AA83501-00 OPERATOR MANUAL WINXRF V3.0-1 AA83501-00 Report MANUAL No AA83501-00 Language E Date May 2001 Department R&D Author R&D AA83501-00 The information in this document is subject to change without notice. ARL assumes no responsibility for any errors that may appear in this document. Die Angaben in diesem Dokument knnen ohne vorherige Information gendert werden. ARL bernimmt keine Verantwortung fr eventuelle Mngel in diesem Dokument. Les informations contenues dans ce document sont sujettes changement sans pravis. ARL nassume aucune responsabilit pour toutes erreurs ventuelles contenues dans ce document. LARL si riserva il diritto di modificare le informazioni contenute nel presente manuale senza preavviso e non assume alcuna responsabilit quanto ad eventuali errori che potrebbero esservi accidentalmente introdotti. Las informaciones contenidas en este documento pueden ser modificadas sin previo aviso. ARL declina toda responsabilidad sobre los eventuales errores contenidos en este documento. PAGE DE MODIFICATION NDERUNGSANGABEN REVISION CONTROL SHEET AA83501-00 Date Datum Date Modification nderung Revision Description Beschreibung Description
TABLE OF CONTENT
Table of Content AA83501 WinXRF Operator Manual I 1 GETTING STARTED............................................................................... 1-1 INTRODUCTION..................................................................................................... 1-1 WINXRF SOFTWARE DOCUMENTATION............................................................ 1-2 Summary of the Operator Manual ....................................................................... 1-2 SOFTWARE INSTALLATION.................................................................................. 1-4 Installation of the Documentation from CD-ROM................................................ 1-5 General Comments......................................................................................... 1-5 Starting the Installation Program..................................................................... 1-5 Installation of the Acrobat Reader................................................................... 1-5 Installation of the Documentation Manuals ..................................................... 1-7 Viewing or Printing the Documentation ............................................................... 1-9 LOGGING INTO WINXRF..................................................................................... 1-12 Password Protection ......................................................................................... 1-15 INSTRUMENT INITIALISATION............................................................................ 1-16 Spectrometer Environment................................................................................ 1-18 Zero Goniometer ............................................................................................... 1-19 X-Ray Tube Conditions ..................................................................................... 1-19 INSTRUMENT SUPERVISION.............................................................................. 1-21 Display Instrument Status ................................................................................. 1-21 Instrument Alarms ............................................................................................. 1-21 INSTRUMENT COMMUNICATION....................................................................... 1-23 Reset Instrument ............................................................................................... 1-23 Abort Instrument Operations ............................................................................. 1-25 WINXRF MENU STRUCTURE.............................................................................. 1-27 Display Modes................................................................................................... 1-27 Icons of the Function Frame.............................................................................. 1-30 Home............................................................................................................. 1-31 Layout ........................................................................................................... 1-31 Exit ................................................................................................................ 1-31 About............................................................................................................. 1-31 Log Off .......................................................................................................... 1-31 Working with Shortcuts...................................................................................... 1-32 2 QUALITATIVE ANALYSIS...................................................................... 2-1 INTRODUCTION..................................................................................................... 2-1 RUNNING A SCAN.................................................................................................. 2-1 On-Line Scanning................................................................................................ 2-2 STARTING SCAN GRAPHICS................................................................................ 2-4 Explanation of the Scan Graphic Functions ........................................................ 2-5 How to use the Mouse in Scan Graphics .......................................................... 2-10 Scan Identification............................................................................................. 2-11 Table of Content WinXRF Operator Manual AA83501 II Manual Scan Identification............................................................................ 2-11 Show Element...................................................................................................................... 2-11 Peak Identification ............................................................................................................... 2-12 Automatic Scan Identification........................................................................ 2-13 Automatic Identification on displayed Scans ....................................................................... 2-14 Unattended Scan Identification............................................................................................ 2-14 Adding Special Identifications ....................................................................... 2-15 Other Scan Graphic Editing Features................................................................ 2-16 Zooming of Scan Graphs .............................................................................. 2-16 Adding Graph Labels .................................................................................... 2-17 Moving Tags and Graph Labels .................................................................... 2-18 Moving Identification Bars ............................................................................. 2-18 Z Scale.......................................................................................................... 2-20 Differential Graph.......................................................................................... 2-21 Peak Resolution............................................................................................ 2-22 Spectra Interpretation........................................................................................ 2-24 3 SEMI-QUANTITATIVE ANALYSIS.......................................................... 3-1 INTRODUCTION..................................................................................................... 3-1 QUANTAS ............................................................................................................... 3-1 Performing Analyses with QuantAS .................................................................... 3-1 Single QuantAS Analysis ................................................................................ 3-1 Multiple QuantAS Analyses............................................................................. 3-5 Interactive QuantAS Analysis.............................................................................. 3-5 Set up QuantAS Standards............................................................................... 3-12 UNIQUANT............................................................................................................ 3-17 Select User Database for UniQuant Measurements ......................................... 3-17 UniQuant Menu ................................................................................................. 3-19 Prepare UniQuant Measuring Tasks............................................................. 3-19 Sample Identification..................................................................................... 3-21 Measure Intensities for UniQuant.................................................................. 3-21 Import of Intensities........................................................................................... 3-22 Calculate Concentrations .................................................................................. 3-25 More advanced Features in UniQuant............................................................... 3-30 Define Materials ............................................................................................ 3-30 Viewed Mass................................................................................................. 3-32 Alternative Lines............................................................................................ 3-32 Case Numbers .............................................................................................. 3-34 Convert a Subset into a measuring Program .................................................... 3-35 4 QUANTITATIVE ANALYSIS.................................................................... 4-1 INTRODUCTION..................................................................................................... 4-1 CONCENTRATION ANALYSIS............................................................................... 4-2 Change Task....................................................................................................... 4-4 Change Program................................................................................................. 4-5 Manual Sample Mode ......................................................................................... 4-6 Table of Content AA83501 WinXRF Operator Manual III Pre-defined Sample Mode................................................................................... 4-6 Recalculate.......................................................................................................... 4-7 Metaverage ......................................................................................................... 4-7 Bad Sample Analysis .......................................................................................... 4-7 Automatic Drift Correction Control....................................................................... 4-8 Setting-up Samples......................................................................................... 4-9 Type Standards............................................................................................... 4-9 Enter EXAN Data .............................................................................................. 4-10 Colours and Result Flags .................................................................................. 4-10 Execution of Analysis Features ......................................................................... 4-12 Manual Run Selection................................................................................... 4-13 Analyses with Quality Check......................................................................... 4-15 Analyses with Quality Sort............................................................................. 4-17 Analyses with Charge Correction.................................................................. 4-18 Perform Charge Correction ................................................................................................. 4-19 Normal Situation........................................................................................................................... 4-21 Special Situations......................................................................................................................... 4-25 Result Modification............................................................................................ 4-27 Result Options................................................................................................... 4-27 Print Mode..................................................................................................... 4-28 Transmit Mode .............................................................................................. 4-29 Storage Mode................................................................................................ 4-29 SPC Transfer ................................................................................................ 4-30 Display Modes............................................................................................... 4-30 Average Calculation with different Samples...................................................... 4-30 INTENSITY MEASUREMENTS............................................................................. 4-32 5 DRIFT CORRECTION OF THE INSTRUMENT....................................... 5-1 INTRODUCTION..................................................................................................... 5-1 QUANTITATIVE ANALYSES................................................................................... 5-1 Performing the Drift Correction Update (Re-calibration)...................................... 5-1 Drift Warnings and Reports............................................................................. 5-9 QUANTAS ............................................................................................................. 