SOLAAR Series Software Manual

Transcription

1 SOLAAR Series Software Manual Thermo Fisher Corporation Registration No SOLAAR House, 19 Mercers Row, Cambridge CB5 8BZ.United Kingdom. Telephone +44 (0) , Fax +44 (0) ,

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3 Contents Chapter 1 Introduction Windows Windows Help Displaying Help for Windows Chapter 2 SOLAAR Installation Spectrometer software GFTV software SOLAARsecurity software Software installation SOLAAR Data Station software Installing the USB drivers on the Data Station Installing the USB drivers on the Data Station (Vista) Determining the COM port of the Spectrometer Determining the COM port of the Spectrometer using Vista 2-8 Installing the Data Station software Initialising the installation Selecting the Installation folder Downloading software to the spectrometer Installing the Support Documentation Installing the Adobe Acrobat Reader The Thermo SOLAAR program group Repairing and removing the SOLAAR software SOLAAR software and printers Getting Help for installing a new printer Starting the SOLAAR application Starting SOLAAR Creating a desktop shortcut to SOLAAR Starting SOLAAR automatically with Windows Logging in to SOLAAR software Startup option Chapter 3 SOLAAR Software Overview Dual Analyses SOLAAR Wizards Methods Sample Details Results Working with SOLAAR SOLAAR Status windows SOLAAR Method property sheet SOLAARsecurity Pre-Installation Manual - Contents i

4 SOLAAR dialogue boxes SOLAAR Menus SOLAAR Tool Bar SOLAAR Status Bars On-line Help Learning to use the On-line Help system Opening the Help Topics: SOLAAR dialogue box SOLAAR Help Table of Contents and Help topics Context-sensitive Help Menu Commands, Status windows and Tools Dialogue boxes and Property pages Controls on dialogue boxes and Property pages Chapter 4 Getting Started A simple flame analysis Before starting Setting up the Method General Method parameters Sequence Method parameters Spectrometer Method parameters Flame Method parameters Calibration Method parameters Saving and loading Methods Saving a Method in the Methods Database Loading a previously saved Method Installing a lamp Setting up the lamp Lighting the flame and optimising the burner parameters Lighting the flame Optimising the burner position Running the analysis Viewing the results Printing the results A simple furnace analysis Before starting Setting up the Method General Method parameters Sequence Method parameters Spectrometer Method parameters Furnace Method parameters Calibration Method parameters Sampling Method parameters Installing and aligning the lamp Installing and aligning the Graphite Furnace Loading the sample solution on to the Autosampler Aligning the Graphite Furnace Autosampler Running the analysis Viewing and printing the results Viewing absorbance signals ii SOLAARsecurity Pre-Installation Manual - Contents

5 A simple vapour analysis Sequence Method parameters Spectrometer Method parameters Vapour Method parameters Calibration Method parameters Lighting the flame Viewing and printing the results Chapter 5 Dual Analyses A simple dual analysis Setting up and running a Dual Analysis Dual Analysis Results Chapter 6 The OQ Tests Software Starting the OQ Tests application Using the OQ Tests Application Customer Diagnostics Appendix 1 Upgrade Considerations SOLAARsecurity Pre-Installation Manual - Contents iii

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7 Chapter 1 Introduction Congratulations on the purchase of your Thermo Scientific Atomic Absorption system and Thermo SOLAAR software. SOLAAR ia a powerful, user-friendly system that will meet all your needs for elemental analysis using Atomic Absorption Spectrometry. We hope that you will quickly become familiar with the operation and capabilities of your system. This manual shows you how to install and use the SOLAAR Data Station and OQ Tests software. It should be used in conjunction with the other AA Series User Documentation supplied with your system, in particular: the Operators manual this describes the installation, alignment and use of the Spectrometer and accessories. the Methods manual this describes the physical and chemical principles underlying the technique of Atomic Absorption Spectrometry, and gives practical guidance on sample preparation and related topics. the On-line Help system this gives a detailed description of the software, together with instructions on how to carry out all the main operations. It also includes the On-Line Cookbook, which gives recommended values for the basic parameters for all the elements that can be measured by Atomic Absorption Spectrometry. This is described in more detail in the SOLAAR Software / On line Help section. The SOLAAR Data Station and SOLAAR OQ Tests software also form part of the SOLAARsecurity software package, which includes additional software components that provide enhanced features such as Access Control and Electronic Signatures. These are required to allow the SOLAAR software to fulfil the requirements of the 21 CFR Part 11 Rule, which applies to organisations regulated by the United States Food and Drugs Administration. Additional documentation is supplied in the SOLAARsecurity package that describes these facilities and their use, and they are not discussed in this manual. SOLAAR Series Software Manual 1-1

8 Windows Windows Your SOLAAR Data Station software operates under the Microsoft Windows 2000 (SP4), Windows XP (SP2) and Windows Vista Ultimate operating systems. SOLAAR software has been designed to use these operating systems and makes optimal use of their facilities. Note: SOLAAR may not work under earlier versions of Windows operating systems. In general SOLAAR follows the general conventions of Microsoft Windows and it is expected that the analyst has a good understanding of the operating system and functions. Commands and functions that are common to Windows application programmes will not be described. It is assumed that buttons such as OK and Apply are to be selected when the analyst has completed a selection of options in a dialog box/window and the Cancel button closes a dialog box/window and erases and data entry or alteration. In many cases there is more than one acceptable way to perform a task, access a window etc. Windows Help All versions of Windows are provided with extensive On-line Help, which covers all aspects of day-to-day operation. Displaying Help for Windows To display the On-line Help system for using Windows: 1. Click on the button at the bottom left-hand corner of the screen to display the Start menu: 1-2 SOLAAR Series Software Manual

9 Windows 2. Click on the Help and Support command. The Windows Help and Support Center window will be displayed: In other versions of Windows, the Help Topics dialogue box may be displayed in a slightly different format. 3. Click on a Help Topic to open it. Navigate through the menus on the left hand side of the window to find the specific subject you re interested in: In other versions of Windows the navigation screens within the Help section may look slightly different. 4. Click or double click on the topic that you want to view to select and display it. For more help in using the Windows On-line Help refer to the information in the Windows basics Tips for using Help topic. SOLAAR Series Software Manual 1-3

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11 Chapter 2 SOLAAR Installation SOLAAR Series Software Manual 2-1

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13 Software installation Spectrometer software The Spectrometer in your AA Series Atomic Absorption system contains a powerful embedded microprocessor to control the low-level operations of the various sub-systems and accessories. This microprocessor runs software that is resident in the Spectrometer itself, which is normally installed and tested during the manufacture of the equipment. From time to time we will release updated versions of this resident software to enhance the performance of the system and provide new facilities these can be installed from your Data Station. Very rarely, a fault in the Spectrometer can corrupt the resident software. A copy of this software is therefore included on the SOLAAR Software distribution CD ROM, so that it can be re-installed in the Spectrometer from the Data Station if required. GFTV software SOLAARsecurity software Your AA Series Atomic Absorption Spectrometer may be fitted with the Graphite Furnace Television (GFTV) accessory. This is included as a standard feature on many instruments and can also be provided as a factory-fitted upgrade. The video from the GFTV accessory is displayed within the SOLAAR software itself. If you have purchased the SOLAARsecurity software package, please refer to the documentation included in that package for installation instructions. If you have bought your computer as part of a complete system from or from one of our Agents, the software may have been pre-installed in our factory. The software will have been fully tested, both in our factory before shipping and again during installation by our trained Service Engineers in your laboratory. Software installation SOLAAR Data Station software If you have supplied your own computer, the Service Engineer will install and test the software during installation. You will only have to install the software yourself if: you want to move the software from one computer to another you want to upgrade the software with a newer version supplied by us your original installation has become corrupted. You will need: a PC of appropriate specification and capable of running the appropriate Microsoft Windows operating system. the appropriate system access rights. the computer must also have the following facilities: a CD-ROM Drive a fixed hard disk drive with at least 1 GByte free space available an SVGA colour monitor (minimum 1024 x 768 resolution with 256 colours) SOLAAR Series Software Manual 2-3

14 Software installation an appropriate port for communication with the spectrometer an appropriate printer port a Windows-compatible mouse an appropriate Windows operating system installed on the computer a SOLAAR Software Installation CD-ROM to upgrade the Spectrometer software, the Spectrometer must be available and correctly connected to the Data Station. Installing the USB drivers on the Data Station The USB drivers are required so that the Data Station can communicate with the spectrometer. The drivers may have been installed on your computer when the SOLAAR Data Station software was installed, either at the factory if it was part of a complete system or by one of our Service Engineers if you supplied your own computer. However, there may be situations where you need to install the drivers yourself, such as moving the SOLAAR software to another computer. To carry out the USB driver installation on your computer you will need the SOLAAR Software Installation CD-ROM. 1. Ensure that the Spectrometer is off. 2. Connect a USB lead between your computer and the USB socket on the Spectrometer. A suitable USB lead is provided with the Spectrometer. 3. Insert the SOLAAR Software Installation CD-ROM into the CD-ROM drive of your PC If the SOLAAR Installation program automatically starts, select Exit. 4. On your computer, launch the Control Panel. 5. In the control panel window, double-click on the System icon. 6. In the System Properties window. Select the Hardware tab, and click on the Windows Update button. 7. In the Connect to Windows Update window, select the Ask me to search Windows Update every time I connect a new device and then click OK. 8. The System Properties window and Control Panel window can now be closed. 9. Turn on the Spectrometer. 10. The Found New Hardware Wizard window will appear. Select the No, not this time radio button and then select the Next button. 2-4 SOLAAR Series Software Manual

15 Software installation 11. Then select the Install from a list or specific location (Advanced) radio button and then select the Next button. 12. In the next window, select the Search for the best driver in these locations radio button. Ensure that the Search removable media (floppy, CD-ROM ) is ticked. Then select the Next button. 13. The wizard will now search for the drivers. Once the wizard has completed, select the Finish button. 14. As there are two or three drivers to install, depending on whether your Spectrometer is fitted with a GFTV. Follow steps 5 to 8 until the computer has found all the new hardware. 15. Your computer is now ready to be used with the Spectrometer. SOLAAR Series Software Manual 2-5

