choose Tutorial to start a self-paced, hands-on introduction to the ChemStation. Deselect the Show on Start box if you do not want the Welcome dialog box to be displayed when the ChemStation starts up in the future. 2. Click the door in the Welcome box to enter the ChemStation. 53

60 Validating and Starting the ChemStation Starting the ChemStation 54

61 Part 2: Understanding the GC-AED ChemStation

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63 5 General Description

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65 General Description General description General description GC-AED This part of the manual describes the concepts behind the GC-AED module of the ChemStation. It complements the information in the Understanding Your ChemStation manual by providing concepts applicable to the GC-AED ChemStation. The GC-AED ChemStation is an instrument control, data acquisition, and data evaluation system for the G2350A or 5921A atomic emission detector used in conjunction with either the 6890 or 5890 gas chromatograph. The software runs on a personal computer with a PCI, ISA or EISA interface bus, and uses a Microsoft Windows NT 4.0 operating environment. The software is sold as a single instrument ChemStation in this version (product number G2360AA), including data acquisition, instrument control, data analysis (integration, quantification, and reporting), automation and customization for one GC AED instrument. An instrument is defined as one GC system running on a single timebase, but can collect data from up to two other standard GC detectors mounted on the same GC simultaneously. The G2368AA AED Data Analysis Only (DAO) Software License allows the use of G2360AA software on a maximum of one additional PC (which is in addition to the PC already used for GC AED operation). This additional PC would be used for AED chromatograms and spectral data evaluation only. The license cannot be used for data acquisition or control, nor can it be upgraded to perform these functions. To perform AED data analysis on additional PC s, you must purchase one G2368AA AED DAO software license for each additional PC. 59

66 General Description About the GC-AED ChemStation software About the GC-AED ChemStation software The ChemStation software runs under Microsoft Windows NT 4.0 with service pack 6 (SP6). Instrument control The instrument control capability of the GC-AED ChemStation is limited to one GC AED system. Data analysis The AED software saves two chromatograms for each element selected. One contains data for the element plus considerable background from other sources. The other contains only the background. The two signals are subtracted to eliminate the background before integration. The amount of background removal is controlled by the Back Amount parameter. It is discussed in detail in chapter 5. Online help A context sensitive, indexed help system is built into the software to provide software reference information. An Analytical Tasks section of the online help provides brief step-by-step summaries of the most frequently used ChemStation tasks. Macros for the ChemStation are described in the online help. System suitability reports System suitability reports enable users to report system performance parameters for individual analysis. 60

67 General Description The GC-AED ChemStation directory structure The GC-AED ChemStation directory structure The directory structure of the GC AED ChemStation consists of generic directories that are shared by all configured instruments and instrument specific directories. The software installation program creates a subdirectory in the ChemStation directory (by default HPCHEM) for each configured instrument, identified by the instrument number. This subdirectory contains all data, methods and sequences for the particular instrument. HPCHEM 1 (see text) DATA DEMO CKO5921 CKO2350 Backup Methods Sequence Temp Verify Core Drivers GC Language Repstyle SYS Helpenu Language Pictures Helpful Language Aeddata Sampapps Helpful Language G Shell.APP Slice.APP 61

68 General Description The GC-AED ChemStation directory structure HPCHEM Contains the programs to configure and start the ChemStation software. It must be part of the PATH variable. This directory is added automatically by the installation program unless you supply an alternative. 1 Used for the configured instrument. This subdirectory contains subdirectories DATA, METHODS, SEQUENCE, TEMP, and VERIFY. DATA Contains the result directories of your analyses. It may contain more subdirectories if you structure the disk with subdirectories by defining them in the Sample Information or Sequence Parameters dialog boxes as you work. Result directory names have a.d extension. DEMOContains some typical result directories. CKO5921A Example data files for Chemical Performance Checkout of the 5921A detector. CKO2350 Example data files for Chemical Performance Checkout of the G2350A detector. METHODS Contains all method directories. Names have a.m extension. SEQUENCE Contains sequence tables. The file names have a.s extension. TEMP Contains temporary work files and the logbook files. For example, for Instrument 1 the online logbook is called INSTR1.LOG and the offline logbook is called INSTRI 2.LOG. VERIFY Contains data files, methods, and the results of data processing stored in register (.REG) files. These files execute the ChemStation verification procedure described in the Online Help. One set of data, method, and register files is used for each verification test. BACKUP Used for backup copies of old files during installation. CORE The core components of the software shared by all chromatographic instrument configurations. This is the ChemStation working directory. HELPENU US English text of the help files for the core software. LANGUAGE Used for programming language specific core software parts. PICTURES Graphics used by the ChemStation. DRIVERS Drivers for the configured instruments. HELPENU US English text of the help files for configured instruments. LANGUAGE Used for programming language specific driver software parts. GC Instrument driver specific code such as INI files. AEDDATA AED specific files. G2350 Recipe files for the G2350A AED Recipe files for the 5921A AED. SAMPAPPS Contains sample application files. SHELL.APP A Visual BASIC program used to send and read data from a ChemStation and to send commands to a ChemStation. SLICE.APP A Visual BASIC program used to transfer AED data to a ChemStation in Microsoft Excel spreadsheet format. LANGUAGE Contains the language specific code of this part of the software. REPSTYLE Used for report templates defined using the report designer. SYS Contains generic components shared by all chromatographic instrument configurations. \hpchem\sys must be part of your PATH variable. By default the installation programs adds it for you. 62