5-10 Performing the QuantAS Re--calibration........................................................... 5-10 UNIQUANT............................................................................................................ 5-12 Measure the Monitor Samples .......................................................................... 5-13 Import Measured Intensities .............................................................................. 5-13 Examination of the Drift ..................................................................................... 5-15 6 CONTROL SAMPLE ANALYSIS ............................................................ 6-1 INTRODUCTION..................................................................................................... 6-1 ANALYSING CONTROL SAMPLES........................................................................ 6-2 TRANSFER TO SPC............................................................................................. 6-10 Bad Sample Transmission ................................................................................ 6-10 Table of Content WinXRF Operator Manual AA83501 IV SPC Messages.................................................................................................. 6-10 7 UNATTENDED OPERATION.................................................................. 7-1 INTRODUCTION..................................................................................................... 7-1 UNATTENDED ANALYSIS...................................................................................... 7-2 ICS Operations Manager..................................................................................... 7-6 Step List Manipulation..................................................................................... 7-6 BATCH OPERATION .............................................................................................. 7-7 Running Batches................................................................................................. 7-7 8 RESULTS RETRIEVAL & STATISTICS.................................................. 8-1 INTRODUCTION..................................................................................................... 8-1 RETRIEVAL & STATISTICS ................................................................................... 8-2 Selection Criteria for Results Retrieval ................................................................ 8-2 Procedure for Results Retrieval........................................................................... 8-3 Database Selection......................................................................................... 8-3 Task Selection................................................................................................. 8-4 Analytical Program Selection .......................................................................... 8-5 Sample Identity Filter ...................................................................................... 8-7 Time Period Filter............................................................................................ 8-7 Result Type Filter ............................................................................................ 8-8 Terminating Selections.................................................................................... 8-9 Actions to be carried out on Retrieved Results ................................................... 8-9 Action Buttons............................................................................................... 8-11 Modification of Results ...................................................................................... 8-11 Export Results ................................................................................................... 8-12 Transmission of Results.................................................................................... 8-15 Statistics............................................................................................................ 8-16 Quality Check .................................................................................................... 8-20 Quality Sort........................................................................................................ 8-21 Charge Correction............................................................................................. 8-22 Send to SPC...................................................................................................... 8-23 9 AUTOMATION AND REMOTE SAMPLE DEFINITION MODES............. 9-1 AUTOMATION MODE............................................................................................. 9-1 Setting Automatic Mode ...................................................................................... 9-1 Using WinXRF in Automatic Mode...................................................................... 9-4 REMOTE SAMPLE DEFINITION MODE................................................................. 9-5 Setting Remote Sample Definition Mode ............................................................ 9-5 Using WinXRF in Remote Sample Definition Mode ............................................ 9-7 10 METAVERAGE OPTION................................................................... 10-1 MANUAL OPERATION ON METAVERAGE PROCESS....................................... 10-1 Table of Content AA83501 WinXRF Operator Manual V Quality Control of the Metaverage..................................................................... 10-6 BEHAVIOUR WITH AUTOMATED MODES.......................................................... 10-7 Metaverage with Automatic Mode ..................................................................... 10-7 Metaverage with Remote Sample Definition Mode ........................................... 10-7 11 ANALYSIS RECALCULATION OPTION........................................... 11-1 USING ANALYSIS RECALCULATION.................................................................. 11-2 Changing Sample Signature.............................................................................. 11-4 Redefining Recalculation Parameters ............................................................... 11-5 Recalculation Process....................................................................................... 11-6 Results Retrieval ............................................................................................... 11-7 Transmission to SPC......................................................................................... 11-8 Properties of Recalculated Results ................................................................... 11-9 Compac Format Type CMP?0_0? ................................................................ 11-9 Other Compac Formats................................................................................. 11-9 DBase and Lotus Formats ......................................................................... 11-10 Telex A and Telex B Formats...................................................................... 11-10 Printed Results............................................................................................ 11-10 ASCII Format .............................................................................................. 11-10 A ABOUT THE WINXRF SOFTWARE....................................................... A-1 THE MOUSE ........................................................................................................... A-1 SPECIAL KEYS....................................................................................................... A-1 Selection of a Group of Items.............................................................................. A-2 WINDOWS TERMINOLOGY................................................................................... A-4 B WINXRF ICONS..................................................................................... B-1 ICON COMPOSITION AND COLOURS.................................................................. B-1 Meaning of the Colours ....................................................................................... B-1 Meaning of the Polygons..................................................................................... B-2 Meaning of the Elements..................................................................................... B-3 Other Symbols..................................................................................................... B-4 ALL WINXRF ICONS AND SHORTCUTS............................................................... B-5 Icons.................................................................................................................... B-5 Menu Function Frame and Log In................................................................... B-5 Generic Icons.................................................................................................. B-5 Instrument Icons.............................................................................................. B-6 General Icons.................................................................................................. B-8 QuantAS Icons.............................................................................................. B-11 Analysis Task Icons ...................................................................................... B-11 Instrumental Check Icons.............................................................................. B-12 Check Task Icons.......................................................................................... B-13 Shortcut and Desktop Icons .............................................................................. B-14 INDEX............................................................................................................. I
GETTING STARTED Getting Started Chapter 1 AA83501 WinXRF Operator Manual 1-1 1 GETTING STARTED Introduction The WinXRF software is described in two manuals, the Configuration Manual and the Operator Manual. The Configuration Manual is intended to be used by the laboratory chief or the system manager. WinXRF needs to be configured before routine operations can be carried out. Many of these configuration steps will be carried out by the Service Engineer installing the system but it is obviously important that these steps are understood so adjustments to them can be made in the light of operational experience. These configuration steps are described in the Configuration Manual. The Operator Manual is intended to be used by an operator. This manual explains the day to day operation of WinXRF. It explains how to use WinXRF to analyse unknown samples and to perform investigations such as semi-quantitative and qualitative analyses. It also describes how to retrieve previously stored results and examine, modify or carry out statistical calculations on these. Various Options are also available with WinXRF, but they are not included in the basic package and may be supplied with the system on request. However, the documentation for the options is included in the standard documentation delivered. A list of these options is given in the WinXRF Configuration Manual. Chapter 1 Getting Started WinXRF Operator Manual AA83501 1-2 WinXRF Software Documentation The WinXRF manuals are supplied on the CD-ROM containing the WinXRF software. The WinXRF Operator Manual is also supplied on paper. The vendor documentation is supplied for the optional third- party software packages (R & R Report Writer, SPC and UniQuant). The list of manuals and their purpose is given in the following table. Manual Description WinXRF Configuration Manual Describes all stages needed to configure WinXRF. WinXRF Operator Manual Describes how to use WinXRF to analyse unknown samples and to carry out other day to day operations. UniQuant Manual (only delivered if this option has been ordered) Describes in full detail how the UniQuant program works and explains the physics and mathematics involved. R & R Report Writer User Guide (only delivered if this option has been ordered) Describes how to install and use the optional R & R Report Writer software. Reference to this should be made for details of the extended features of the R & R Report Writer that are not covered in the WinXRF manuals. SPC Light User Guide (only delivered if this option is included) Describes how to install and use the optional SPC-Light software. Reference to this should be made for details of the extended features of the SPC-Light software that are not covered in the WinXRF manuals. Summary of the Operator Manual A summary of the content of the WinXRF Operator Manual is given in the following table. Chapter Title Description 1 Getting Started This chapter introduces the WinXRF software. It describes the documentation available with WinXRF and the purpose of the manuals supplied. It also suggests how each manual should be used and for whom they are intended. Furthermore, it describes the basic instrument operations. 2 Qualitative Analysis This chapter is only relevant for instruments equipped with a goniometer. It explains how to perform scans over specific angular ranges with the goniometer and how to identify the found peaks. A qualitative analysis may serve as a first step in the process of an instrument calibration. 3 Semi-Quantitative Analysis This chapter explains how to perform analyses with the two available semi-quantitative programs QuantAS (formerly ASQ) and UniQuant. 4 Quantitative Analysis This chapter describes principally how to perform concentration analyses on unknown samples. Analytical programs and analytical tasks have to be set up and the instrument calibrated before unknown samples can be measured. Getting Started Chapter 1 AA83501 WinXRF Operator Manual 1-3 5 Drift Correction of the Instrument This chapter explains how to correct the instrumental drift on a regular basis. 6 Control Sample Analysis This chapter explains how to measure Control Samples. Appropriate samples and tasks must have been defined before this feature can be used. Control sample analysis is mainly used with the SPC option (Basic or Full). 