16 Software installation Installing the USB drivers on the 1. Ensure that the Spectrometer is off. Data Station (Vista) 2. Connect a USB lead between your computer and the USB socket on the Spectrometer. A suitable USB lead is provided with the Spectrometer. 3. Insert the SOLAAR Installation CD-ROM into the CD- ROM drive of your PC. If the SOLAAR Installation starts automatically, select Exit. Installing the 4. USB On drivers your computer on a Data launch Station the (VISTA) Control Panel. 5. In the Control Panel window, double click on the System icon 1. Ensure that and the then Spectrometer double click is on off. the Advanced System Settings on 2. Installing Connect the a Task USB USB List drivers lead between on a Data your Station computer (VISTA) and the USB socket on the Spectrometer. A suitable USB lead is provided with the Spectrometer. 3. Insert 6. the In SOLAAR the System Installation Properties CD-ROM window into select the CD-ROM the Hardware drive of tab your and PC. If the 1. Ensure that the Spectrometer is off. SOLAAR 2. Connect click Installation a USB the lead starts Windows between automatically, your Update computer Driver select and Exit. the Settings USB socket button the 4. On your Spectrometer. computer A launch suitable the USB Control lead is provided Panel. with the Spectrometer. 5. In 3. the Insert 7. Control In the the SOLAAR Panel Windows window, Installation Update double CD-ROM Driver click into on Settings the System CD-ROM window icon drive select and of your then Ask PC. double If the click on the SOLAAR Advanced me Installation each System time starts I connect Settings automatically, a on new Task device select List Exit. before checking for 6. In 4. the On System your drivers. computer Properties Click launch OKwindow the Control select Panel. the Hardware tab and click on the Windows 5. In the Control Update Panel Driver window, Settings double button click on the System icon and then double click on 7. In the 8. the Windows The Advanced System System Update Properties Settings Driver Settings and on Control Task List window Panel select windows Ask me can each now time I 6. In the System Properties window select the Hardware tab and click on the connect be a new closed. Windows Update device Driver before Settings checking button for drivers. Click OK 8. The 7. In 9. System the Turn Windows Properties on the Update Spectrometer and Driver Control Settings Panel window windows select can Ask now me be each closed. time I 9. Turn connect the Spectrometer a new device before checking for drivers. Click OK 10. The 8. The 10. Found System The New Found Properties Hardware New and Hardware Wizard Control window Wizard Panel will windows appear. can will Select now appear. be Locate closed. and install 9. Turn on the Spectrometer 10. The Found New Hardware Wizard window will appear. Select Locate and install driver software. driver software. Select Locate and install driver software. 11. In the next window select Don t search on line 11. In the 11. next In window the next select window Don t select search Don t search line on line. 12. When the next wizard dialogue box appears click Next. 2-6 SOLAAR Series Software Manual 12. When the next wizard dialogue box appears click Next.

17 Software installation 12. When the next wizard dialogue box appears click Next. 13. Once the driver has been installed the Found New Hardware 13. Once Wizard the should driver has advise been you installed that the the installation Found New is Hardware complete. Wizard shoul 13. Once the you driver that has the been installation installed is complete. the Found New Hardware Wizard should advise you that the installation is complete. 14. Once the wizard has completed, select the Close button. 14. Once 14. Once the wizard has completed, select the Close button. 15. the As wizard there has are completed, two or three select drivers the to Close install, button. depending on whether your Spe 15. As there 15. is are As fitted two there with or three are a two GFTV. drivers or three Follow to install, drivers steps depending to 10 install, to 14 until on whether depending computer your Spectromete on has found a is fitted with hardware. a GFTV. Follow steps 10 to 14 until the computer has found all the ne hardware. whether your Spectrometer is fitted with a GFTV. Follow steps 16. Your computer is now ready to be used with the Spectrometer. 16. Your computer 10 to 14 is now until ready the computer to be used has with found the Spectrometer. all the new hardware. 16. Your computer is now ready to be used with the Spectrometer. SOLAAR Series Software Manual 2 -

18 Installing the Data Station software Determining the COM port of the Spectrometer To determine which COM port the Spectrometer has been assigned on your computer: 1. Connect the Spectrometer to your computer using the supplied USB cable. 2. Ensure the Spectrometer is turned on. 3. Click on the button on the desktop and then select Control Panel. 4. In the Control Panel window, double click on the System icon. 5. In the System Properties window, select the Hardware tab. Then click on the Device Manager button. 6. In the Device Manager window, click on the + next to Ports (COM &LPT). 7. The COM port that is assigned to your Spectrometer is the first in the list labelled CP210x USB to UART driver (COMx). Where COMx is the COM port number. Determining the COM port of the Spectrometer using Vista When setting up the communications port in the SOLAAR Data Software, select the COM port that is assigned to the spectrometer. Determining the COM port of the Spectrometer using VISTA To determine which COM port the Spectrometer has been assigned on your computer: Determining the COM port of the Spectrometer using VISTA 1. Connect the Spectrometer to your computer using the supplied USB cable. 2. Ensure 1. Connect the the Spectrometer to your is turned computer using on. the supplied USB cable. To determine which COM port the Spectrometer has been assigned on your computer: Determining the COM port of the Spectrometer using VISTA To determine 2. which Ensure COM the Spectrometer port the Spectrometer is turned on. has been assigned on your computer: 3. Click on the button on the desktop and then select 3. Click on the button on the desktop and then select Control Panel. Control 4. In the Control Panel. Panel window, double click on the System icon. 5. In the System Properties window, click on the Device Manager button. 4. In the Control Panel window, double click on the System icon. 5. In the System Properties window, click on the Device Manager button. 1. Connect the Spectrometer to your computer using the supplied USB cable. 2. Ensure the Spectrometer is turned on. 3. Click on the button on the desktop and then select Control Panel. 4. In the Control Panel window, double click on the System icon. 5. In the System Properties window, click on the Device Manager button. 6. In the Device Manager window, click on the + next to Ports (COM &LPT). 7. The COM port that is assigned to your Spectrometer is the first in the list labelled Silicon Labs CP210x USB to UART Bridge (COMx). Where COMx is the COM port number. 2 - SOLAAR Series Software Manual 6. In the Device Manager window, click on the + next to Ports (COM &LPT). 7. The COM port that is assigned to your Spectrometer is the first in the list labelled Silicon Labs CP210x USB to UART Bridge (COMx). Where COMx is the COM port number.

19 Installing the Data Station software In the In the Device Manager window, click on the + next to Ports (COM &LP 7. (COM The COM & LPT). port that is assigned to your Spectrometer is the first in the lis 7. The Silicon COM Labs port that CP210x is assigned USB to to UART your Bridge Spectrometer (COMx). is Where the first COMx is number. in the list labelled Silicon Labs CP210x USB to UART Bridge (COMx). Where COMx is the COM port number. Installing the Data Station software Initialising the installation To install the SOLAAR software: 1. Turn on your Data Station and wait until Windows has started if the Data Station is already turned on, exit from any programs that are running. 2. Insert the Software Installation CD-ROM into the PC s CD- ROM drive. If your PC has been set up to start programs automatically when a CD-ROM is inserted (this is the default), the SOLAAR Installation program will start automatically and you should go straight to Step 7 below. Otherwise, follow Steps 3 to 6 first. 3. Click on the button on the taskbar to display the Start menu. 4. Click on the Run command to display the Run dialogue box. 5. Type D:\autorun.exe (replace D with the appropriate letter if your CD-ROM drive is not the D drive) into the Open box: SOLAAR Series Software Manual 2 -

20 Installing the Data Station software 6. Click on OK to close the dialogue box and start up the SOLAAR Installation program. The following dialogue will be displayed: To install the SOLAAR Data Station software, move the mouse pointer over Install SOLAAR Data Station and click the mouse button. The Security Options dialogue will be displayed. If you are installing the SOLAAR Data Station software only (i.e., you are NOT installing the data station for operation with the full SOLAARsecurity package), select the No option and click OK. If you ARE installing the data station for operation with the full SOLAARsecurity package, then you should refer to the installation instructions included in the user documentation supplied with the package. The automatic installation Wizard will then start. A series of dialogue boxes will be displayed, reporting the progress of the installation and prompting you to make certain choices. When you have read the contents of a dialogue box, and supplied any necessary information, click the Next button to move on the next step SOLAAR Series Software Manual

21 Installing the Data Station software Selecting the Installation folder. During the installation this dialogue will be displayed, to allow you to install SOLAAR into a folder of your choice. We recommend that you accept the default folder. When the Installation Wizard has all the information that it needs, the Wizard will display the Start Installation dialogue. You can use the Back button on this dialogue to return to any of the previous dialogues to change the information you have entered. When you click on the Next button, the installation will start. When the installation has been completed, the Wizard will display a final dialogue confirming that the installation has been successful. Click the Finish button to complete the installation. Downloading software to the spectrometer To download the spectrometer software to the spectrometer: 1. Turn on the spectrometer and ensure the Data Station is connected to the PC via an appropriate cable. 2. Start up the SOLAAR Installation program see the previous section. 3. Click on Download System Software on the first Installation dialogue box to display the Download Parameters dialogue. SOLAAR Series Software Manual 2-11

22 Installing the Data Station software 4. Use the drop down list at the left of the dialogue to select the Data Station s USB/serial port that you are using. 5. Use the four radio buttons in the middle of the screen to select the type of download that you want to perform. Use the first radio button to download new software to the spectrometer. Use the second radio button to download new software to a Graphite Furnace accessory connected to the spectrometer. Use the third radio button to download a new version of the Local Control software. You must have a Local Control module fitted before you can do this. Use the fourth radio button to download new software to the VP100 vapour accessory. 6. When you have selected the type of download required, click on the Download button to display the dialogue below. 7. Confirm that you have correctly connected an appropriate cable to the spectrometer and then click the Continue button. 8. You will then be prompted to turn the target systems OFF, then ON again. This will ensure that the software in the target system has been correctly initialised. Click OK when you have done this and the download will take place. 9. A dialogue showing the progress of the download will be displayed. 10. When the download has been successfully completed, a prompt will be displayed instructing you to switch the target system OFF, then ON again, to initialise the new software. Click OK when you have done this. The system with the new software is then ready to be used SOLAAR Series Software Manual

23 Installing the Data Station software Installing the Support Documentation The Support Documentation contains a wealth of Applications data, Technical information and On-line versions of the system Manuals. The Installation program will create shortcuts to these from the SOLAAR program group and optionally copy the files on to your hard drive. Install Support Documentation. Follow the instructions on the screen to complete the installation of the Support Documentation. Installing the Adobe Acrobat Reader The Support Documentation is provided as Portable Document Format (.pdf) files. To access these files you must install the Adobe Acrobat Reader. Follow the instructions on the screen to complete the installation of the Adobe Acrobat Reader. SOLAAR Series Software Manual 2-13