69 6 Methods

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71 Methods Multiple injections Multiple injections Different elements require different conditions, particularly the choice of reagent gases, for satisfactory detection. If two or more elements are chosen that require the same conditions, the AED can measure them all using a single sample injection. However, if the conditions differ, multiple sample injections will be needed, one for each distinct set of conditions. An AED method can set up and run multiple injections by repeating the Injection and Data Collection processes as many times as needed. Note that this is different from a non-aed method, and is not the same as running multiple samples with a sequence. ChemStation status First sample Last sample Post-run macro Evaluate data Collect data Repeat as needed for multiple elements Inject sample Pre-run macro Load method Start sequence Data file closed End of sequence Time 65

72 Methods Default method A method is identified by a name of up to eight alphanumeric characters, with a.m extension to identify it as a method. Methods are stored as MS DOS directories that contain individual files relating to the components of the method. Method Part Method Information Instrument Control Data Analysis Sequence Recalibration Run Time Checklist Function Descriptive information about the method. Parameters that control the instrument or its components. Example: For a GC, includes parameters such as inlet temperature, inlet pressure, packed column flow setting, etc. Parameters that control the data processing, calibration, and reporting. Recalibration frequency and other parameters. Parts of the method that will be executed. Default method When the GC-AED ChemStation is started for the first time, the default AED method supplied by Agilent Technologies is loaded. A copy of the default method is placed in memory and becomes the current method. You can load a different method at this point and it will become the current method. Caution Do not delete the default method (DEF_AED.M). It is used as a template to create new methods. AED checkout method An automated chemical performance test can be run using the sequence CKO_TST.S (select Load Sequence within the Sequence parameters). 66

73 Methods Checkout test for the 5921A AED Checkout test for the 5921A AED This procedure tests the chemical performance of the GC-AED System. 1. Install the AED checkout column (25 m 0.32 mm id 0.17 mm film thickness, HP-1, part number 19091Z-012) in the split/splitless inlet of the GC and connect the outlet to the AED. Set the split vent flow to 100 ± 5 ml/min and the column inlet pressure to 20 psi. Heat the column at 200 C for 30 minutes to clean it out. 2. Place a vial of AED Checkout Sample #1 (part number ) in position 1 of the autoinjector (or tray) and a vial of AED Checkout Sample #2 (part number ) in position Run the method CKO_TIME.M. This method will print a report showing chromatograms for carbon, sulfur, and nitrogen. For the performance calculations to work correctly, the retention time of the t butyldisulfide must be between and minutes. If the retention time of the peak is in the correct range, the message Retention time of sulfur peak OK is printed. 4. If the retention time is outside the required window, the message Suggested pressure change (psi) = X.XX is printed, where X.XX is the amount by which the column inlet pressure should be changed to bring the peak into the window. If necessary, change the pressure and run CKO_TIME.M again to confirm that the retention time is correct. 5. Load and run the sequence CKO_TST.S. This requires about 1 hour. When finished, a report is printed showing the detection limit, noise, selectivity, and back amount for each of the test elements. 6. At the end of the sequence, you will be asked if you want to save the measured back amounts for the tested elements. If the test results look acceptable, we recommend that they be saved. If there is any doubt about the results, click Cancel to finish. 67

74 Methods Checkout test for the 5921A AED 68

75 7 Selectivity and Sensitivity

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77 Selectivity and Sensitivity Figure 1 is a typical chromatogram from the AED. Many compounds are detected simultaneously on the carbon, sulfur, and nitrogen channels. Each compound is present at the 2-to 5-nanogram level, except the last one which is 100 times more concentrated. Figure 1 Chromatograms showing simultaneous detection of carbon, sulfur, and nitrogen on the AED. 71

78 Selectivity and Sensitivity Interferences Interferences The AED uses real time multipoint background correction to improve selectivity. This technique is only possible with multiple detectors, such as the photodiode array (PDA) in the AED, and permits the reduction of undesired responses by two or three orders of magnitude. The basis for this process is found in the spectra collected during the chromatogram. Figures 2 and 3 show portions of spectra taken during the elution of the sulfur containing peak, the nitrogen containing peak, a hydrocarbon peak, and a baseline region between peaks. 400 K 30 2a K 0 60 K 40 K 20 K 0 20 K 40 K 60 K 30 Figure 2 Sulfur Compound Hydrocarbon b Spectra taken during peaks of figure 1. (a) a sulfur containing compound, (b) a hydrocarbon. Figure 2 spans a wavelength region of 168 to 184 nm (lower axis), which was sensed by 80 of the detecting diodes in the PDA. These diodes are numbered 30 72