7 Unattended Operation This chapter explains how to set up and perform operations without operator interactions, either in the Unattended Analysis mode or using the Batch Operation. 8 Results Retrieval & Statistics This chapter describes the facilities available for examining stored results. It explains how selected results can be retrieved for examination, modification, printing, exporting and transmission, if available. It also explains how further post analysis treatments such as quality checks and statistical calculations can be performed. 9 Automation and Remote Sample Definition Modes This chapter explains how to use the Automation Mode and the Remote Sample Definition Mode options. 10 Metaverage Option This chapter explains how to use the Metaverage option and its behaviour in automated mode. 11 Analysis Recaculation This chapter explains how results can be reprocessed after the analysis. A About the WinXRF Software Some explanations are given to help you become familiar with the common actions in WinXRF. B WinXRF Icons This appendix explains in detail the significance of the icons used in WinXRF. You will find a complete list of the WinXRF icons. Chapter 1 Getting Started WinXRF Operator Manual AA83501 1-4 Software Installation Notes: WinXRF requires Internet Explorer 5.0 or higher and the Internet Information Services (IIS). The Internet Information Services for Windows 2000 must first be configured before the installation of WinXRF. If there is no Internet Explorer on the computer, the WinXRF installation wizard will automatically install the IE5 release (English version only) before starting the WinXRF installation. Third-party optional packages, such as SPC, UniQuant and R&R, must be installed prior to their WinXRF option installation. The WinXRF software is provided with a comprehensive installation wizard. When the WinXRF CD-ROM is inserted in the CD drive, the following window is displayed after a short while. Figure 1.1 You can select the items you want to install and press on the Install selection button, then follow the on- screen instructions. If you are not familiar, we recommend you follow the installation instructions given in the Software I nstallation Chapter of the WinXRF Configuration Manual. However you may first need to install the documentation option, in order to be able to read or print the instructions of the Software Installation Chapter of the WinXRF Configuration Manual. The installation of the documentation option is therefore described in the next section. Getting Started Chapter 1 AA83501 WinXRF Operator Manual 1-5 Installation of the Documentation from CD-ROM General Comments The installation of one (or more) set(s) of documentation manual(s) creates a folder ARL Doc in the Program folder of the Windows Start menu, and as many shortcuts as manuals inside the folder. The documentation itself can be loaded on the hard disk, or read from the CD-ROM. The documentation manuals are available as PDF files. Therefore, the Acrobat Reader freeware must be installed on your computer for viewing and printing the documentation. Note: The WinXRF documentation and the Acrobat Reader are the only items that can be installed without installing the basic WinXRF software. This can be useful if you want to consult the documentation on a computer other than the one used with your instrument! The complete installation of the WinXRF software and its options is described in the WinXRF Configuration Manual. Here below, the steps for installing the WinXRF documentation only are described. Starting the Installation Program Insert the WinXRF CD-ROM in the CD-ROM disk drive unit. The installation process starts automatically (autostart). Alternatively, the installation can also be started manually by pressing on the Windows Start button, choosing Run and then typing L:\START (assuming L is the identity letter of the CD-ROM drive unit). After some seconds the installation wizard displays the WinXRF installation dialog box as shown in Figure 1.1. Please refer to the next sections for installing a particular documentation set. Installation of the Acrobat Reader The following will install the Adobe Acrobat Reader (freeware product) onto the hard disk. On the WinXRF installation dialog box (Figure 1.1) select the Acrobat Reader item. Click on the Install selection button, the program prepares to install the Acrobat Reader on your hard disk. After some seconds the following dialog box is displayed. Chapter 1 Getting Started WinXRF Operator Manual AA83501 1-6 Figure 1.2 Press on the Next button. Figure 1.3 Getting Started Chapter 1 AA83501 WinXRF Operator Manual 1-7 Press on the Accept button. Figure 1.4 Keep the proposed destination folder and press on the Next button. The installation starts. At the end the following message box is displayed. Figure 1.5 Click on OK. The Adobe Acrobat Reader program is installed. Installation of the Documentation Manuals The following will install one documentation manual on your system. Note: The Acrobat Reader must first be installed on the hard disk in order to read the WinXRF documentation. Start the installation as described in Section Starting the Installation Program. In the installation dialog box, select the WinXRF/Doc item of the desired language. Click on the Install selection button, the following dialog box is displayed. Chapter 1 Getting Started WinXRF Operator Manual AA83501 1-8 Figure 1.6 Press on the Next button. Figure 1.7 Choose one of the two optional radio buttons. We recommend you copy the PDF files to the hard disk. One set of WinXRF documentation (one language) will take approximately 30 MB on the hard disk. Note: If you keep the PDF files on the CD-ROM, you will leave more space on your hard disk, but each time you want to consult the documentation you will need to insert the CD-ROM in the CD drive unit. Consulting from the CD-ROM is also slower than when the PDF files are located on the hard disk. Nevertheless, if you want to keep the files on the CD-ROM, then we recommend you to leave the CD-ROM in the CD drive unit. Getting Started Chapter 1 AA83501 WinXRF Operator Manual 1-9 Press on the Next button. Figure 1.8 Press on the Next button. Figure 1.9 Press on the Finish button. You are returned to the WinXRF installation dialog box (Figure 1.1). Repeat the procedure if another set of documentation manuals must be installed. Otherwise press on the Exit button to leave the installation wizard. Viewing or Printing the Documentation The Adobe Acrobat Reader must be available on your computer system, and the WinXRF Documentation must be installed. For installing the Acrobat Reader and the Documentation, refer to the previous sections. Chapter 1 Getting Started WinXRF Operator Manual AA83501 1-10 To view the documentation, click on the Windows Start menu, select Programs and then the Arl-doc folder, and finally click on the manual you want to consult, as shown below. Figure 1.10 If the PDF files were not installed on the hard disk you need to insert the WinXRF CD-ROM in the disk drive. Note: When you insert the disk in the CD drive unit, it starts automatically and the Installation dialog box is displayed. Just press on the Stop installation button to stop the installation process. Alternately you can keep the s key pressed some seconds when inserting the CD to disable the autostart. Getting Started Chapter 1 AA83501 WinXRF Operator Manual 1-11 After having selected the manual to consult, the Acrobat Reader is automatically started and the required documentation file is opened at the first page, as shown in the example below. Figure 1.11 You can scroll the text with the right scroll bar. You can flip the pages with the ! and " buttons of the bottom menu bar. After some pages you should find the table of contents. A simple click on a heading in the table of contents will immediately link you to the concerned section. To print the document, use the Print command of the File menu or the printer button of the toolbar. Depending on the printer, the complete printout of the manual may take several hours and requires several hundred sheets of paper. Note: The printing layout is optimised for the A4 size paper format; and consequently the table of content and index page references correspond to this size as well. For more information, use the Help menu of the Acrobat Reader. Chapter 1 Getting Started WinXRF Operator Manual AA83501 1-12 Logging into WinXRF There are three ways to launch WinXRF from Windows: Double click on the WinXRF shortcut on the desktop. Double click on any of the WinXRF function shortcuts on the desktop; WinXRF will start before calling the function defined by the shortcut.. From the Windows Start menu, select Programs, then Arl and click on WinXRF V3.0-1, as shown in Figure 1.13. Figure 1.12 Getting Started Chapter 1 AA83501 WinXRF Operator Manual 1-13 Figure 1.13 All three ways launch the software and perform some preliminary checks. WinXRF background applications are also launched. Note: At the very first launch, and if an earlier version of WinXRF was installed and not properly uninstalled, several warning messages may be displayed before the WinXRF program is accessed. If the system detects an actual database that requires to be revived, you will automatically be prompted to revive the database with the wizard. After a short while the main page of WinXRF, showing the available Shortcuts, is displayed, as shown below. However, if the password option has been switched on, then the Log in screen will be displayed instead, see Section Password Protection. Chapter 1 Getting Started WinXRF Operator Manual AA83501 1-14 Note: If you have launched WinXRF from a shortcut on the desktop, you will not see the main page as shown below, but directly the analysis window corresponding to the shortcut definition. Figure 1.14 An explanation of the WinXRF graphical interface is given later in Section WinXRF Menu Structure. The significance of the pictorial material (icons) is given in Appendix WinXRF Icons. Some other WinXRF associated tasks are also automatically launched in the background, represented by icons in the Windows taskbar. Depending on the options already set, additional taskbar items can also be found, as shown in the example below. Figure 1.15 The taskbar items related to WinXRF can be: Alarm Reporter Alarm/Result Print Manager Line Communication Monitor of ICS Line Communication Monitor of Automation Instrument Status Monitor Net Result Net Interface Getting Started Chapter 1 AA83501 WinXRF Operator Manual 1-15 Password Protection To protect the analytical database, the WinXRF users' privileges may be restricted by a Log In procedure, which requires the input of a User name and a Password. In such a case, XRF has to be specified in both entry boxes and the WinXRF start-up procedure will be completed. Figure 1.16 Chapter 1 Getting Started WinXRF Operator Manual AA83501 1-16 Instrument Initialisation When the WinXRF Software is started, various application programs are installed first and the instrument may then be brought into communication, i.e. ICS/ACS liaison is established, by use of the ICS Instrument Initialisation dialog box which is presented. Figure 1.17 In this dialog box, all or any of the tables offered can be sent to the corresponding microprocessors by selecting the appropriate check boxes. For instruments with a goniometer the option Line Library is enabled for selection and if it is selected, the option Select lets you choose the category of lines to be sent to the instrument (see figure below). The initialisation is started by clicking the OK button. Figure 1.18 Note: At the end of the proper initialisation the content of the Dialog File INIT.MIO is transmitted to the instrument. This file contains some additional configuration data, which should not be changed, but can also be used to configure the instrument in a non-standard way (see WinXRF Configuration Manual). Getting Started Chapter 1 AA83501 WinXRF Operator Manual 1-17 If during this time you watche the synoptic panel of the instrument the following will be observed: 1st Top row (Top left) displays RESET and goes to STAND BY 2nd Middle row (Top right) nothing happens (or INIT and then IDLE) 3rd Bottom row (Bottom) flashes and displays current position of selected goniometer in terms of Angle, Crystal/Detector combination. After a reset the 3 rows read: Top (Top left) STAND BY Middle (Top right) displays the current tube conditions (or IDLE) Bottom (Bottom) Actual Goniometer Parameters Failure of any of the three display areas to respond as expected from hardware fitted, indicates, that the respective microprocessor is not in communication. Note: In the case of a simultaneous instrument with no goniometer, the bottom line will remain blank; for a double goniometer instrument or an instrument combined with an XRD goniometer channel the synoptic panel will display a fourth row (i.e. two bottom rows). On older instruments the display rows are arranged differently (shown in parenthesis). Nevertheless, the sequence of information shown during the system start-up is basically the same as described above. Generally, it is necessary to load the microprocessors with the tables of information they need to operate in the following cases: when the instrument is first commissioned, if it has had a microprocessor replaced or repaired, after a long power break, as a first step in case the instrument reports error messages related to these tables. The instrument can also be initialised manually, by clicking on the Send Instrument Configuration icon of the Initialisation menu as shown below, or by typing the function key ^ . Chapter 1 Getting Started WinXRF Operator Manual AA83501 1-18 Figure 1.19 Spectrometer Environment During the initialisation sequence the hardware configuration of the instrument and the default parameter settings are transferred to the microprocessors automatically, except the parameter defining the spectrometer environment. Therefore, during a complete system start-up the environment has to be defined. This is done by selecting the Set Environment icon in the Initialisation folder, as shown in the previous figure. The dialog box shown in the figure below is used to