24 The Thermo SOLAAR program group The Thermo SOLAAR program group During the installation of the SOLAAR software, a Start Menu All Programs group is created that contains shortcuts to the SOLAAR application and to other related applications and documents. Click on the item in the menu to start the application or view the document. The following table gives a very brief summary of what each of the main icons represents. The main SOLAAR application select this to start the SOLAAR software. The SOLAAR Help system select this to display On-line Help for using SOLAAR software. The OQ Tests select this to start the SOLAAR OQ Tests program. This program also includes a set of Customer Diagnostics tests, to allow you to identify simple faults that may occur. Repairing and removing the SOLAAR software Repairing and removing the SOLAAR software The Installation Wizard can repair a SOLAAR installation if the program files become corrupted or damaged. It can also remove the application, or roll back to the previous version. To repair or remove the main SOLAAR software from your Data Station: 1. Turn on your Data Station and wait until Windows has started. 2. Click on the button to display the Start menu SOLAAR Series Software Manual

25 Repairing and removing the SOLAAR software 3. Click on Control Panel to display the Control Panel: (Different operating systems may display differently) 4. Click on Add or Remove Programs to display the Add or Remove Programs menu. 5. Click on the Remove a Program icon to display the Add or Remove Programs Properties dialogue box: SOLAAR Series Software Manual 2-15

26 Repairing and removing the SOLAAR software 6. Click on SOLAAR in the list, and then on Change/Remove to display the Select Uninstall Method dialogue box: 7. Click on Custom if you want to be able to select which files, folders and settings to remove; otherwise leave Automatic selected and click on Next to display the Perform Rollback dialogue box: 2-16 SOLAAR Series Software Manual

27 Repairing and removing the SOLAAR software 8. If your current version of SOLAAR software was installed over an earlier version and you chose to backup that earlier version when you installed the newer one, the uninstall procedure will allow you to remove the newer version and replace it with the older one. This facility is provided to assist with fault diagnosis; usually you will not need to use it. Click on Next to display the Perform Uninstall dialogue box: 9. If you are sure you want to uninstall SOLAAR click on Finish to remove the program, otherwise click on Cancel. Note: This procedure will NOT remove any data files created by the SOLAAR software to remove, back up or copy these, refer to the Windows On-line Help. For this reason, it is likely that the c:\solaarm folder and one or more files or folders contained in it will remain on your hard disk. If you are sure that there are no necessary data files in these folders, remove them using the normal Windows techniques for deleting files and folders. SOLAAR Series Software Manual 2-17

28 SOLAAR software and printers SOLAAR software and printers Getting Help for installing a new printer The SOLAAR Data Station software will work with any type of printer that is supported by the Windows operating system. Before you can use a printer, you must first install it into your Windows system. The Windows On-line Help system will guide you through this process if you have to install a new printer. To get Help for installing a new printer: 1. Turn on your Data Station and wait until Windows has started. 2. Click on the button on the taskbar to display the Start menu. 3. Click on the Help and Support command to display the Windows Help dialogue box. 4. Click on the Printing and Faxing link in the Help topics menu on the left-hand side of the screen. 5. On the Printing and Faxing Help screen click on Printing and then on Basic Printing Tasks. This will bring up a menu that allows you to select Help topics for either connecting a printer directly to your computer, or connecting to a printer on a network. In other versions of Windows, the procedure required to locate and access this information may be slightly different. 6. Follow the instructions given in the Help topic SOLAAR Series Software Manual

29 Starting the SOLAAR application Starting the SOLAAR application During installation a Thermo SOLAAR submenu is added to the Program section of the Start menu. The instructions in the next subsection show you how to use this to start SOLAAR software. However, Windows provides several other ways of starting an application, which you may find more convenient. You can, for example: create a shortcut on the desktop that will start the application without using the Start menu at all. create a SOLAAR shortcut in the StartUp folder, so that SOLAAR starts automatically when Windows is started. Starting SOLAAR To start the SOLAAR software: 1. Turn on your Data Station and wait until Windows has started. 2. Turn on the Spectrometer and its services if required. 3. Click on the button to display the Start menu. 4. Click on All Programs to display the list of program groups, then Thermo SOLAAR to display the SOLAAR icons: 5. Click on SOLAAR to start the SOLAAR software. Creating a desktop shortcut to SOLAAR To create a desktop shortcut to SOLAAR: 1. Right-click on the background of the desktop to access a pop-up menu. 2. Click on New to display a submenu. 3. Click on Shortcut in the New submenu to display the Create Shortcut dialogue box: SOLAAR Series Software Manual 2-19

30 Starting the SOLAAR application 4. Enter the path to the SOLAAR application program (the default is C:\SOLAARM\PROGRAM\Solaar32.exe), or click on Browse to display a standard Windows file browser dialogue box so that you can select the file. 5. Click on Next to display the Select a Title for the Program dialogue box: 6. Edit the name for the shortcut to read SOLAAR and click on Finish. The new shortcut will appear on the desktop: To start SOLAAR using the desktop shortcut double-click on the SOLAAR icon. Starting SOLAAR automatically with Windows To make SOLAAR start automatically when Windows is started: 1. Click on the button on the taskbar to display the Start menu. 2. Navigate to the Thermo SOLAAR program group. 3. Right-click on the SOLAAR icon and select Create Shortcut: 2-20 SOLAAR Series Software Manual

31 Logging in to SOLAAR software 4. Clicking on Create Shortcut will produce a second icon with the default name SOLAAR (2). 5. Drag and drop the SOLAAR (2) shortcut into the Startup folder: SOLAAR will now start automatically when Windows starts. Logging in to SOLAAR software When SOLAAR starts up, it first displays the Login dialogue box so that you can log in as the current user. To log in with the Security System disabled: 1. Start SOLAAR and wait until the Login dialogue box is displayed. 2. Either accept the default user name SOLAAR Operator or type your own name in the Operator name field. If your Windows installation is set up so that you have to log in to Windows when you start up the Data Station, the SOLAAR software will automatically display your Windows login User Name. You can change this if you were not the person who logged in to Windows. 3. Click on OK to log in and start SOLAAR. SOLAAR Series Software Manual 2-21

32 Logging in to SOLAAR software Startup option Once you have logged in, SOLAAR will start up. You will be able to choose what happens when the program opens, but the default is for the Wizard Launcher dialogue box to be displayed see SOLAAR Software / Overview / SOLAAR Wizards section for an overview of the SOLAAR Wizards. If you want to choose another Startup option, you will need to close the Wizard Launcher dialogue box first. To do this: Click on Close in the Wizard Launcher dialogue box. To choose the Startup option: 1. Click on Options on the View menu to display the Options dialogue box. 2. Click on the Startup tab to display the Startup page: 3. Click on the radio button for the option you require. If you choose Display Wizards on Startup the Wizard Launcher dialogue box will be displayed when the program opens this is the default. If you choose Display Method on Startup, when the program opens the Method property sheet will be displayed showing the Method that was the Current Method when the program closed see Section for an overview of Methods. If you choose Neither the program will start up without opening any dialogue boxes. 4. Click on OK to close the dialogue box and set the Startup option SOLAAR Series Software Manual

33 Chapter 3 SOLAAR Software SOLAAR Series Software Manual 3-1

34 Overview This page is intentionally blank. 3-2 SOLAAR Series Software Manual

35 Overview Overview Overview Overview The SOLAAR The SOLAAR Data Data Station Station software software works works with the with AA the Series AA Series Spectrometers Spectrometers and accessories and accessories to produce to produce analytical analytical results results from from your your samples samples using using Atomic Atomic Absorption Absorption analysis. analysis. In order In order to carry to carry out an out an analysis analysis by Atomic by Atomic Absorption Absorption Spectrometry Spectrometry using using the AA the Series AA Series system, system, you will you need will to need carry to carry out some out some or all or of all the of following the following steps: steps: develop the develop methodology the methodology prepare the prepare samples the and samples standard and solutions standard solutions set up and set align up the and instrument align the instrument and accessories and accessories set up the set analysis up the on analysis the Data on Station the Data Station carry out the carry analysis out the analysis review and review present and the present results. the results. Development Development of the of analytical the analytical methodology methodology should should cover cover the whole the whole analysis, analysis, including including sample sample collection, collection, sample sample preparation, preparation, selection selection of the of the elements elements to be measured, to be measured, the instrument the instrument and accessories and accessories to be used to be and used and the values the values of their of operating their operating parameters. parameters. SOLAAR SOLAAR software software provides provides many many tools to tools help to you help select you select and optimise and optimise the instrument the instrument parameters, parameters, but the but the process process of developing of developing methodology methodology is outside is outside the scope the scope of this of manual. this manual. Standard Standard and sample and sample preparation preparation techniques techniques are discussed are discussed in some in some detail detail in the in Atomic the Atomic Absorption Absorption Methods Methods Manual Manual and will and not will be not be discussed discussed further further here. here. Instrument Instrument setup setup and alignment and alignment is described is described in detail in detail in the in Hardware the Hardware manual, manual, while while techniques techniques for aligning for aligning the system the system and accessories and accessories are also are also described described in the in How the How to section to section of the of SOLAAR the SOLAAR On-line On-line Help Help system. system. Setting Setting up an up analysis an analysis using using SOLAAR SOLAAR software software involves involves changing changing the default the default values values of parameters of parameters and options and options to suit to the suit methodology the methodology defined defined for the for analysis. the analysis. The information The information that SOLAAR that SOLAAR handles handles is is grouped grouped into distinct into distinct functions, functions, shown shown below: below: SOLAAR Series Software Manual - SOLAAR Series Software Manual 3-3

36 SOLAAR Wizards The parameters associated with the operation of the Spectrometer and its accessories are grouped together into Methods a single Method specifies all the parameters necessary to analyse a set of samples for a set of elements by a specific technique. The Method also includes an Action List, which specifies the operations that you want to carry out during the analysis. Possible actions include the analysis of samples, determination of blank values, calibration and a variety of QC tests. For some types of analysis when you are not using an autosampler, you can specify the actions required as you make the measurements. For analyses where you are using an autosampler and more complex manual analyses, you can specify the actions required before you start the analysis. The Action List appears in an Analysis Matrix. This allows you to choose which actions in the Action List should be carried out for each of the elements during the analysis. When the analysis is run, the results are stored in a database and can be viewed in a Results window. You can choose which results to view and what data to see for each result. You can display a detailed view of the results showing several or all of the result parameters, or a summary showing a selected parameter for each of the elements in the analysis. The Final Results can be printed to produce a Report of the analysis. SOLAAR provides you with considerable flexibility in choosing what to include in the Report. Saved results can also be exported to other applications for further processing or archiving. As well as exporting saved results, SOLAAR software can export results as they are produced to one of the serial communications ports on the Data Station, which can be connected to a Laboratory Integrated Management System (LIMS). Dual Analyses Some models in the AA Series range of spectrometers are equipped with dual sample compartments. The SOLAAR software enables you to run a Method in the left-hand compartment and then automatically switch to the right-hand compartment and run a second method. This is referred to as a Dual Analysis. SOLAAR Wizards SOLAAR provides a number of software Wizards to help you with some of the more complex tasks you will need to carry out when you are using the program. Wizards guide you step-by-step through the procedure of setting up and carrying out operations using the software. The Getting Started chapter in this manual gives instructions for setting up and carrying out operations manually rather than by using a Wizard. 3-4 SOLAAR Series Software Manual