specify the desired spectrometer environment which is normally Vacuum. The same procedure applies if the environment of the spectrometer has to be switched from Vacuum to Helium or Air (in case the spectrometer needs to be opened). Please note that for Advant'X and 9400 instruments two modes of Helium operations are available, i.e. with or without Helium shutter, as shown in the second figure. Figure 1.20 Getting Started Chapter 1 AA83501 WinXRF Operator Manual 1-19 Figure 1.21 Note: When the spectrometer environment is Helium the sample is automatically ejected after 20 minutes to prevent the Polypropylene or Mylar foil becoming damaged due to excessive exposure to X-rays. This is also the reason why the foil should be changed after each exposure to X-rays. Even if the foil still seems to be satisfactory it can become brittle and therefore break very quickly. Zero Goniometer As a result of the initialisation procedure, the system requires the execution of the Zero Goniometer function. Even if this operation is not explicitly required, it is good practice at this stage to perform this function by selecting the corresponding icon in the Intialisation folder, see Figure 1.19. If more than one goniometer is mounted the zero operation has to be done on each goniometer separately by selecting its number first. The operation is started by clicking the OK button. Figure 1.22 X-Ray Tube Conditions Normally, selection of combinations of kV and mA is programmed within analytical and all measurement programs. It is however possible to change the setting manually. Access to this is obtained by selecting the corresponding icon in the Intialisation folder, see Figure 1.19. The dialog box shown in the next figure is then displayed offering the conditions described below. Chapter 1 Getting Started WinXRF Operator Manual AA83501 1-20 Figure 1.23 X-ray state On slow Changes take place at the rate of one 5 kV or one 5 mA step per 20 seconds interval. On fast Changes take place at the rate of one 5 kV or one 5 mA step per 5 seconds interval. Off The tube is switched off. No change The last selected X-ray state and mode conditions apply. X-ray mode Operational The generator will always return to this value after a power failure. Non-autostart The tube will remain switched off after a power failure. Standby Defines a period of non-operation. A setting such as 20 kV/ 20 mA is recommended to reduce the power consumption of the instrument. X-ray Voltage and Current The desired tube settings are specified here. Anode target Not used. Getting Started Chapter 1 AA83501 WinXRF Operator Manual 1-21 Instrument Supervision Display Instrument Status There are 4 different ways to display the actual values of the status channels: Read Instrument Status (this section) Analytical Program (Configuration Manual) Status Reporter (Configuration Manual) Alarms and Status Monitoring (Configuration Manual) The selected status values can be displayed by clicking on the Read Instrument Status icon (see Figure 1.19), or simply by pressing the function key F7. The screen as shown in the figure below is then displayed. The status channels can be selected through the Status Reporter see WinXRF Configuration Manual. Figure 1.24 Instrument Alarms The options available in the Alarm Reporter allows you to direct the reported alarms in different ways. An alarm logger records alarms in a file for recall after a period of unattended operation. Provision is made to display them on the screen and to print as required. In order to make use of the options, the Alarm Reporter has to be restored by double-clicking onto the corresponding icon and the screen in the figure below will then be displayed. Figure 1.25 Chapter 1 Getting Started WinXRF Operator Manual AA83501 1-22 The selection of an option is indicated by a checkmark on its left side. These are: Report on screen This option is selected by default. When alarms are received from the instrument a message box containing a description of the alarms is displayed (see figure below). Figure 1.26 An additional explanation of the highlighted alarm message can be obtained by selecting the Description option. Normally, this explanation has to be set up by the user himself. Figure 1.27 Log on printer The alarm messages are reported on the printer. File tracing on/off (ALARM.DMP) The alarm messages are stored in the file ALARM.DMP. Print file trace This file can be printed with the corresponding function. Messages Always on Top The alarm messages will always stay on top, i.e. they are not hidden by other application windows and are therefore always visible. Note: Alarms can also be recorded and graphically displayed with the Alarms and Status Monitoring (see WinXRF Configuration Manual). Getting Started Chapter 1 AA83501 WinXRF Operator Manual 1-23 Instrument Communication It may happen that the communication between the Analytical Control System (ACS) and the XRF instrument (ICS = Instrument Control System) is interrupted. In such a case an error message, as shown in the figure below, is given when the system tries to communicate with the instrument. Figure 1.28 In order to re-establish the communication with the instrument, the communication link has to be reset and re-synchronised. This is done by initialising the instrument as explained in Section Instrument Initialisation. Another way consists of executing the Synch function (see Section Reset Instrument). Reset Instrument If for any reasons the instrument has to be reset when a task is not running (thus the Abort function is unavailable) the icon as shown in the figure below has to be selected (Utilities - Communication - Terminal Mode). Chapter 1 Getting Started WinXRF Operator Manual AA83501 1-24 Figure 1.29 This displays the dialog box shown in the next figure. The commands to be entered in the corresponding box are so-called terminal mode commands and are addressed directly to the instrument microprocessors. The mnemonic command re resets the instrument. Note: By pressing on the Synch button a BREAK/DEL/DEL sequence is sent, causing the communication between the ACS (Analytical Control System, i.e. Computer) and the ICS (Instrument Control System, i.e. Instrument) to be synchronised and the instrument reset. Getting Started Chapter 1 AA83501 WinXRF Operator Manual 1-25 Figure 1.30 Abort Instrument Operations At any time a currently running operation can be interrupted with the Abort function. During manual analyses this function is directly visible, as shown in the example below. Figure 1.31 For all other instrument operations, like Scans or Unattended Analyses, this function is hidden in the ICS Operations Manager, which normally runs in the background as an icon. Therefore, in order to abort such an operation the Line Communication Monitor has to be restored by double-clicking on the corresponding icon and the dialog box shown below will be displayed. Chapter 1 Getting Started WinXRF Operator Manual AA83501 1-26 Figure 1.32 Note: The execution of the Abort function interrupts the currently running operation immediately by resetting the instrument. Alternatively, if the Halt function is selected, the currently running operation is finished before the instrument is reset. Getting Started Chapter 1 AA83501 WinXRF Operator Manual 1-27 WinXRF Menu Structure The WinXRF menus are displayed as web pages in HTML format. Commands and functions are called by a single click on the left button of the mouse. The mouse pointer changes from to when it is moved on the screen on an available function or command. Display Modes WinXRF is displayed in an HTLM window, which is divided into three frames as shown below. Title bar Header Frame Menu Functions Frame Menu Content Frame (Folders / Commands / Shortcuts) Figure 1.33 Chapter 1 Getting Started WinXRF Operator Manual AA83501 1-28 There are two display modes as shown in the next two figures: Icon (shortcut) mode Tree mode In the menu function frame, the currently selected function is on a blue background with a red border. The other available functions are on a blue background with a light blue border. Figure 1.34 Main Menu in Icon Mode Getting Started Chapter 1 AA83501 WinXRF Operator Manual 1-29 Figure 1.35 Main Menu in Tree Mode The switching from one mode to the other is done by a simple click on the Tree / Icon Mode toggle icon. The latter and the other icons of the function frame are explained in the next Section Icons of the Function Frame. The meaning and decoding of all pictorial material is explained in Appendix WinXRF Icons. Chapter 1 Getting Started WinXRF Operator Manual AA83501 1-30 Icons of the Function Frame The Function Frame on the left of the main HTML window has menu buttons and function icons (see the following figure). Figure 1.36 The meaning of these icons is given below. Home Layout Exit About Log off Figure 1.37 These direct functions are described in the following sub-sections. An additional icon may be visible, as it is possible to display a client logo (see WinXRF Configuration Manual). The client logo icon does not call any function. Getting Started Chapter 1 AA83501 WinXRF Operator Manual 1-31 Home Calls back the Shortcut frame, as shown in Figure 1.36. Layout This function toggles the layout display from Icon view to Tree view and vice versa, as shown in Figures 1.34 and 1.35. Exit A click on this icon closes the WinXRF software. It is equivalent to typing a +$ . About This icon calls the About WinXRF information page as shown in the next figure. Log Off It is possible to exit from the WinXRF software by using the Log Off icon. This function is available only when the password protection feature is selected. After the Log Off function is selected the system returns to the Log In page, as shown in Figure 1.16. A new user can then enter his name and password to use the WinXRF software. The Log Off function does not close WinXRF. For this purpose, type a +$ or use the Exit icon as described in the next section. Chapter 1 Getting Started WinXRF Operator Manual AA83501 1-32 Figure 1.38 Click on the button at the top right of the window to go back to WinXRF. Working with Shortcuts Note: How to create and define shortcuts is explained in the WinXRF Configuration Manual. The shortcut allows the operator to start a specific analysis or function with only one click. The shortcuts are identifiable by the yellow triangle on the left bottom corner of an icon. They are stored in the Shortcut folder of the Production / Analysis menu, and can also be placed as a shortcut icon on the computer desktop. The shortcut folder can be accessed at any time by clicking on the Home icon of the menu function frame. Getting Started Chapter 1 AA83501 WinXRF Operator Manual 1-33 Figure 1.39 Shortcut folder QUALITATIVE ANALYSIS Qualitative Analysis Chapter 2 AA83501 WinXRF Operator Manual 2-1 2 QUALITATIVE ANALYSIS Introduction In all XRF instruments equipped with one or more goniometers, it is possible to scan areas of the spectrum to perform qualitative analyses and to verify peak and background positioning. In the case of multiple goniometer instruments up to 3 goniometers may be scanned simultaneously (see Chapter Unattended Operation). Running a Scan Previously prepared scan parameter sets (see WinXRF Configuration Manual) may be run by selecting Production / Analysis - Qualitative Analysis - Run Scans (see next figure). Figure 2.1 The screen shown in the next figure is then presented. The combo box Database Category is used to select the category from which the parameter files can be selected. The parameter files belonging to the selected category are then displayed in the corresponding list box. The name of the file for the scan results can either be entered directly into the corresponding edit box or is selected from the list box on the right-hand side, in case an existing scan results file can be overwritten. A text string may be entered for additional identification when the scan is displayed graphically on the screen. Chapter 2 Qualitative Analysis WinXRF Operator Manual AA83501 2-2 Figure 2.2 Sample Identifier The default WinXRF sample identity scheme is displayed to identify the sample. At least one sample identity must be given before the scan can be started. Print Scan Graph The recorded scan will be printed automatically if either the option Print in Linear Scale or Print in Logarithmic Scale is selected. Automatic Peak Identification If this option is selected, WinXRF performs a scan identification automatically at the end of the measurement. The result of this identification will also be printed, if one of the print options is selected, together with a list of the found peaks (see Section Automatic Scan Identification). When the option Peak Details is selected, the peak resolution of the identified peaks will be displayed. Cassette (./+) The cassette number or magazine position (9400 and 9800) is specified here. '.' indicates the cassette on the lift and '+' indicates the next cassette. If scans are to be performed on more than one goniometer simultaneously, then the Batch Operation can be used where it is possible to predefine various analysis sequences (see Chapter Unattended Operation). On-Line Scanning After a scan has been launched, the spectrum can be displayed on-line while it is being recorded. This is done by selecting Production / Analysis - Qualitative Analysis - View Scans (see next figure). Qualitative Analysis Chapter 2 AA83501 WinXRF Operator Manual 2-3 Figure 2.3 The dialog box in the figure below is then presented allowing the required goniometer activities to be displayed (Current Active Scanning). After every 30 measurements the screen is refreshed and the new measurements added to the displayed graphic. Figure 2.4 Chapter 2 Qualitative Analysis WinXRF Operator Manual AA83501 2-4 Starting Scan Graphics The Scan Graphics function is invoked by selecting Production / Analysis - Qualitative Analysis - View Scans (see next figure). Figure 2.5 From the dialog box shown in the figure below, up to three scans can be displayed simultaneously. These can either be recorded scans or scans that are currently being recorded (On-Line Scanning). The latter possibility lets you follow the progress of a qualitative analysis directly (see Section On-Line Scanning). Qualitative Analysis Chapter 2 AA83501 WinXRF Operator Manual 2-5 Figure 2.6 The combo box Database Category is used to select the category from which the recorded scan files can be selected. The recorded scan files belonging to the selected category are then displayed in the corresponding list box. If the list box is not accessible the option Saved Results Set has to be selected first. An On-Line activity can be displayed by selecting the corresponding Goniometer (Current Active Scanning). After confirmation by pressing the OK button, the graphic is displayed (see Figure 2.7). Subsequent scans can now be selected using the Add Scan option (Display menu) or, for a new set of scans, the Get Scan option. Various functions and options are provided within Scan Graphics to help the user to identify the peaks, to compare different scans, to make overlap investigations, etc. Explanation of the Scan Graphic Functions In order to get an idea of the possibilities offered by the Qualitative Analysis function, a short description of each function and option is given in the following list: Exit The Scan Graphic function is left. Chapter 2 Qualitative Analysis WinXRF Operator Manual AA83501 2-6 Display Menu Figure 2.7 Get Scan The displayed scans are erased and the dialog box to select a new scan is presented. Add Scan Another two scans can be superimposed sequentially on the currently displayed scan. Add Difference Graph Two scans can be selected for which the difference is displayed. Remove Green Scan The green scan is erased (i.e. first scan selected). Remove Cyan Scan The cyan scan is erased (i.e. second scan selected). Remove Magenta Scan The magenta scan is erased (i.e. third scan selected). Qualitative Analysis Chapter 2 AA83501 WinXRF Operator Manual 2-7 Options Menu Figure 2.8 Graduation in Degrees This is the default x-axis graduation for XRF scans. Graduation in d Spacing (Nanometer) This graduation is available for XRD scans only. Graduation in d Spacing (Angstrom) This is the default x-axis graduation for XRD scans. Graduation in Nanometer This graduation may be selected if scans are to be displayed which were recorded with different crystals over the same wavelength range (instead of Angstroms). Graduation in Angstrom This graduation is proposed if a subsequent scan, recorded with a different crystal, is selected for display. Graduation in Energy scale This graduation is suitable for wide range scans. Because the energy is indirectly proportional to wavelength, the elements are more equally distant from one another. Graduation in Z scale This graduation is based on Moseley's law who established a relationship between the atomic number and the wavelength (i.e. the 2 Theta angles). When this graduation is selected, the user is asked to specify for which X-ray series the x-axis is to be graduated (i.e. Ka, Kb, La, Lb, Ma and Mb). The corresponding chemical symbols are shown in the upper right corner of the screen. Chapter 2 Qualitative Analysis WinXRF Operator Manual AA83501 2-8 Point Markers On/Off The measured points, forming the scan, are indicated by white crosses. Tag Lines On/Off When this option is selected, a vertical line is displayed in addition to the identification tag. This identification line can be displaced by moving the mouse pointer onto it and a subsequent dragging action (move the cursor while keeping the right mouse button pressed). The possibility to move the identification line is indicated by a different mouse pointer (see Section How to use the Mouse in Scan Graphics). As an alternative, the left and right arrow keys can be used. This option is always selected when scan graphic is entered. Peak Resolution On/Off If selected, the half peak position and the calculated background are indicated with red lines in addition to the calculated peak resolution. These indications are also printed. See Section Peak Resolution. Logarithmic Scale On/Off The y-axis is graduated using a logarithmic scale. Add/Remove Graph Labels This function allow you to enter up to 10 labels or scan titles in the graphic area as additional information especially for printed hardcopies. Identification Interval The default identification interval of 0.4 degrees can be changed with this function. This may be of particular interest if overlap investigations are to be made for which the interval may be changed to 1 or 2 degrees. Relative Intensity Threshold The default threshold of 5 % suppresses weak lines, which may not be of primary interest in peak identifications. In case the very weak peaks are also to be identified, this threshold may be put to 0 %. Peak Details Parameters This is used to specify the parameters to be applied for the determination of the Real Peak Position and the Peak Resolution. Record Identifications in File The identification tags are stored in the corresponding scan results file. Add/Amend Line in Line Library This is used to add a new line or amend an existing line in the line library with the parameters used when the scan was recorded and the parameters that have been determined through scan investigation, i.e. real peak and background positions. Full explanations are given in the WinXRF Configuration Manual. Add/Amend Background Lines in Line Library This is used to add a new separate background line or amend an existing one in the line library with the parameters used when the scan was recorded and the parameters that have been determined through scan investigation, i.e. background position. Full explanations are given in the WinXRF Configuration Manual. Print using Non Solid line When this option is selected the scan graphs are printed with different dashed lines to clearly distinguish them on photocopies made from a colour printing. Qualitative Analysis Chapter 2 AA83501 WinXRF Operator Manual 2-9 Show Menu (Figure 2.11) Element This function displays the periodic table on the left hand side of the screen allowing the family lines of the selected element to be displayed, if these fall into the spectrum shown on the screen. Compound This function is only available if an XRD goniometer is installed in the instrument. Similar to the function above, it displays a list box containing possible phases. Please refer to the XRD manual for more details. Peak Details When this option is selected, the peak resolution of all identified lines will be calculated (see Section Peak Resolution). Remove Peak Details When this option is selected, all indications related to Peak Resolution will be removed. Manual Peak Resolution This option is used to manually determine the peak resolution for already identified lines. Identification Menu (Figure 2.13) Automatic Identification The identities of the elements found in the displayed scan are inserted automatically. Erase Identifications The peak identifications are removed. Background (see WinXRF Configuration Manual for further details) Figure 2.9 Chapter 2 Qualitative Analysis WinXRF Operator Manual AA83501 2-10 Define Positions This is used to define background positions that will be employed with various mathematical functions to calculate net peak intensities. Iteration Limits This is used to define the maximum number of iterations and the correlation factor used to determine the background curve. Calculation This is used to select the mathematical evaluation function and calculate the background curve. Subtract This is used to subtract the background curve from the displayed scan to obtain net intensities. Undo Subtraction This is used to cancel the background subtraction so as to be able to eventually repeat the evaluation with a new function. Print This function is used to print the displayed scans. Note: If the option Print using Non Solid line is selected (see Figure 2.8), the scans are printed with different dashed lines to clearly distinguish the recorded spectra of the analysed samples on photocopies made from a colour printing. Lines (identification dialog box) 1st Order ... 9th Order Selects the order of the lines to be identified. Add Displays the family lines of the selected (highlighted) element. Del Erases the currently displayed lines of the selected element. Edit Displays an edit box to enter an identification tag. This is then used instead of the tag proposed by the selected element line. Finish Erases all element lines except the selected (highlighted) one, which is kept as the identification. The Lines dialog box disappears and the process can be started again in a similar way for the next identification. How to use the Mouse in Scan Graphics In order to offer a maximum of simple-to-use features within Scan Graphics, using a mouse was essential and thus, some of the features are only available through the mouse functions. These functions may require some exercise especially to gain the ability to employ the features using single and double-clicks with the same mouse button. Depending on where the mouse pointer is located on the scan display the symbol of the cursor changes. In addition to the normal cross the mouse pointer can have two slightly different shapes indicating that the standard actions provided by the two mouse buttons have changed or a new action has become available. The three shapes of the mouse pointer look as follows: Qualitative Analysis Chapter 2 AA83501 WinXRF Operator Manual 2-11 Figure 2.10 1) This is the standard mouse pointer. The identification (double-click with left mouse button) and zoom functions (single click with left mouse button) are available. A click with the right mouse button cancels the last zoom occurrence. 2) This cursor indicates that the mouse pointer is located on an identification tag or a graph label. This tag or label can then be moved to another place in all four directions by dragging it with the left mouse button pressed, or removed by a double-click with the same button. 3) The mouse pointer changes to this shape when the vertical line of the cross matches with the red identification bar. This identification bar can then be moved horizontally by dragging with the right mouse button pressed. Whenever the mouse pointer is moved the co-ordinates of its position in terms of x-axis and y-axis units are shown in the upper right corner. Scan Identification Identification of the elements present in a scan is carried out by finding the element lines corresponding to the various peaks in a scan. To simplify this task the WinXRF software has all important element lines stored in a file. The information held in this file is used to identify the elements in the scan either manually or automatically. The proposed identifications are tagged with the names of the corresponding element lines and vertical red bars indicating the position and the relative sensitivity of the different lines. On confirming the proposed identifications, the positions of the element lines are then indicated by identification markers, if the option Tag Lines On/Off is selected within the Options menu (Figure 2.8). On the other hand, the identifications are only indicated by the line tags. Please note that this option is selected by default on entering the Scan Graphics function. The following sections explain the mechanisms of scan identification in more details. Manual Scan Identification Two methods of manual scan identification are available. Amongst other differences it is important to observe that with the Show Element method it is possible to retain the displayed spectrum whereas for the Peak Identification method only the selected element line is retained, i.e. the family lines are removed when the process is concluded. Show Element If we know that an element is in the analysed sample this method should be used to identify the corresponding peaks, by selecting the Show menu and subsequently the Element option. A list box with the Chapter 2 Qualitative Analysis WinXRF Operator Manual AA83501 2-12 elements from the periodic table in ascending atomic numbers is displayed on the left-hand side of the screen. After selection of the required element the Draw button has to be clicked and the 'fingerprint' of this element is displayed. Please note, that a double-click with the left mouse button and the cursor pointing at the required element has the same effect. Figure 2.11 The positions of the element lines are indicated by vertical lines of different size corresponding to the relative sensitivity of these lines. If a consecutive selection of an element is effected while staying in the Show Element function, the current fingerprint is removed prior to displaying the new one. If the identifications are to be retained then the function has to be left by pressing the Finish button before the next element can be selected by a subsequent recall of the same function. In order to store the identifications with the scan, the function Record Identifications in File should be used (Figure 2.8). Peak Identification The peak (or position) to be identified is selected by moving the mouse pointer onto that peak. A double- click with the left mouse button reads the pointer position and an identification interval is displayed, symmetrical to the pointer position. All possible lines occurring in the displayed interval are proposed in the list box appearing on the left-hand side of the screen. The line with the highest relative sensitivity among the possible choices is automatically highlighted. Any other element can be selected with the mouse pointer. A click onto the Add button causes the system to display all family lines of the selected element (with a higher relative sensitivity than the sensitivity threshold). Qualitative Analysis Chapter 2 AA83501 WinXRF Operator Manual 2-13 The length of the bars corresponds to the relative sensitivity relative of the respective family lines when related to the sensitivity of the chosen line. The relative sensitivity of the selected element line is adjusted to the mouse pointer position (y-axis) when the peak (position) being identified is finally chosen. If the 'fingerprint' of this element matches with the peaks in terms of positions and peak heights there is a good chance that the peak corresponds to the selected element line. This identification can be retained