37 SOLAAR Wizards SOLAAR Wizards can help you to: create a new method run an analysis adjust and optimise the flame system set up and optimise a graphite furnace analysis adjust and align accessories optimise the spectrometer parameters for your analysis measure and calculate performance criteria, such as Characteristic Concentrations and Detection Limits, for your analysis. choose what Results to display and what data should be shown for them print a Results Report. To use one of the Wizards: 1. Click on the Wizards toolbar button or click on Wizards in the Help menu to display the Wizard Launcher dialogue box. Note: By default, the Wizard Launcher dialogue box is opened when you start up SOLAAR see SOLAAR Installation / Start up Option Section for how to set the Startup option. 2. Click on the button for the Wizard you want to run. SOLAAR Series Software Manual 3-5

38 Methods Methods SOLAAR Methods allow you to: use one of the Flame, Furnace or Vapour techniques for an analysis for certain types of Vapour analysis, you can specify which dual atomiser spectrometer sample compartment is to be used use Autosamplers and a variety of other accessories for an analysis measure up to 500 samples in a single analysis measure 1 to 16 elements in these samples in a single analysis control the sequence of actions to be performed for each element in an analysis access all instrumental parameters needed to analyse samples for each element using the Method property sheet use default values for all instrumental parameters edit the default parameters define Sample Details consisting of a Sample Identification label, a Dilution Factor and a Sample Mass for each sample SOLAAR Methods can be: set up using the SOLAAR Method Wizard viewed, created and edited in the Methods tabbed dialogue box saved in and loaded from the Method Library Techniques for working with Methods are described in the Methods Overview section of the SOLAAR On-line Help system. Sample Details SOLAAR Sample Details: allow naming of samples random or sequential names can be used. can correct results for sample dilution can correct results for sample mass can be used to change the concentration units of the results can be exported and imported as text or CSV files can be viewed and edited in the Sample Details dialogue box Techniques for working with Sample Details are described in the Sample Details Overview section of the SOLAAR On-line Help system. Results SOLAAR Results: are generated when you run an analysis of your samples using a Method are saved in a Results database. The following data is stored with the results: the Sequence parameters all Method parameters the Sample Details used 3-6 SOLAAR Series Software Manual

39 Working with SOLAAR the signal results the concentration and corrected concentration results the relative standard deviations of the results the raw signal data this can be deleted to save space in the database can be viewed in the Results and Signal Windows: results are displayed in real time as they are produced you can choose which results to display and what data to show for each result. can be viewed in Detail or Summary mode can be edited. You can: delete and restore individual resamples and mean results recalculate standard curves change the type of calibration algorithm used change the sample details used change the type of transient signal between height and area change the time period used for measuring transient signals can have changes traced, since all changes are logged in a separate audit trail for each element in each analysis can be printed in a Detail or Summary Report. You can: control precisely what is printed in the report using the Print Options command preview the printed report using the Print Preview command can be exported to text files and to the Clipboard: as text for use in word processors in.csv format for use in spreadsheets and databases Working with SOLAAR SOLAAR software provides several ways to interact with the Atomic Absorption system: Status Windows are used to display information about the system and the analysis and do not generally require you to enter information. The Status Bars at the bottom of the screen display the System Status, the sample being measured and a progress indicator showing the percentage of the current analysis that has been completed. If a flame or furnace analysis is being undertaken they will also display information about the parameters being used in the analysis. Dialogue boxes, including Property Sheets and their Property Pages, allow you to enter information such as parameter values and to select options. Unlike Status Windows dialogue boxes always contain at least one button, usually labelled OK. Clicking this button will close the dialogue box and implement the changes to parameter values or carry out the actions set in the dialogue box. SOLAAR Series Software Manual 3 -

40 Working with SOLAAR Most dialogue boxes also have a Cancel button. Clicking this will close the dialogue box, discarding any changes you have made to settings and without carrying out any actions. Menu commands and Tool Bar buttons are used to issue commands to the system to cause things to happen, such as an analysis to start or a dialogue box to open. Status windows: are used to display information: about your analysis about the system hardware can be opened or brought to the front of the display: by double-clicking the relevant icon if the window is minimised by clicking on the name of the window on the Windows menu have associated menus, which: appear on the menu bar when the window is active contain commands relevant to the window s content have context menus, which: appear when you right-click inside the window contain commands relevant to the window s content SOLAAR Status windows SOLAAR provides eight Status windows, although the windows that are displayed on the screen at any time will depend on the type of analysis being undertaken. The Status windows are: the Spectrometer Status window provides facilities for monitoring the Spectrometer optical system the Vapour Status window shows the status of the vapour system the Calibration window shows the calibration graph and calibration statistics the Signal window shows the analytical signal as it changes with time the Flame Optimisation Graph window shows the signal as it changes during a gas flow/burner height optimisation and has the title Gas Flow Graph or Burner Height Graph depending on the data it shows the QC Protocol window shows the QC Control Chart for all the results selected for display in the Results window for the element selected in the Results window. The chart plots corrected concentration (Y axis) for each result (X axis), with results ordered chronologically with the earliest results first 3 - SOLAAR Series Software Manual

41 Working with SOLAAR the Results window shows the analytical results for the current analysis, or from a Results file the Ash Atomise window displays the results of an Automatic Ash Atomise experiment during and immediately after the experiment, or when you have loaded an Ash Atomise file SOLAAR Method property sheet The SOLAAR Method property sheet: provides one stop access to all instrumental parameters via the Method property pages provides default values for all instrumental parameters allows you to edit the default parameters allows you to save and load Methods can be opened by clicking on the Method Tool Bar button by clicking on Method on the Edit menu can be automatically opened when SOLAAR starts See... SOLAAR Installation / Start up option section SOLAAR provides nine Method property pages, although the pages that are included in the Method property sheet at any time will depend on the type of analysis being undertaken and, in certain cases, on options selected. The following list gives a brief description of each of the Method property pages: the General Method property page allows you to: name a Method identify the Operator describe the Method load and save Methods to and from the Methods Library create a new Method set the analysis technique specify whether standard solutions should be shared between... elements specify which Autosampler and rack you are using specify which flame dilutor or vapour system you are using the Sequence Method property page allows you to: set up the sequence of actions to be carried out during the analysis choose which elements are included for analysis at each step in the sequence set up sample details add reagent details for a furnace analysis view an Autosampler loading guide, which allows you to control the placement of samples and standards in the Autosampler SOLAAR Series Software Manual 3 -

42 Working with SOLAAR the Spectrometer Method property page allows you to view and edit: the Spectrometer optical parameters the signal measurement parameters the type of background correction used the Flame Method property page allows you to view and change: the type of flame the flame fuel gas flow rate flame stabilisation and nebuliser uptake time the burner height the Furnace Method property page allows you to view and edit: the Graphite Furnace parameters the Graphite Furnace program The Vapour/SFI Method property page allows you to view and edit: the vapour mode used Vapour/SFI analysis parameters the Calibration Method property page allows you to: select the calibration method and calibration algorithm view and edit the number and concentrations of your standard solutions set acceptable limits for calibration curvature, correlation coefficient and rescaling the Sampling Method property page allows you to: view and edit the Autosampler parameters view and edit the automatic solution preparation parameters (only available for flame/vapour analyses if the Flame Diluter accessory is fitted) for furnace analyses, view and edit the matrix modification parameters The QC Method property page provides facilities for you to: view and edit the parameters for the different QC Tests set the failure actions for the different QC Tests give a name to each type of QC test SOLAAR dialogue boxes SOLAAR dialogue boxes are used to view and edit other associated groups of parameters. There are many dialogue boxes used throughout the SOLAAR software, but the following are some examples that you will use frequently: The Log In dialogue box allows you to identify yourself and when SOLAAR is started. The Setup Dual Analysis dialogue box allows you to specify Methods for each sample compartment of a dual sample compartment instrument, and then run both Methods automatically SOLAAR Series Software Manual

43 SOLAAR Menus The Sample Details dialogue box allows you to view and edit the Sample Identification, Mass correction factors and Dilution Ratio for each sample in your analysis. The Reagent Details dialogue box allows you to view and edit the names of the reagents used in the Furnace Autosampler. The Autosampler Volumes dialogue box allows you to view the volumes of the different solutions that will be used by either the Flame Autosampler and Diluter accessory, or the Furnace Autosampler. The Autosampler Loading Guide dialogue box allows you to view and edit the layout of the different solutions in both Flame and Furnace Autosamplers. SOLAAR Menus SOLAAR Menus are used to issue commands to the software and hardware modules that make up the Atomic Absorption System. The menus are displayed on the menu bar at the top of the screen. The following gives a brief overview of the contents of the main SOLAAR Menus: The File menu contains commands for loading, saving, importing, exporting and printing files created by SOLAAR. When there is no open Results database, the File menu contains commands for creating and maintaining Results and Method databases. The Copy submenu in the Edit menu contains commands for copying information to the Windows Clipboard so that you can then paste it into documents in other Windows applications running on your Data Station. The remaining commands display the Method property sheets, dialogue boxes to specify and control lamp properties, a command to switch on the GFTV accessory (if fitted) and a screen to configure the OQ and PQ Results databases. The View menu contains commands to open non-editable dialogue boxes to view details of the Autosampler contents, to view the current OQ and PQ results and to turn on/off the Tool Bar and Status Line displays. It also contains a command to display the Options dialogue box, which allows you to configure a number of options controlling the program s operation. Another option allows you to hide the status bar at the bottom of the screen, while the final option allows you to customise the toolbars at the top of the screen. The Action menu contains commands controlling the connection between the Data Station and the Spectrometer, and the setup and operation of the Spectrometer and accessories. The Security command opens the Security dialogue box so that you can check which options have been enabled by the administrator to control access to SOLAAR features and data. The Stop command, which will only be enabled when an analysis is in progress and the System Status is BUSY, aborts the current analysis as soon as it is safe to do so. The current sample result will be lost, but all completed sample results will be available for you to save or print SOLAAR Series Software Manual 3-11