temporarily, by clicking onto the Finish button. This causes all element lines to be erased, except the selected (highlighted) one, which is kept as the identification. The Lines dialog box disappears and the process can be started again in a similar way for the next identification. Figure 2.12 In order to distinguish between the lines of different diffraction orders, higher order peaks are automatically labelled with a _2, _3, etc. suffix. Note: It should be noticed that a double-click with the left mouse button, while the mouse pointer is placed on the desired element line in the list box, does not have the same effect as that described above. In this way of identification the corresponding line is taken as the identification but without showing the family lines. Furthermore, the position of the identification line does not correspond to the theoretical but to the position of the cursor when the peak position was entered. In order to store the identifications with the scan, the function Record Identifications in File should be used (Figure 2.8). Automatic Scan Identification An automatic scan identification can be performed either on stored scans within Scan Graphics or in an unattended way at the end of the scan recording. Both methods are described in the following two sections. Chapter 2 Qualitative Analysis WinXRF Operator Manual AA83501 2-14 Note: Only first order lines are identified. This may therefore be one of the reasons why not always all peaks are identified. Automatic Identification on displayed Scans The Automatic Identification function is part of the Identification menu in Scan Graphics (see figure below). By selecting this function the system searches for peaks in the recorded spectrum first. Confirmation of these possible identifications for the found peaks is then sought using the presence or absence of family line peaks. If such peaks are present then the correct identification is much easier especially when multiple possibilities exist, as this is often the case. If, however, possible identifications cannot be checked in this way then the element line with the highest relative sensitivity is chosen. Depending on the smoothness of the scan, the complexity of the analysed sample in terms of elements and thus possible overlaps, and the recorded spectrum length, not always all identifications are found correctly. It may also happen that some peaks have not been identified. In such cases it is always possible to correct these errors manually using the standard identification functions (see Section Manual Scan Identification). Figure 2.13 All identifications are removed with the Erase Identifications function. Unattended Scan Identification The option Automatic Peak Identification is included in the dialog box through which the user is asked to define the parameters necessary to run a scan, like the Scan Parameters Set, the Scan File Name, the Sample Identity and the Cassette number (refer to Section Running a Scan). If this option is selected prior to starting the scan operation, the scans will be automatically identified after the end of each scan recording and a print-out similar to the one shown in Figure 2.14 is produced. Qualitative Analysis Chapter 2 AA83501 WinXRF Operator Manual 2-15 This feature is especially useful if a lot of samples need to be analysed qualitatively in which case the list of scans to be run may be stored in a Batch for unattended operation, for instance over night. Please refer to Chapter Unattended Operation for details on how to use the batch operation. ARL Demo & Application Laboratory 28-Apr-94 16:23:10 1024 Ecublens, Switzerland Analysis Scan Result ------------------------------------------------------------------------------------- Scan: GEO-12 (Special Sample), from: SC12, Gonio: 1, 101 steps Figure 2.14 Parameters: Sample Name: GEO Sample Number: 12 Instrument Type: XRF Goniometer 1 Crystal LiF220 Detector SC Collimator 0.15 kV/mA 50/50 Line Intensity(Kcps) Wavelength(A) Angle(deg) SrKa1,2 0.718 0.8768 35.86 BrKB1,3 5.903 0.9331 38.25 SeKB1,3 7.812 0.9924 40.79 BrKa1,2 25.140 1.0413 42.89 SeKa1,2 32.91 1.1064 45.72 GeKB1,3 5.767 1.1294 46.73 AsKa1,2 7.54 1.1774 48.84 GaKB1,3 3.040 1.2083 50.21 GeKa1,2 25.681 1.2555 52.31 GaKa1,2 9.722 1.3416 56.21 Adding Special Identifications There are cases where one wants to change the identification tags proposed by the system or add identification lines which are not contained in the repertoire of element lines, like background positions, absorption edges or satellite peaks. The simplest way to add such an identification is described below: Place the mouse pointer onto the x-axis position where the identification line and tag should be added. Double-click with the left mouse button to call up the Peak Identification function. As for a normal identification, an interval and the list box containing possible element lines are displayed (Figure 2.12). Chapter 2 Qualitative Analysis WinXRF Operator Manual AA83501 2-16 Instead of selecting an element line from the list box (if there are any), press the Edit button. An edit box is now displayed allowing the identification tag to be entered (figure below). After confirming the input by pressing the OK button, the tag is added at the selection position and directly above the scan graph. Figure 2.15 Press the Finish button to conclude the addition. Repeat this operation if other identifications need to be added. Note: The tags and the identification bars can be moved for adjustment, if necessary (refer to next section for details). Other Scan Graphic Editing Features In this section a description of the various graphic functions included in the Scan Graphics package is given and the appended figures illustrate these explanations. Zooming of Scan Graphs The zoom function is used to magnify selected details of the displayed scans at will. This is done by first placing the mouse pointer at the bottom left corner of the region to be zoomed and subsequent pressing of the left mouse button to anchor this position. The mouse pointer is now moved to the top right corner and the same mouse button pressed again to read in the white-framed area of the scan graph (figure below) Qualitative Analysis Chapter 2 AA83501 WinXRF Operator Manual 2-17 which is then blown up to full screen size. This zooming operation can be repeated up to six times to see even the smallest features of the scan graph. Figure 2.16 Pressing the right mouse button causes the last zooming operation to be undone. Through repeated pressing of the same button the zoom events are further undone until the original representation is finally displayed. Pressing the right mouse button without a previous zooming operation causes the y-axis to be displayed with a 0 intensity value as the origin, if the graduation is not logarithmic. Adding Graph Labels Extra information or descriptions, which will appear in the hardcopies of scans, can be placed anywhere in the graphics picture, by means of up to ten Graph Labels. This is done by selecting Add/Remove Graph Labels within the Options menu (Figure 2.8). The dialog box shown next is then displayed allowing a new text string to be entered, an existing label to be changed or deleted. Chapter 2 Qualitative Analysis WinXRF Operator Manual AA83501 2-18 Figure 2.17 After confirming the inputs by pressing the OK button, the text strings are added to the graphic picture at a default position (i.e. at the top and from the left to the right of the graphic area). Note: The graph labels can be moved to their relevant positions if necessary (refer to next section for details). Moving Tags and Graph Labels Both, the identification tags and the graph labels can be moved easily with the mouse pointer. As soon as the pointer is placed onto a tag or label (or to its close vicinity) the shape of the cursor changes (Cursor 2 in Figure 2.10). The tag or label can then be moved to another place in all four directions by dragging it with the left mouse button pressed. The tag or label can also be removed by a double-click with the same mouse button. Moving Identification Bars The identification bars can be moved horizontally for adjustment using the mouse or the keyboard. Both methods are described hereafter. Note: The identification bars are only shown if the Tag Lines On/Off option is selected (checked) in the Options menu which is the default setting. With the Mouse When the vertical line of the cross matches with the red identification bar the shape of the mouse pointer changes (Cursor 3 in Figure 2.10). The identification bar can then be moved horizontally by dragging it with the right mouse button pressed. While the right mouse button is pressed the scan intensities corresponding to the identification bar position are indicated on top of the screen. Qualitative Analysis Chapter 2 AA83501 WinXRF Operator Manual 2-19 Figure 2.18 With the Keyboard With the Tab key the identification bars can be activated one by one and from left to right (or backwards with Shift + Tab) for displacement. The activated identification bar is shown in blue and can be moved with the left and right arrow keys. Not only the left and right arrow keys are available, but Shift + left and Shift + right arrow keys as well. The normal arrow keys move the line by the smallest screen unit while the Shift arrow keys move the line by a larger step to facilitate moving along the graph quickly. While an identification bar is active the corresponding scan intensities are indicated on top of the screen. Furthermore, an indication of the x-axis position of the bar is given in addition to the indications of the cursor position in the top right screen corner (figure below). Note: For printing the scan graphic no identification line should stay activated. This is achieved by repeatedly pressing the Tab key until all lines appear in red. Chapter 2 Qualitative Analysis WinXRF Operator Manual AA83501 2-20 Figure 2.19 Z Scale The Z - Scale function graduates the x-axis in atomic numbers of a selected X-ray series. This allows you to get a quick idea of which elements are present in the sample. On selecting this feature the operator is asked which spectral series he wants the x - axis scaled for, i.e. Ka, Kb, La, Lb, Ma or Mb. Figure 2.20 The next figure shows a scan with the x - axis scaled for the Ka spectral series. Qualitative Analysis Chapter 2 AA83501 WinXRF Operator Manual 2-21 Figure 2.21 Because the process uses Moseley's Law who established a relationship between atomic numbers and 2 Theta angles the accuracy is limited in some cases to +/- 1 atomic number. In the right top corner the system displays the intensity (y - axis), the atomic number and the name of the element (x - axis) corresponding to the mouse pointer position. Differential Graph This function allows you to subtract one scan from another and to display the result graphically. This may be used to get a graphical result of a background subtraction, for instance. The function is invoked by selecting Add Difference Graph within the Display menu. Chapter 2 Qualitative Analysis WinXRF Operator Manual AA83501 2-22 Figure 2.22 From the two list boxes contained in the dialog box shown in Figure 2.22, the two scans can then be selected. Please note that the second scan is subtracted from the first one. Figure 2.23 Peak Resolution The following options contained in the menus Show and Options are used to determine the peak resolution either automatically or manually: Peak Details When this option is selected, the peak resolution of all identified lines will be calculated. If the option Peak Resolution On/Off is selected, the half peak position and the calculated Qualitative Analysis Chapter 2 AA83501 WinXRF Operator Manual 2-23 background are indicated with red lines in addition to the calculated peak resolution (see Figure 2.24). Furthermore, these indications are also printed. Remove Peak Details When this option is selected, all indications related to Peak Resolution will be removed. Manual Peak Resolution This option allows manual determination of peak resolution for those lines already identified, in case the system cannot find the optimum background positions because of heavy line overlaps. When this option is selected, a small list box appears allowing you to select the line for which this operation should be done. After the line is selected, the background positions found automatically are displayed. These lines can then be moved with the mouse cursor by pressing the right mouse button. As the relevant background positions are moved the new resolution is calculated interactively. Figure 2.24 Peak Resolution On/Off If selected, the half peak position and the calculated background are indicated with red lines in addition to the calculated peak resolution (see figure below). Furthermore, these indications are also printed. Chapter 2 Qualitative Analysis WinXRF Operator Manual AA83501 2-24 Figure 2.25 Peak Details Parameters The dialog box that appears when this option is selected, is used to specify the parameters to be applied for the determination of the Real Peak Position and the Peak Resolution. The value specified in the upper entry box determines in which range, relative to the peak maximum, the position of the peak maximum should be determined through interpolation. The values specified in the lower two entry boxes (Peak Resolution Calculation) fix the range in which the background has to be determined. Figure 2.26 Spectra Interpretation In interpretation of the spectra, the following comments may be useful in selecting and identifying element lines (see figure below): a) K lines are asymmetric because they are doublets, made up of K 1 and K 2 in close proximity. Qualitative Analysis Chapter 2 AA83501 WinXRF Operator Manual 2-25 b) K 1,3 lines are normally sharp and nearly symmetrical which is also the case for L 1 and L 1 lines. c) The relative proportions of the K, K, etc. lines should be as expected from the data tables (Blue Book), but the K may be diminished if an appreciable amount of an element with an absorption edge between the two peaks appears in the sample. The presence of an absorption edge normally causes a step in the background, which can be a clue to a change of sensitivity. d) With the ARL goniometers for crystals, other than PET and multilayers, peaks are normally found to be within 0.01 to 0.015 from the expected position unless apparently displaced by a large neighbouring unresolved peak. It should, however, be remembered that the step size (interval 2) used in recording the scan will have an influence on the accuracy of the peak position. e) For low angle scans where typically 0.03 is used, errors of at least half a step can occur since the peaks are displayed by joining up the measured points in the graphic picture. Figure 2.27 SEMI-QUANTITATIVE ANALYSIS Semi-Quantitative Analysis Chapter 3 AA83501 WinXRF Operator Manual 3-1 3 SEMI-QUANTITATIVE ANALYSIS Introduction Semi-quantitative analysis programs allow you to perform analyses of totally unknown samples without prior calibration of the instrument. This can be very useful in cases where an appropriate calibration is difficult or even impossible. It may also be a means of quick investigation. Two different programs are available and described in the following sections of this chapter: QuantAS (formerly ASQ) UniQuant QuantAS QuantAS operates on scans acquired using the goniometer. Altogether, 5 scans are used to cover the range of elements from F to U using the following crystal/detector/collimator combinations: Scan Crystal Detector Collimator 1 LiF220 SC Fine (0.15) 2 LiF200 SC Fine (0.15) 3 LiF200 FPC Fine (0.15) 4 PET FPC Fine (0.15) 5 AX06 FPC Medium (0.60) The five scans are grouped into a single scan file with the extension *.ASQ. Note: The five scans are stored in the files *.SC1 to *.SC5. The QuantAS scans can thus be examined in Scan Graphics through these files. Performing Analyses with QuantAS The analysis of unknown samples with QuantAS requires only a few inputs that have to be given prior to starting the analysis. Some of the inputs deal with the unknown sample itself, like the matrix type and the concentrations of unanalysed elements or components. All the other inputs are required for sample identification and to guide the QuantAS operations. Basically, the user has two options: A manual mode where the QuantAS scan is recorded and the system waits for the user to retrieve the scan in the QuantAS graphics mode and process it interactively, as described in Section Interactive QuantAS Analysis. An automatic mode where a complete processing with a concentration report is done. The QuantAS scan is of course always available even in this mode for post analysis user interaction. This automatic mode can be used to create a batch of QuantAS analyses on a series of unknown samples. Single QuantAS Analysis The single QuantAS analysis is invoked through the selection of Production / Analysis - QuantAS - Run Scans. Chapter 3 Semi-Quantitative Analysis WinXRF Operator Manual AA83501 3-2 Figure 3.1 The screen shown below will then be displayed. Figure 3.2 Semi-Quantitative Analysis Chapter 3 AA83501 WinXRF Operator Manual 3-3 The required inputs are described hereafter: Scan Time The scanning speed, and therefore the accuracy of the analysis is defined here. The longer the recording time the better the analysis of trace elements. The time required to record the full spectrum is about 10 minutes (Basic time). In order to achieve a better detection limit of the elements, the recording time can be increased by the Factor specified here. QuantAS Results Name of the QuantAS results file. Description This is a free text field which can be used to describe the type of analysis to be performed. Cassette (./+) The cassette number (= cassette position for 9400 and 9800 instruments) is entered here. A . symbol can be given if the cassette is on the lift, or the + symbol if the next cassette is to be analysed. Sample Identifier The sample identity fields and prompts shown in Figure 3.2 are an example. They can be defined with the Sample Identity Scheme function. Please refer to the Configuration Manual for more information. Options The option Processing after analysis is used to select the actions to be carried out automatically after recording the scans. As soon as the button Processing Options is pressed the dialog box shown in the figure below is displayed. Figure 3.3 Following options are available: Matrix Type The matrix type is input by the user depending on whether the sample is a metal or an alloy (Element), an Oxide (cement, geological, ceramics), a Fusion (diluted in a flux) or if the unknown sample is to be compared to a typical sample of the same matrix (QuantAS Standard). Chapter 3 Semi-Quantitative Analysis WinXRF Operator Manual AA83501 3-4 Note: For fusions, Li 2 B 4 O 7 is taken as the flux and the dilution ratio is, by default 1:10, e.g. 1 part of sample for 9 parts of flux. If a different dilution is used, then the Matrix Type Oxide should be selected and the ratio entered under Binder/Flux by specifying the corresponding weights. QuantAS Standard In case this Matrix Type is selected, then the QuantAS Standard matching the unknown sample can be selected here. Film Factor In case a sample is analysed with a film (loose powders, liquids, small samples, etc.) the absorption due to the film can be compensated by selecting the film used. Unknown Rest % In case a sample contains elements that can not be analysed with QuantAS, these can be declared here either as a pure element or as a compound. QuantAS takes into account the matrix of the unknown rest to determine the composition of the sample. Known Elements The known concentration of an element or a compound can be specified here, e.g. in the case of fusions and oxides prepared at high temperatures, loss on ignition occurs and this should be taken into account in determining the normalised concentrations. Further, the sample may contain elements, which are not analysed using QuantAS. For example, C and H in the case of plastics and polymers; B, N and O in other organic and inorganic matrices. QuantAS has the provision to introduce the concentrations of many elements and compounds, like: Li, Be, B, C, N, O, LOI (Loss on Ignition), etc. Note: The program normalises the final concentrations after taking into account the input values. In cases where this data is available, the QuantAS result achieved will be improved accordingly. Binder/Flux If the dilution of the sample differs from 1:10 (see Matrix Type), then the respective weights of sample and flux have to be entered here. Please note that in such a case the Matrix Type has to be Oxide. Similarly, if a binder is used, then the respective weights of the binder and the samples have to be specified. Options Print Scans The acquired scans will be printed in 4 parts: Part Wavelength Range (Angstroms) 1 0.4 - 1.8 2 1.8 - 3.8 3 4.5 - 8.4 4 9.2 - 22.0 Print Report The QuantAS result is printed automatically after each analysis. Store Results The QuantAS analysis is stored in the Results Database for later treatment. Note: The QuantAS results can be retrieved by specifying the task category UCN and by typing ASQ in the task name entry box. Semi-Quantitative Analysis Chapter 3 AA83501 WinXRF Operator Manual 3-5 Save as QuantAS Standard If a sample serves as a typical sample to improve the accuracy of unknown samples of the same type, then this option has to be selected. Once the inputs are confirmed with the OK button, the execution of the analysis starts immediately by performing automatically five scans on the sample. Multiple QuantAS Analyses In case a series of samples has to be analysed automatically the list of operations for each sample can be stored in a batch file. Please refer to Chapter Unattended Operation for detailed information about the batch operation. Interactive QuantAS Analysis The interactive mode lets you perform analyses on stored QuantAS scans. All standard QuantAS functions are available as menu functions. In addition to these, the possibility to modify the list of found elements is offered in this mode as well. The interactive QuantAS mode is invoked as shown in the next figure. Figure 3.4 This causes WinXRF to display the following screen. Chapter 3 Semi-Quantitative Analysis WinXRF Operator Manual AA83501 3-6 Figure 3.5 From the list box the stored QuantAS scans can be selected. As soon as the selection is confirmed, the five scans are displayed, juxtaposed to each other on the screen, as shown below. By default, the x-axis is scaled in decreasing Energy (keV) values and the intensities on the y-axis follow a linear-logarithmic scale. The available menu functions are explained hereafter. Figure 3.6 Display With the Get QuantAS File function, the recorded scans of a new sample can be displayed and the analysis performed. With the Add QuantAS Standard function, a QuantAS Standard can be selected if the analysis of the unknown sample is done by comparison with a typical sample. With the Remove QuantAS Standard function the standard can be erased from the display. Semi-Quantitative Analysis Chapter 3 AA83501 WinXRF Operator Manual 3-7 Options This menu offers the following x - and y - scales for the graphics display of the scans (Figure 3.7): X - Scale Y - Scale Energy (keV) Linear Wavelength (Angstroms) Logarithmic Linear-Logarithmic In addition to the display functions, the Show Found Elements option lists the elements, which have been identified by QuantAS in a list box (Figure 3.8). Figure 3.7 In order to check which peak is matched by such an element the Show function has to be selected after having chosen the element from the list box. Chapter 3 Semi-Quantitative Analysis WinXRF Operator Manual AA83501 3-8 Figure 3.8 The Show Scan Ranges function indicates the limits of the 5 scans. This function may be helpful in case a scan section has to be selected for investigation with the Scan Graphics function. Processing This menu contains the three functions shown in the figure below. Semi-Quantitative Analysis Chapter 3 AA83501 WinXRF Operator Manual 3-9 Figure 3.9 Selecting the Options function causes the system to display the dialog box shown in Figure 3.3 and allows you to specify details about the sample preparation and the nature of the sample, like the Matrix Type, Film Factor, Unknown Rest, Known Elements, etc., in order to improve the QuantAS result, as is described in Section Single QuantAS Analysis. Selecting the Manual Identification function causes the system to display two list boxes, as shown in Figure 3.10. The list box on the left contains all the elements, which were identified by QuantAS and the list box on the right side the remaining (eliminated) elements from among the 70 analysed by QuantAS. If an element has not been found, or if an element corresponds to an artefact rather than to a real peak, then the two element lists can be edited by transferring elements from one box to the other. This is done by double-clicking onto the corresponding elements. Chapter 3 Semi-Quantitative Analysis WinXRF Operator Manual AA83501 3-10 Figure 3.10 Note: The elements contained in the two list boxes correspond to the 70 elements that are analysed by QuantAS. They are displayed exclusively, e.g. an element contained in the first list is removed from the second list, and vice versa. The Complete Analysis function performs an QuantAS analysis on the displayed scan set. This process is instantaneous and the result is displayed automatically. Report This function displays the result of the QuantAS analysis on the screen, as shown below. Figure 3.11 Note: The intensities shown in the column Net Intensity correspond to the directly measured intensities as shown in the graphics. Whenever a calculation is performed, these intensities Semi-Quantitative Analysis Chapter 3 AA83501 WinXRF Operator Manual 3-11 will be corrected according to the latest drift correction. Therefore, a QuantAS analysis is only really valid a few days before or after the last drift correction (re-calibration). This time span depends on the overall stability of the instrument (see also Section Set up QuantAS Standards). A hardcopy can be obtained with the Print Report function and the result can be stored in the Results Storage Area with the Store Results function. ARL 9800 Application & Demo 20.05.98 09:33:56 QuantAS Semi-Quantitative Analysis Result ------------------------------------------------------------------------------- File Name: BOIL_C71.ASQ File Date: 03.04.98 12:20:42 Description: Boillat C71x23 Matrix Type: Element Sample Identity: Boillat C71x23 Net Intensity Concentration Normalised Elements (Kcps) (%) Concentration (%) Cu 554.424 87.1 % 83.8 % Zn 51.370 6.22 % 5.99 % Sn 11.541 5.35 % 5.15 % Pb 8.416 3.66 % 3.53 % Ni 4.338 0.739 % 0.712 % As 0.231 0.217 % 0.209 % Fe 3.437 0.190 % 0.182 % Sb 0.320 0.166 % 0.160 % P 0.225 820 ppm 790 ppm Mn 0.961 800 ppm 770 ppm Bi 0.078 380 ppm 370 ppm S 0.136 340 ppm 320 ppm Si 0.027 190 ppm 190 ppm Film: Binder/Flux: Concentration: 0.000 % Weight: 0.000 [g] Sample Weight: 0.000 [g] Scan time factor: 4 Total number of elements identified: 15 Sum before normalisation to 100%: 103.9 The function Save as QuantAS Standard is used to create a typical standard that can be used in future for the analysis of unknown samples of similar type employing a simple comparative procedure (see Section Set up QuantAS Standards). Print This function contains two options to print a hardcopy of the displayed scan graphics: Print Screen This option prints the scans as shown on the screen. Print Scans This option prints the shown scans in four parts with the identified peaks labelled. This option is only made available after a Complete Analysis has been performed. Scan Graphics This function is used to select one of the five scan sections, which will be used for the investigation with the standard Scan Graphics functions. Upon selecting this option the desired scan section has to be chosen whereupon it is displayed. Chapter 3 Semi-Quantitative Analysis WinXRF Operator Manual AA83501 3-12 Figure 3.12 After investigation of the scan section the Scan Graphics functions can be left with Return to QuantAS. Exit The QuantAS analysis and graphics function is terminated with this option. Set up QuantAS Standards The function Save as QuantAS Standard is used to save the analysis of a typical