44 SOLAAR Menus as required. In most circumstances, it will be possible to continue the analysis at a later time, from the point at which it was stopped. The Windows menu contains commands controlling the display of the Status windows and icons in the main SOLAAR window. The Help menu contains commands that open the on-line Help system. Several of the Status windows have associated pop-up Context Menus, which can be displayed by right-clicking within the window area. These menus contain commands controlling the function and display of the specific Status window. For convenience, these menus are also displayed on the menu bar when the appropriate window is selected. The following gives a brief overview of the contents of the Status window menus: The Signal window context menu (and the Signal menu when the Signal window is selected) contains commands for adjusting the display of the signal, for setting and clearing reference signals and for placing a tracking cursor on the window. The Spectrometer Status window context menu (and the Signal menu when the Spectrometer Status window is selected) contains commands for adjusting the display of the signal, for displaying, hiding, freezing and unfreezing the Running Signal display and for choosing between displaying the signal and concentration. The Results window context menu and the Results menu contain commands for selecting the results to display and the data that should be displayed for them, for editing the results, and for viewing data related to a result. When an analysis is in progress, commands are available for adding actions to the sequence of the running analysis. If the displayed results belong to an analysis that was stopped before it was completed, a command to continue the analysis will be available. The Calibration window context menu and the Calibration menu contain commands for controlling the display of the Calibration Graph on the Calibration window, for changing the Calibration Line fit algorithm for the current calibration and for deleting and restoring calibration standards. The Ash Atomise window context menu and the Ash Atomise menu contain commands for controlling the display of the Ash Atomise graph on the Ash Atomise window and for choosing which elements in the current method should use the optimised values from the Ash Atomise experiment. The QC Protocol window context menu and the QC Protocol menu contain commands for controlling the display of the QC Control Chart on the QC Protocol window and for displaying details of a QC Test s results. The Flame Optimisation Graph window context menu and the Flame Optimisation menu contain commands for controlling the display of the Gas Flow Graph or Burner Height Graph depending on the data shown SOLAAR Series Software Manual

45 SOLAAR Tool Bar SOLAAR Tool Bar SOLAAR Tool Tool Bar Bar The The SOLAAR SOLAAR Tool Tool Bar Bar provides provides direct direct and and convenient convenient access access to to several several commonly commonly used used commands, commands, so so that that you you do do not not have have to to open open and and display display the the menus menus to to issue issue the the commands. commands. The The following following table table shows shows the the equivalent equivalent menu menu command command for for each each button button and and a a brief brief description description of of what what it it does: does: Action Autozero Action Setup Optics Action Flame Setup Action Flame Fuel Up Action Flame Fuel Down Action Flame Burner Up Action Flame Burner Down Action Autosampler Wash Action Autosampler Purge Action Clean Cuvette Action Autosampler Align Capillary Tip Action Analyse Action Pause Analysis Action Continue Analysis Action Single Solution Action Run Dual Analysis Edit GFTV Edit Lamps Edit Method Help Wizards View Customise Toolbars Help About SOLAAR Help What s This? performs an Autozero action sets up the spectrometer optics sets up the spectrometer gas control system increases the fuel flow rate to the flame by 0.1L/min, unless the fuel flow rate is at the maximum for the current type of flame decreases the fuel flow rate to the flame by 0.1L/min, unless the fuel flow rate is at the minimum for the current type of flame raises the position of the burner by 0.1mm, unless the burner is at its highest position lowers the position of the burner by 0.1mm, unless the burner is at its lowest position washes the Autosampler purges the Autosampler cleans the cuvette positions the furnace Autosampler capillary tip over the cuvette for alignment runs an analysis using the Current Method pauses the current analysis when the current sample measurement has been completed continues the current analysis after it has been paused runs a Single Solution analysis displays the Setup Dual Analysis dialogue box so that you can set up and run a dual analysis using both spectrometer compartments on a dual atomiser instrument displays the GFTV dialogue box so that you can switch the GFTV accessory on or off displays the Lamp Configuration and Status dialogue box so that you can control and specify the properties of the lamps displays the Method property sheet so that you can view or edit the current method, save the current method or load a saved method displays the Wizard Launcher dialogue box so that you can start one of the SOLAAR Wizards allows you to edit the buttons placed on the main toolbar and save customised toolbar designs displays the About dialogue box showing details of the version of the program you are running changes the pointer to the Help pointer, which causes the Help topic for the next item you click to be displayed. Thermo Thermo Fisher Fisher Scientific Scientific SOLAAR SOLAAR Series Series Software Software Manual Manual

46 SOLAAR Status Bars SOLAAR also provides facilities for you to create your own tool bars and buttons, to provide convenient access to commands that you use frequently. You can access these facilities from the Customise Tool Bars dialogue, which you can open by clicking the shortcut button on the Tool Bar, by selecting the Customise Tool Bars command from the View menu, or by right-clicking on the tool bar area of the screen and selecting the Customise command from the context menu displayed. Click on the Help button to access the On-line Help system, where you will find detailed instructions for creating and maintaining your own Tool Bars. SOLAAR Status Bars The SOLAAR Status Bars appear at the bottom of the screen. The right-hand end of the bottom Status Bar gives information about the current status of the software and the system, including the current element, the current sample identification and resample number, and the System Status. When an analysis is running, the centre area of the Status Bar contains a progress indicator showing the approximate percentage of the analysis that has been completed. The left-hand end of the Status Bar is used to give a brief Help message for the Tool Bar tool or Menu command underneath the pointer. The flame and furnace Status Bars are displayed only when a burner or furnace are fitted to the instrument. The flame Status Bar shows the status of the flame, the fuel flow rate, the type of burner fitted, the burner height and the status of each of the gases (air, acetylene and nitrous oxide). Several of these status sections are labelled either red or green, providing a simple, visual indication of the condition of that parameter. The furnace Status Bar displays information about the furnace phase, temperature, gas type and gas flow rate, number of cuvette firings and the status of the Autosampler SOLAAR Series Software Manual

47 On-line Help On-line Help Learning to use the On-line Help system SOLAAR contains a comprehensive On-line Help system giving full details of the operation of the software. There are several different ways to get help from the On-line Help system. You can get Help by: using the SOLAAR Help dialogue box see Sthe SOLAAR Software / On-line help / Opening the Help topics:solaar dialogue box section. using context-sensitive Help. This can display the appropriate Help for the specific tool, command, window, dialogue box or control you are using in the program. See the SOLAAR Software / On-line help / Context-sensitive help section for the different ways to get context-sensitive Help. Before learning about the SOLAAR Help in particular, you may want to look at the next section, which describes how to get general Help for using the Windows On-line Help system. Windows provides an On-line Help file explaining the basics of using the On-line Help system. SOLAAR gives you direct access to this file from the Using Help command on the Help menu. To learn how to use the On-line Help System: 1. Start SOLAAR, and close the Wizard Launcher dialogue box (click on Close) or Method property sheet (click on Cancel) if either was opened automatically. 2. Click on Help on the menu bar to display the Help menu: 3. Click on Using Help to display the Windows Help dialogue box. 4. If necessary, click on the Contents tab to display the contents page (this is the default page, but if you have used the dialogue box before, it will open at the page that was open when you last used it). In Windows XP you will see: SOLAAR Series Software Manual 3-15

48 On-line Help 5. Click in the left-hand pane on the topic for which you want help, to display the Help in the right-hand pane. Other versions of Windows provide similar facilities, but the details of the dialogue box displayed may be different. Opening the Help Topics: SOLAAR dialogue box To display the SOLAAR Help Topics: SOLAAR dialogue box: 1. Start SOLAAR, and close the Wizard Launcher dialogue box (click on Close) or Method property sheet (click on Cancel) if either was opened automatically. 2. Click on Help on the menu bar to open the Help menu. 3. Click on Help Topics to display the SOLAAR Help dialogue box. 4. If necessary, click on the Contents tab to display the Contents page: 3-16 SOLAAR Series Software Manual

49 On-line Help The Help Topics: SOLAAR dialogue box has three pages you can use: the Contents page to view a structured list of the main topics in the Help system so that you can select the topic giving the information you need. The topics in the list are grouped together in books. To open a book, simply slick on the relevant book. To display a Help topic from the Table of Contents, click on the topic. See the next section for a description of the structure of the Contents table. the Index page to find a topic using a keyword. the Search page to search the text in the Help system for a particular word or phrase. If you need Help in using the Index and Find pages, consult the Windows On-line Help for using Help (see the SOLAAR Software / On-line Help / Learning to use the on-line help system section) or the context-sensitive Help on those pages (see the SOLAAR Software / Online help / Context-sensitive help section). SOLAAR Help Table of Contents and Help topics The topics in the On-line Help system are grouped into five sections: Overviews these topics provide brief descriptions of the major features of the software. How to these topics provide detailed, step-by-step instructions for carrying out everyday tasks with SOLAAR. Troubleshooting these topics help you to identify and correct common problems experienced when making Atomic Absorption spectrometry measurements. Cook Book these topics give summaries of the instrumental parameters, performance figures and known interferences for all the elements that can be measured by your SOLAAR Atomic Absorption system. Application Notes this link provides access to a large library of applications support documentation. It is highly recommended that new users, or experienced users analysing an unfamiliar sample, should look through this information. Many of the Help topics contain underlined phrases. These underlined sections provide links to related topics. For example, many of the Overview topics provide links to How to topics showing how a particular software feature is used to carry out a task and many of the How to topics have links to relevant overviews. Troubleshooting topics also contain links to other Troubleshooting topics to guide you through the troubleshooting procedure and to How to topics that can provide solutions to the problems. SOLAAR Series Software Manual 3-17

50 On-line Help Some words or phrases in a topic may be underlined and coloured: When you move the pointer over these it changes to a pointing hand: When you click on an underlined phrase you may be taken directly to another topic or presented with a list of topics within a pop-up box, for example: 3-18 SOLAAR Series Software Manual

51 On-line Help There is one more type of link you will find in the Help system. A few topics have pictures that have links built in to them. For example, the Status Bar topic has a picture of the Status Bar. When you move the pointer over these pictures, the pointer again changes to a pointing hand showing that they contain links. If you click on the picture, Help for the item clicked on will be displayed in a pop-up window. Context-sensitive Help When you are using the program you may come across a feature that you are not sure how to use, such as a Tool Bar tool or a menu command, a control in a dialogue box, or even a whole dialogue box, or Status window. When this happens you can use Context-sensitive Help to display specific help for the item. There are several different ways to display Context-sensitive Help, depending on the type of item for which you need Help and, to some extent, personal preference. The following paragraphs describe how to display Context-sensitive Help in different circumstances. Menu Commands, Status windows and Tools To display Context-sensitive Help for items in the main program window (Menu Commands, Status windows and Tools): 1. Click on What s This? in the Help menu or click on the What s This? button in the Tool Bar. The pointer will change to the Help pointer: 2. Use the pointer to click on the Tool or Status window or select the command. Help for the selected item will be displayed in a pop-up window or one of the main Help windows. Some of the pop-up Help topics have underlined, coloured phrases, which you can click to close the pop-up and display further Help in one of the main Help windows. Otherwise, to close a pop-up window, click anywhere. You can also display the Context-sensitive Help for a: Status window by selecting it and pressing F1 on the keyboard Menu command by clicking on the menu in the Menu Bar to display it, moving the pointer over the command, pressing (but not releasing) the mouse button and then pressing F1 on the keyboard. Note: As well as the Help described above, brief help is given in the Status Bar when you move the pointer over a tool or menu command. You can also get Tool Tip Help for the Tool Bar tools by moving the pointer over the tool button and waiting for a few seconds the name of the button will be displayed in a popup. SOLAAR Series Software Manual 3-19

52 On-line Help Dialogue boxes and Property pages To display Context-sensitive Help for a dialogue box or Property page: 1. Open the dialogue box or the property sheet and tab to the relevant property page. 2. Click on the Help button. Help for the dialogue box will be displayed in one of the main Help windows. Note: The function of some simple dialogue boxes is selfexplanatory, so they do not have Help buttons. Controls on dialogue boxes and Property pages To display Context-sensitive Help for a control on a dialogue box or Property page (for example, a text box for entering data, a check box, a radio button or a push button): 1. Click on the What s This? Help button at the top right-hand corner of the dialogue box to change the pointer to the contextsensitive Help pointer: 2. Click on the control in the dialogue box for which you want help. The Help will be displayed in a pop-up window. Some of the pop-up Help topics have underlined, coloured phrases, which you can click to close the pop-up and display further Help in one of the main Help windows. Otherwise, to close a pop-up window, click anywhere. You can also display this Context-sensitive Help by selecting the control (you can select a button control without pressing it by moving the pointer over the button, pressing the mouse button but not releasing it until you have moved the pointer off the button) and pressing F1 on the keyboard SOLAAR Series Software Manual

53 Chapter 4 Getting Started SOLAAR Series Software Manual 4-1

54 A simple flame analysis This page is intentionally blank. 4-2 SOLAAR Series Software Manual

55 A simple flame analysis A simple flame analysis Before starting Setting up the Method This section will guide you through the process of setting up and performing a simple flame analysis for copper. Before starting, make sure that your AA Series Spectrometer system has been correctly installed and tested, and that the various services are correctly connected. To carry out a simple flame analysis you have to: set up a Method and, optionally, save it in the Methods database. install a hollow cathode lamp. light a flame. optimise the burner and nebuliser impact bead positions. You can then run the analysis, view the results and finally print a Report of the results. To work through the example described below, you will need: a copper hollow cathode lamp. three copper standard solutions containing 1.00, 2.50 and 5.00 mg/l of copper in 0.1% v/v nitric acid. sample solutions containing unknown copper concentrations in the range 0 5 mg/l of copper. a blank solution containing 0.1% v/v nitric acid. deionised water. Refer to the safety notices dealing with flame operation in the operator manual and ensure that you understand the hazards involved and the precautions necessary. Flame analyses are always carried out in the left-hand sample compartment of dual atomiser spectrometers. Start the SOLAAR software and log in as described in the SOLAAR Installation / Starting the SOLAAR Application and SOLAAR Installation / Logging in to SOLAAR Software sections. Close the Wizards dialogue box if necessary. You will set up the Method using the Method property pages provided on the Method property sheet. For this analysis you will use the default values for the most of the parameters, then save the Method in the Methods database. To display the Method property sheet so that you can set up the method: 1. Click on the Show Method button to open the Method property sheet. The following subsections describe how to set the parameters on each of the pages in the Method property sheet. SOLAAR Series Software Manual 4-3

56 General Method parameters General Method parameters To set general analysis parameters for the method: 1. If the General Method property page is not displayed, click on the General tab: 2. Click on the New button to create a new Method. The Element dialogue will be displayed: 3. Select Cu from the Periodic Table and confirm that the Technique is set to Flame. Click OK to close the dialogue and return to the General page of the Method. 4. Type in a Method Name for the Method. 4-4 SOLAAR Series Software Manual

57 General Method parameters 5. If required, edit the name in the Operator field it shows the name of the logged in user by default. 6. Type a description of the analysis in the Description field. 7. Set the remaining controls to the following values: Segmented Flow Injection = unchecked Autosampler = None Rack Code = this is disabled when Autosampler is set to None Flame Dilution = None Shared Standards = unchecked Sequence Method parameters You can specify the element for which you want to run the analysis and the actions to be carried out during the analysis on the Sequence page. 1. Click on the Sequence tab to display the Sequence Method property page: The first (and only) element column will now show Cu and there will be a Cu element button on the right-hand side of the property page the element buttons are used to switch the property pages to different sets of parameters in multi-element methods. The next step is to define the sequence of actions that will be carried out during the analysis. SOLAAR software offers you two methods of doing this a) You can define the sequence before you start the analysis. This is the most convenient method when you know how many SOLAAR Series Software Manual 4-5

58 MethodsGeneral Method parameters samples you want to analyse and you wish to repeat certain actions at regular intervals throughout the analysis. This is also the only method that can be used with an autosampler. b) You can define an initial action (usually a calibration), then later define subsequent actions while the method is running. This is convenient for manually analysing small numbers of samples, but does not allow the full range of actions to be used. For this experiment you will use the first method and define the sequence fully before you run the analysis. When you create a new Method the default sequence contains a single calibration action in the first position in the sequence. 2. Right-click in the second row of the sequence grid to pop-up the sequence context menu and click on Insert Action to display the Insert Action dialogue box: 3. Leave Sample(s) selected and set the Number of Samples field to the number of samples you have prepared use a minimum of Click on OK to close the Insert Action dialogue box and return to the Sequence Method property page. 4-6 SOLAAR Series Software Manual

59 General Method parameters Four Sample actions will now appear in rows 2 to 5 of the sequence grid. They will be given the default Solution IDs Sample ID 1, Sample ID 2 and so on: The next step gives you the opportunity to give the samples your own Solution IDs. If you do not want to do this you can go straight to the next set of instructions. 5. Click on Sample Details to display the Sample Details dialogue box: a. Click on the name in the first cell of the Sample ID column to place an editing caret, then edit the name or delete it and type a suitable name for the first sample. Note: The Sample Mass, Dilution Ratio and Nominal Mass fields allow you to specify factors that SOLAAR will use to calculate a corrected concentration. However, we will not use this feature in this experiment see the Help system if you want to learn how to use it. You can repeat Step a. for the other samples, but the remaining steps show how SOLAAR provides a shortcut if you just want to use the same root name for all the samples with an increasing number to distinguish them. b. Click in the first row and then SHIFT-click in the last row to select all the rows. SOLAAR Series Software Manual 4 -

60 General Method parameters Note: You can also select a range of rows by dragging or all the rows by clicking in one of the headings. c. Right-click in the grid to pop up the Sample Details context menu. d. Click on Clone Details to display the Duplicate Sample Details dialogue box. e. Check Duplicate Sample Identifier this enables Auto Increment ID. f. Check Auto Increment ID. g. Click on Copy to close the Duplicate Sample Details dialogue box and return to the Sample Details dialogue box. The first sample name will be copied to the other samples, with the last digit in the name automatically incremented to all the selected samples: 6. Click on OK in the Sample Details dialogue box to confirm the settings, close the dialogue box and return to the Sequence Method property page. You have now completed all the necessary tasks on the Sequence page. You will next display the Spectrometer Parameters page and set up the 4 - SOLAAR Series Software Manual

61 Spectrometer Method parameters Spectrometer Method parameters Spectrometer Parameters for your analysis. To view the Spectrometer parameters for copper analysis in the method: 1. Click on the Spectrometer tab to display the Spectrometer property page: 2. Confirm that the Measurement Mode is set to Absorption and that all the other settings are also set to their default values, as in the picture above. 3. Click on Cook Book to display a Help window with the Cook Book information for copper. Note: The Cook Book will stay open through the following steps unless you open another Help page. However, it may become hidden by the program window. If it does you can bring it back to the top by clicking on its icon in the Windows Task Bar, or by pressing ALT+TAB repeatedly until it is selected. You have now completed all the necessary tasks on the Spectrometer page. The next step is to set the Flame Parameters for the analysis. SOLAAR Series Software Manual 4 -

62 Flame Method parameters Flame Method parameters To view the Flame parameters for the method: 1. Click on the Flame tab to display the Flame property page: 2. Review the default parameters, but do not change any at this stage. You have now completed all the necessary tasks on the Flame Parameters page. The next step is to set up the Calibration Parameters for the analysis. Calibration Method parameters To set the Calibration parameters for the method: 1. Click on the Calibration tab to display the Calibration property page: 2. Confirm that the Calibration Method is set to Normal Segmented Curve Fit. 3. Confirm that the Concentration Units field shows mg/l. 4. Set the Number of Standards to 3 the first three fields in the Standard Concentrations table will become enabled SOLAAR Series Software Manual

63 Saving and loading Methods 5. Set the first three fields in the Standard Concentrations table to the concentration values of the standard solutions you have prepared. 6. Confirm that the other calibration parameters are set to their default values, as in the picture above. You have now completed all the necessary tasks on the Flame Parameters page Since we have not included any QC Test actions in the sequence, the settings on the QC Method property page are irrelevant and your Method is now complete. When you close the Method property sheet the method you have defined will become the Current Method, which will be used when you next run an analysis. However, you can also save the Method in the Methods Library so that you can load it again later after you have defined other Methods. You do this using the General Method property page, so don t close the Method property sheet yet. Saving and loading Methods Saving a Method in the Methods Database The Method you have defined will remain as the Current Method until you edit it, load a saved Method or create a new Method. This means that it doesn t matter if you have closed the Method property sheet before saving the Method if you open the Method property sheet again it will show the settings you made before closing it. Note: A default Methods database is created for you when the software is installed, but you can set up as many different Methods databases as you require. For further information open the SOLAAR On-line Help Contents window and view the SOLAAR How to work with Methods To work with Methods databases topics (this list shows the Help contents books you need to open to find the topics). 1. Click on the General tab to display the General property page: SOLAAR Series Software Manual 4-11

64 Installing a lamp 2. Click on Save. 3. You will be asked to confirm that you want to save the Method in the database using the name in the Method Name box: 4. Click on Yes to save the Method and close the dialogue box and return to the General Method property page. 5. Click on OK to close the Method property sheet. Note: When you save the Method a new record is created for it in the SOLAAR Methods Database it is not saved as a separate file. The record is identified by the Method name and by the date and time it was saved. This means that you do not need to give the Method a unique name; though in practice this will make identifying the Methods easier at a later date if you do give them unique and meaningful names. Loading a previously saved Method Installing a lamp 1. Click on the Methods button or click on Method in the Edit menu to open the Method property sheet at its General property page. 2. Click on Load to display the Method Library dialogue box. This lists the Methods saved in the Methods database. 3. Click on the required Method in the list the description entered when you created the Method will be shown in the Description box to help you identify the Method. 4. Click on Load to close the dialogue box and load the Method. To perform any atomic absorption analysis, you must first install a hollow cathode lamp in the Spectrometer. The procedure below describes the installation of a Thermo Scientific coded hollow cathode lamp. Refer to the How to section of the On-line Help system to learn how to install other types of lamps. To install the hollow cathode lamp: 1. Check the Status Bar and confirm that the Data Station is ON LINE with the Spectrometer SOLAAR Series Software Manual

65 Installing a lamp If the Status Bar says OFF LINE, click on Connect in the Action Communications submenu. 2. Click on the Lamps button or click on Lamps in the Edit menu to open the Lamp Configuration and Status dialogue box. 3. Select the Carousel Position that you want to use for the lamp and make sure that Automatic Lamp Alignment is checked. 4. If there are any lamps fitted already and their State is On, click in their State boxes to set them to Off. 5. Refer to the Hardware manual and remove any lamps fitted. 6. Fit the new lamp. If you are using an uncoded lamp, you will need to define its characteristics. For details, open the On-line Help Contents window and view the SOLAAR How to work with lamps To install Hollow Cathode Lamps topic. 7. Confirm that: the element(s) in the lamp are displayed in the Element field. the Type field shows Coded or Uncoded as appropriate. the Max Current field shows the maximum current marked on the lamp. SOLAAR Series Software Manual 4-13

66 Installing a lamp SOLAAR can monitor and record the usage of your lamps. To do this, you must register the lamp s Serial Number in the Lamps database, so that SOLAAR can identify which lamps are being used. The next steps show you how to do this. Go to Step 16 if you do not want to register the lamp. 8. Click on Lamp Usage to display the Lamp Usage dialogue box: 9. Click on Add Lamp to display the Add Lamp Serial Number dialogue box: 10. Click in the Element(s) box to display the Lamp Elements dialogue box: 11. Click on the lamp s elements in the periodic table to select them. You can select more than one element by clicking on them in turn. If you accidentally select an incorrect element, click on it again to deselect it SOLAAR Series Software Manual

67 Setting up the lamp 12. Click on OK to close the dialogue box and return to the Add Lamp Serial Number dialogue box. 13. Enter the lamp s Serial Number. 14. Click on Add to close the Add Lamp Serial Number dialogue box and return to the Lamp Usage dialogue box. The new lamp will be added to the list of lamps showing its Element(s) and Serial Number as it is a new lamp the usage (ma Hours) will be Click in the new lamp s row to select it and click on Close to close the Lamp Usage dialogue box and return to the Lamp Configuration and Status dialogue box. The Lamps grid will show the selected Serial Number with 0 ma Hours. 16. Click in the State field for the new lamp to set it to On and confirm that the lamp has come on. 17. Click on OK to close the Lamp Configuration and Status dialogue box. The hollow cathode lamp is now installed and ready to be aligned with the Spectrometer optical system. Setting up the lamp All Thermo Scientific AA Series spectrometers provide automatic lamp alignment facilities. Before setting up the lamp, check the Spectrometer Sample Compartments to confirm that the optical path is clear of obstructions. We recommend that you remove any Sample Compartment accessories before attempting to align a hollow cathode lamp. 1. Set up a Method using the default parameters for copper as described above, or load the previously saved Method. 2. Click on the Lamp button or click on Lamps in the Edit menu to open the Lamp Configuration and Status dialogue, and confirm that the Automatic Lamp Alignment checkbox is checked. 3. Click on the Optical Setup button. confirm that the System Status changes to BUSY during the optical setup. provided that Automatic Lamp Alignment is checked in the Lamp Configuration and Status dialogue box, the lamp will be aligned automatically as part of the setup procedure. when the optical setup is finished, the System Status will return to ON LINE. The lamp is now aligned and ready for use. SOLAAR Series Software Manual 4-15

68 Lighting the flame and optimising the burner parameters Lighting the flame and optimising the burner parameters It is good practice to optimise the burner position and the nebuliser impact bead before starting work. The Optimise burner and nebuliser positions wizard can help you to do this. The best procedure to follow is to light the flame, then aspirate a test solution and monitor the absorbance signal while adjusting the burner position and impact bead controls to obtain the maximum possible signal. Before lighting the flame, you must first check that: an intact explosion disk is fitted in the back of the spray chamber. the correct gases are: connected to the Spectrometer. set to the correct pressures. the drain trap is full. the drain is flowing freely. the burner is clean and fitted correctly. the Spectrometer Sample Compartment door is fitted and closed. Refer to the Hardware manual to learn how to carry out these checks and note the relevant safety warnings. Lighting the flame To light the flame: 1. Set up a Method using the default parameters for copper as described above, or load the previously saved Method. 2. Check the Flame Status Bar at the bottom of the screen and: confirm that the burner is Present and that the correct Burner Type is displayed. confirm that the Gas Pressures for the necessary gases are OK. 3. Confirm that the IGNITE switch on the Spectrometer front panel is flashing. 4. Press and hold the IGNITE switch until the flame is established. 5. Confirm that the Flame Status Bar displays are updated. 6. Click on the Flame Setup button to set up the flame parameters specified in the Method. The flame is now established. It is good practice to aspirate deionised water through the flame system while a flame is burning. So when the flame is established you should place the nebuliser capillary tip into a container of deionised water. It is important to allow the burner to warm up and stabilise before taking measurements, but the alignment procedure below can be carried out after a few minutes SOLAAR Series Software Manual

69 Lighting the flame and optimising the burner parameters Optimising the burner position You will need: a test solution containing the appropriate analyte at a concentration of x the characteristic concentration given in the Cookbook. The 5.00 mg/l copper standard solution mentioned above will be suitable. WARNING. Do NOT attempt to carry out this task while a nitrous oxide-supported flame is burning. To set up the burner and nebuliser: 1. Set up a Method for flame copper analysis using the default parameters. Set up the optics and light the flame as described above. 2. Open the Spectrometer Status window and confirm that the absorbance signal display is active. 3. Aspirate deionised water. 4. Click on the Autozero button and confirm that the absorbance display shows ± Aspirate the test solution. 6. Refer to the Hardware manual and: open the Sample Compartment door. locate the burner position adjustment controls. adjust the angular and transverse positions of the burner to obtain the maximum absorbance signal from the test solution. after each adjustment, aspirate the blank solution and autozero the instrument. locate the impact bead adjustment control. adjust the control to move the impact bead back towards the nebuliser as far as it will go. the absorbance signal will decrease. carefully adjust the control to move the impact bead away from the nebuliser until the signal reaches a maximum. close the burner compartment door. 7. Click on Burner Height on the Action Optimise submenu to optimise the burner height automatically the Burner Height Graph window will show the optimisation results as they are produced. The burner and nebuliser system is now correctly adjusted and the Spectrometer is ready to make measurements. Turn off the flame until you are ready to carry out the analysis. The Optimise burner and nebuliser positions wizard can also be used. SOLAAR Series Software Manual 4-17

70 Running the analysis Running the analysis Before running the analysis you should install and align the lamp, and set up and optimise the burner and nebuliser as described above. The analysis uses the Current Method you can see the definition of the Current Method by opening the Method property sheet. If you do not want to use this method, use the Method property sheet to define the required Method or to load a previously saved one. Before starting, turn on the lamp and light the flame. Aspirate deionised water for at least ten minutes to allow the instrument to warm up and stabilise. Ensure that your blank, standard and sample solutions are available and clearly labelled. To run the flame analysis: 1. Open the Results window so that you can see your results as they are measured, and the Calibration window to see the calibration plot as it is built up from the standard solution results. 2. Click on the Analyse button to display the Start Analysis dialogue box: 3. Type in an Analysis Name for the analysis this will be used to identify the results. 4. If required, edit the name in the Operator field it shows the name of the logged in user by default. 5. Type any notes that you want to save with the results of the analysis in the Analysis Notes field. 6. Click on Analyse to start the analysis and confirm that: the System Status shown on the right of the Status Line changes to BUSY while the Spectrometer is set up SOLAAR Series Software Manual

71 Running the analysis 7. As the analysis proceeds you will be prompted to aspirate the solution required for each stage, for example: or for samples: (This dialogue box allows you to set or edit the Sample Details as the analysis is run.) Aspirate each solution as you are prompted and click on OK. The solution will be measured, and the result will appear on the Results window. 8. When all the solutions have been measured, a prompt will be displayed for you to specify your next action: Select the Stop action by clicking on the Stop button. the System Status changes to ON LINE. You have now carried out a simple flame analysis. SOLAAR Series Software Manual 4-19

72 Viewing the results Viewing the results When you run an analysis the results are saved automatically in the Results database. You can view any or all of the results stored in the database in the Results window in any combination. However, when you run an analysis SOLAAR automatically restricts the results shown in the Results window to the results for the current analysis (this is the default; if you wish you can add results from other analyses as the current analysis is running). To view the results of your analysis: 1. Open the Results window the mean results for each solution will be displayed in the upper table: Note: SOLAAR allows you considerable flexibility in choosing what data to show in the Results table so your results window may not be the same as in the example picture see the Help system for details. 2. Use the scroll bar to the right of the upper table to scroll through the results. 3. To display the resample results for a sample, click on its mean result in the upper table its resamples will be displayed in the lower table. 4. Open the Calibration window. Confirm that the calibration graph is displayed in the upper part of the window and the Calibration Details are displayed in the lower part of the window SOLAAR Series Software Manual

73 Printing the results Printing the results Before printing from the SOLAAR application, ensure that your printer is correctly installed in Windows, that it is turned on and that it is loaded with paper. Make sure that the printer is ready to accept data most printers have an indicator labelled ON LINE, which should be illuminated. You can print results at any time, even while another analysis is in progress. Note: Printed SOLAAR Reports contain details of the results currently displayed in the Results window. Immediately after you have run an analysis these will just be the results for that analysis, which is what we want for this example. However, you can click on Options in the Results menu to display the Results Display Options dialogue box to select which results to include from the whole Results database see the Help system for details. To print a Results Report: 1. Click on Print Setup on the File menu to open the Print Setup dialogue box, then: a. make any necessary changes to the parameters displayed in the dialogue box to match those of the printer that you want to use. b. Click on OK to close the Print Setup dialogue box. 2. Click on Print Options on the File menu to display the Report Printing Options dialogue box: 3. Click on the options that you want to use and click on OK to close the dialogue box. 4 Either: a. Click on Results in the File Print Preview menu, to check that the Report contains the information that you want to print. b. Click on the Print button on the top left corner of the Print Preview display to print the Report as it is shown, or click on Close to return to the normal display. or Click on Results in the File Print menu to send the report to the printer. Your report containing the results of the analysis will be printed. SOLAAR Series Software Manual 4-21

74 A simple furnace analysis A simple furnace analysis This section will guide you through the process of setting up and performing a simple graphite furnace analysis. This is in many ways similar to setting up a flame analysis and we suggest that you first read Section 2.1 above, if you have not already done so. To carry out a simple furnace analysis, you must: set up a Method install and align a hollow cathode lamp install and align the Graphite Furnace install and align the Graphite Furnace Autosampler load the sample solution into the Autosampler. You can then run the analysis, save the results and print a Report of the results. To work through the example described below, you will need: a manganese hollow cathode lamp three manganese standard solutions containing 1.0, 5.0 and 10.0 µg/l of manganese in 0.1% v/v nitric acid sample solutions containing unknown manganese concentrations in the range 0 10 µg/l of manganese a blank solution containing 0.1% v/v nitric acid a ridged, coated cuvette for the Graphite Furnace. It is usually accepted that the use of an Autosampler for Graphite Furnace analysis is essential to make full use of the capabilities of modern furnace designs. We have assumed in the following section that a Furnace Autosampler is available. There are a range of Graphite Furnace systems available for Thermo Scientific AA Spectrometers. Although the furnaces differ in mechanical design, the principles involved in using them and the software that controls them are identical. The Hardware manual covers the details of the mechanical controls of all designs of furnace. Before starting Check that your AA Spectrometer system, Graphite Furnace accessory and Furnace Autosampler have been correctly installed, and that the necessary services are correctly connected and adjusted to their normal operating conditions. Graphite Furnace Atomic Absorption Spectrometry is an inherently safe procedure, as no inflammable or explosive gases are used. However, you should still review the appropriate sections of the Hardware manual and ensure that you understand the hazards involved and the precautions necessary. Graphite Furnace analyses are always carried out in the left-hand sample compartment of dual atomiser spectrometers. Start the SOLAAR application, and log in as described in the SOLAAR Installation / Starting the SOLAAR Application and SOLAAR Installation / Logging into SOLAAR sections SOLAAR Series Software Manual

75 A simple furnace analysis Setting up the Method General Method parameters Set up the Method using the Method property pages provided on the Method property sheet. For this example analysis you will use the default values for most of the parameters, then save the Method in the Methods database. To set up the furnace Method: Click on the Methods button to open the Method property sheet. The following subsections describe how to set the parameters on the Method property sheet pages. To set general analysis parameters for the method: 1. If the General Method property page is not displayed, click on the General tab. 2. Set the Technique to Furnace: 3. Type in a Method Name for the analysis Method. 4. If required, edit the name in the Operator field it shows the name of the logged in user by default. 5. Type a description of the analysis in the Description field. 6. Set the remaining controls to the following values: Autosampler = Furnace Rack Code = this is disabled when Autosampler is set to Furnace Shared Standards = Checked SOLAAR Series Software Manual 4-23

76 Sequence Method parameters Sequence Method parameters Spectrometer Method parameters The next step is to specify the element for which you want to run the analysis, the actions to be carried out during the analysis and the Sample Details. You do this in exactly the same way as for a Flame Method. See the instructions for setting the Sequence Method parameters in Section and set up a Sequence for a manganese analysis containing a Calibration action, and at least three Sample Actions. Additional actions are available for you to use in a Furnace Method. In particular, it is good practise start the Action List with a Cuvette Clean action, which will cause a Cuvette Clean cycle to be run automatically before making any measurements. This will ensure that the cuvette is clean and that the components in the Graphite Furnace have reached their normal operating temperatures. To view the Spectrometer parameters for manganese analysis in the method: 1. Click on the Spectrometer tab to display the Spectrometer property page: 2. Confirm that the Background Correction technique is set to D2 Quadline. 3. Confirm that the other settings are set to their default values, as in the picture above. 4. Click on Cook Book to display a Help window with the Cook Book information for manganese SOLAAR Series Software Manual

77 Calibration Method parameters Furnace Method parameters To view the Furnace parameters for the method: 1. Click on the Furnace tab to display the Furnace property page: 2. Review the default parameters, but do not change any at this stage. Calibration Method parameters To set the Calibration parameters for the method: 1. Click on the Calibration tab to display the Calibration property page: 2. Confirm that the Calibration Method is set to Normal Segmented Curve Fit. 3. Confirm that the Concentration Units field shows µg/l. 4. Set the Number of Standards to 3 the first three fields in the Standard Concentrations table will become enabled. 5. Set the first three fields in the Standard Concentrations table to the concentration values of the standard solutions you have prepared. 6. Set the Master Standard Conc: field to the concentration of your top standard. 7. Confirm that the other calibration parameters are set to their default values, as in the picture above. SOLAAR Series Software Manual 4-25

78 Sampling Method parameters Sampling Method parameters To set the Sampling parameters for the method: 1. Click on the Sampling tab to display the Sampling property page: 2. Set the Working Volume to 10.0 µl. 3. Confirm that the other Sampling parameters are set to their default values, as in the picture above. Note: Since we have not included any QC Test actions in the sequence, the settings on the QC Method property page are irrelevant. Installing and aligning the lamp This completes the definition of the Method see Getting Started / A Simple Flame Analysis / Saving and Loading Methods Section for how to save the Method in the Methods database. Ensure that the optical path in the left-hand (flame) sample compartment of your dual atomiser instrument is clear. If you have a tilt mounted furnace you can ensure that the optical path in the righthand compartment is also clear while aligning the lamp by tilting the Furnace Head forward towards the front of the instrument. If you have a furnace on the fixed mount, confirm that a cuvette is correctly fitted and that the furnace windows are clean. If you have a single atomiser instrument, the combined Autosampler and Furnace System will be fitted in the sample compartment. If you are not confident that the alignment of the Furnace is approximately correct, remove the furnace before attempting to align the lamp. Refer to the Operators Manual for instructions as to how to do this. See Getting Started / A Simple Flame Analysis / Installing the Lamp and Getting Started / A Simple Flame Analysis / Setting up the lamp sections for how to install and align the hollow cathode lamp SOLAAR Series Software Manual

79 Installing and aligning the Graphite Furnace Installing and aligning the Graphite Furnace Aligning the Graphite Furnace Autosampler Your Furnace system will have been installed on to your dual atomiser Spectrometer by the Thermo Scientific Service Engineer. When the Furnace on a dual atomiser instrument has been installed in the Spectrometer, it will have been aligned with the optical system. Once aligned, the Furnace should not go out of alignment during normal use. However, you may have cause to remove the Furnace to use another accessory in the Right Hand Sample compartment of the spectrometer. You can remove and refit the Furnace System without losing the alignment; nevertheless, it is good practice to check the alignment at regular intervals. A trained Service Engineer will install and align the Furnace system on your single atomiser instrument. You can remove and refit the Furnace System without losing the alignment; nevertheless, it is good practice to check the alignment at regular intervals. Alignment procedures for all types of Furnace system are provided in the Operators Manual. You must align the Graphite Furnace Autosampler so that the capillary tip enters the injection hole in the cuvette vertically, without touching the sides of the injection hole. This adjustment may have been set up on installation, however you should check it at regular intervals and whenever you change the autosampler Capillary Tip. You must then set the vertical position of the tip inside the cuvette, so that the sample solution is deposited correctly on to the floor of the cuvette. The GFTV accessory will greatly simplify this process. If this is not available you can use a small dental mirror, positioned to the right of the furnace head, to view the capillary tip inside the cuvette. You will need: either: the GFTV accessory fitted, or a small dental mirror. a small torch or desk lamp positioned over the furnace head will also be useful if the lighting is poor. Before starting to align the Autosampler, you should: install and align a hollow cathode lamp. install and align the Graphite Furnace in the Spectrometer. install and align a cuvette. check that the communications, power, cooling and gas supply services are properly connected to the Graphite Furnace. SOLAAR Series Software Manual 4-27

80 Aligning the Graphite Furnace Autosampler To align the Graphite Furnace Autosampler: 1. Check the Status Line and confirm that the System Status is ON LINE. 2. Refer to the Hardware Manual and: a. Fit the Autosampler to the Spectrometer and locate the position adjustment controls. b. Confirm that the capillary tip is fitted correctly and is not bent. c. Confirm that the electrical and gas connections are correct. d. Confirm that the Autosampler wash reservoir is full. 3. Click on the Methods button to open the Method property sheet at its General page dialogue box and confirm that the Autosampler is set to Furnace (this may differ depending upon your instrument type). Close the Method property sheet. 4. Click on the Align Capillary Tip button to move the Autosampler arm into position over the furnace head. 5. Adjust the position of the Autosampler until the capillary tip enters the cuvette injection hole. 6. To adjust the height of the capillary tip until it is just above the cuvette ridges: either Position the dental mirror to the right of the furnace head, to view the reflected image of the capillary tip inside the cuvette. or a. Click on the GFTV button to display the GFTV dialogue box: b. Set the Camera Mode to Analysis. c. Click on OK to display the GFTV image (note: the GFTV image appears in the Spectrometer Status window. You must have this window open to view the GFTV video): d. Finally, optimise the height of the capillary tip by observing a sample injection and adjusting the height to obtain a smooth, complete deposition of the sample in the bottom of the cuvette SOLAAR Series Software Manual

81 Aligning the Graphite Furnace Autosampler You have now correctly aligned the Furnace Autosampler. It is good practice to purge the Autosampler after fitting and aligning it, to remove any contamination from the capillary tip and ensure that there are no bubbles trapped in the liquid handling system. To purge the Autosampler: Click on the Autosampler Purge button. It will take approximately two minutes to purge the Autosampler. The System Status will be BUSY while the Autosampler is being purged and will return to ON LINE when the purge has finished. Loading the sample solution on to the Autosampler After you have defined a Method, SOLAAR determines the default positions for the solutions on the Autosampler. You can find out what these are using the Autosampler Loading Guide, usually abbreviated to ASLG. If you need to change the positions of any samples or standards you can simply drag them from their original place on the schematic of the autosampler (right-hand side of the screen), and drop them in a new location. The list view on the left-hand side of the screen will automatically update as you modify the locations of samples, standards or blanks. To look at the Autosampler Loading Guide: Click on ASLG in the View menu: Note: You can also open the Autosampler Loading Guide by clicking on ASLG on the Sequence property page of the Method property sheet. To print the Autosampler Loading Guide: Click on the Print command on the File menu and then click on Autosampler Loading Guide. Refer to the Autosampler Loading Guide and place your solutions in sample cups in the correct positions on the Autosampler carousel, then replace the carousel on the Autosampler. SOLAAR Series Software Manual 4-29