standard that can be used for the analysis of unknown samples of similar type employing a simple comparative procedure. Once, such an analysis is saved, the standard can be set up by selecting Production / Analysis - QuantAS - QuantAS Standards. Semi-Quantitative Analysis Chapter 3 AA83501 WinXRF Operator Manual 3-13 Figure 3.13 A dialog box containing the list of the available QuantAS standards and the functions to Delete, Amend or Copy a standard in the list. The Exit function closes the dialog box. Figure 3.14 In order to set up a QuantAS standard, the Amend function has to be used, which causes the dialog box shown in the next figure to be displayed. Chapter 3 Semi-Quantitative Analysis WinXRF Operator Manual AA83501 3-14 Figure 3.15 The items contained in this dialog box are described hereafter: Description This box contains the information about the sample or the analysis that was entered when the standard was measured. This information can be changed, if necessary. Compton Intensities (kcps) This group box shows two different intensities of the Rhodium Compton peak. The Nominal intensity corresponds to the measured intensity and the Corrected intensity corresponds to the final intensity that was corrected for drift and adjusted for the intrinsic sensitivity of the instrument. Please note that there should be no need to change these intensities; they are shown for investigation purposes only. Known Elements The concentrations of elements or compounds that are not measured with QuantAS can be specified here. If necessary, the name of an existing Compound can be changed through the corresponding entry box. Default Matrix The matrix specified here just serves as an indication. Element Details This function calls the dialog box shown in the next figure and is used to specify the true concentrations of the QuantAS standard. Semi-Quantitative Analysis Chapter 3 AA83501 WinXRF Operator Manual 3-15 Figure 3.16 The following items are contained in the dialog box: Add This function is used to add a new Element or Compound with the values specified in the corresponding entry boxes. Delete This function is used to delete an element or compound from the list. Update This function is used to update the values of an element or compound in the list with the values specified in the corresponding entry boxes. Nominal Net Intensity The intensity shown in this box corresponds to the intensity that has been adjusted to the intrinsic QuantAS calibration of the instrument. This is the intensity that is used to calculate the concentration of the unknown sample. Corrected Net Intensity The intensity shown in this box corresponds to the Net Intensity in the QuantAS analysis report. Therefore, if one wants to compare the intensities between the standard and the unknown sample, then this intensity should be compared to the Net Intensity in the QuantAS analysis report. Ratio with Compton If this option is selected, then the intensities of the standard and the unknown sample are first divided by the corresponding intensity of the Rh Compton line and these ratios are then used to calculate the concentration of the unknown sample. Please note that this option should only be selected, if the standard and the unknown sample are well defined, i.e., same size, all elements analysed, etc. If this is not the case, then the Rh Compton intensity will be greatly affected by the differences, and the result may be completely wrong. Certified Value The true concentration of the QuantAS standard can be specified here. Units The unit of the certified values can be selected between % and ppm or another unit can be specified in the corresponding entry box. Chapter 3 Semi-Quantitative Analysis WinXRF Operator Manual AA83501 3-16 Sample Identifier This function calls the dialog box shown in the next figure and is used to change or complete the sample identity of the QuantAS standard. Figure 3.17 Semi-Quantitative Analysis Chapter 3 AA83501 WinXRF Operator Manual 3-17 UniQuant The WinXRF software is used to measure the intensities of the element lines required to perform an UniQuant analysis. These intensities are stored in a named results file in ASCII format. This ASCII file is then imported by UniQuant and the calculation of the concentrations can be performed. Select User Database for UniQuant Measurements UniQuant requires special element lines in order to form large groups of lines, which are measured with the same conditions. This is why a dedicated WinXRF database category has been set up for this purpose, containing the special line library. This reduces the danger that the parameters of any of these lines are altered inadvertently. If the Database Mask is set up appropriately, then there is no need to select a separate WinXRF database for UniQuant. This is indicated by the presence of the UniQuant programs and tasks in the list boxes of the UniQuant menu functions. However, if an older version of WinXRF has been updated and if the database inclusion has not been performed, then the UniQuant parameters are stored in a separate database. In such a case, this special database has to be selected (as before) to measure samples for UniQuant evaluations, as is shown in the figure below. Note: It is strongly recommended to perform the database inclusion as is described in the WinXRF Configuration Manual. Chapter 3 Semi-Quantitative Analysis WinXRF Operator Manual AA83501 3-18 Figure 3.18 The path of the user database is selected in the standard Windows way, i.e. by double-clicking onto the [..] symbol to select the next higher directory level, and subsequently onto UQ2, UQ3, UQ4 or UQ5 (see figure below). Figure 3.19 Semi-Quantitative Analysis Chapter 3 AA83501 WinXRF Operator Manual 3-19 UniQuant Menu The WinXRF software includes a special Main Menu item with three functions which are dedicated to UniQuant analyses, as shown in the figure below. Figure 3.20 Generally, in order to perform any UniQuant measurement (i.e. measuring CAL samples, MONITOR samples, Unknowns, samples to evaluate the "Film Factors", etc.) the three menu functions have to be executed from right to left. Please note however, that normally the programs necessary are prepared already and therefore only the following steps have to be executed for a UniQuant analysis: 1) Prepare the UniQuant measuring task. 2) Measure the intensities. 3) Import the intensities into UniQuant. 4) Calculate the concentrations. Prepare UniQuant Measuring Tasks The following steps are to be executed to create a measuring task (see Figure 3.21 and Figure 3.22): UniQuant Prepare Tasks Create (enter name:UNKNOWN) OK Chapter 3 Semi-Quantitative Analysis WinXRF Operator Manual AA83501 3-20 select _UQ from Programs list enter optional Description enter name of Results file enter Sample ID in Sample List Append repeat for remaining samples OK Exit Figure 3.21 Unlike in standard WinXRF measuring tasks, the analytical programs are also part of the task list in the special UniQuant measuring tasks. Therefore, it is very simple to set up an UniQuant task to run samples with various programs. Note: It is recommended to always enter a new Result Name in order to avoid that results which already exist are erased before they have been processed with UniQuant. Alternatively, make sure that the option Append to existing file is selected. Figure 3.22 Semi-Quantitative Analysis Chapter 3 AA83501 WinXRF Operator Manual 3-21 Sample Identification The three sample identification fields provided for UniQuant measurements are fixed and are to be set up in the following way: Sample Name Sample Number UniQuant Identification free field free field EJOB.x (X=1 - 999) free field free field NJOB.x (x= 1 - 999) The choice of NJOB or EJOB affects the import of JOBs as follows (see Section Prepare UniQuant Measuring Tasks): *JOB File exists in UniQuant File doesnt exist in UniQuant N (New) Existing General Data are not affected, except: the Application description from the sample identification is taken. Intensities are first set to blank, then Intensities are imported. File is created and General Data are set at default values, but the Application description is taken from the sample identification. Intensities are imported. E (Existing) Existing General Data are not affected. Intensities are imported. Same as above. Measure Intensities for UniQuant After having prepared the tasks for various purposes, the measurement can be started by the execution of the following steps (see also figure below): UniQuant Measure Intensities Select UniQuant Task from the list box OK As soon as the OK button is pressed the list of samples to be measured is copied into the ICS Operations Manager. The evolution of the measurement can be followed by opening the ICS Operation Manager by clicking on the corresponding icon on the task bar (see Figure 3.24). Figure 3.23 Chapter 3 Semi-Quantitative Analysis WinXRF Operator Manual AA83501 3-22 Figure 3.24 An UniQuant task can also be included as a step in a batch (refer to Chapter Unattended Operation) or added to the ICS Operations Manager by selecting the UniQuant button and a subsequent selection of the task to be executed from the displayed list box (same as in Figure 3.23). Import of Intensities The WinXRF software has been adapted to facilitate the transfer of the measured intensities to UniQuant. The intensities are stored directly in a named ASCII file in the user directory. The name of the results file is specified in the measuring tasks (see Section Prepare UniQuant Measuring Tasks). These files can then be imported directly into UniQuant for further treatment. Note: The description that follows is related to UniQuant Version 4. Because there are small differences with respect to former versions of UniQuant, the user is asked to consult an older WinXRF manual for an exact description of the installed UniQuant version. The file to be imported is selected in the following way: Start the UniQuant program by double-clicking the corresponding shortcut. Before the menu Main Menu is displayed, the system reads in tables and performs some checks and calculations, as commented on the bottom line of the screen. After a few seconds the following menu is displayed: Semi-Quantitative Analysis Chapter 3 AA83501 WinXRF Operator Manual 3-23 Figure 3.25 From the two available possibilities it is strongly recommended to select option J for Menus for JOBs only to continue as the screens shown hereafter are related to this mode of operation. Furthermore, the full mode includes all menus and functions used during the UniQuant calibration procedure and thus gives access to the calibration data that should remain untouched. Figure 3.26 Then, the function I for IMPORT of intensities has to be selected. Chapter 3 Semi-Quantitative Analysis WinXRF Operator Manual AA83501 3-24 Figure 3.27 In order to import the intensities, the appropriate file has to be selected, by pressing I for import from \name of database path. At the displayed screen, the existing result files will then be displayed, sorted in reverse chronological order (i.e. the youngest at the top, the oldest at the bottom). The file to be imported is selected by moving the highlight onto it and pressing the right arrow key or the right mouse button. Figure 3.28 While importing, the process of breaking up the intensity file into separate JOB files (one for each sample) is displayed on the screen. Semi-Quantitative Analysis Chapter 3 AA83501 WinXRF Operator Manual 3-25 Figure 3.29 After completion, you should return to the Main Menu, by confirming the message that appears as soon as the intensities have been imported. Calculate Concentrations After having imported the intensities into UniQuant, the actual evaluation of the analysed samples can be started. At this point it is suggested that the user gets familiar with the UniQuant commands by selecting K for KEYS conventions in the JOBS menu and then clicking onto the various commands to get an explanation of their function. Especially, the keys F2 for printing and F1 to go backwards should be remembered. Figure 3.30 Chapter 3 Semi-Quantitative Analysis WinXRF Operator Manual AA83501 3-26 The next step consists of entering the job number by typing J and the number in the subsequently displayed entry box at the bottom of the screen. After confirmation with Enter, the menu shown below is displayed. Figure 3.31 When a job is treated for the first time, the next step consists in typing G and the screen shown below will be displayed. Figure 3.32 The available functions are shown on the top of the screen. In order to change any of these items E has to be pressed, causing the cursor to jump onto the first line of the editable part of the screen. With the up and down arrow keys the cursor can be moved from one line to the next. For a first evaluation of the unknown sample, it is recommended to consider the following specifications only: Semi-Quantitative Analysis Chapter 3 AA83501 WinXRF Operator Manual 3-27 1) Select Elements or Oxides. 2) Select 1 = Teflon for Shape & ImpFc. 3) If the sample was run in Helium atmosphere, select 1. 4) If a Film was used, select 1 for 6 and 2 for 4 Polypropylene film (Standard film factors). 5) Put the value for the Height to 0. When done, the changes and inputs have to be confirmed by pressing F1. By pressing F1 a second time the former menu is displayed again. If we now check the Intensities by typing I, the screen below will be displayed. The shown data is what has been imported from the WinXRF result file, i.e. the name of the lines, the measured gross intensities and the counting times. All other columns will be filled after a calculation has been performed. Please note that the next and previous pages can be displayed by pressing the Page Down and Page Up keys. This screen is left by pressing F1 and the former menu is displayed again. Figure 3.33 Because the column CalcBg is empty, the next function to be used is C causing Uniquant to determine the backgrounds prior to calculating the concentrations of an unknown sample. In our example we are assuming that all elements in the sample have been measured with the X-ray technique and the sample is well defined. Thus we have chosen case number 0: Case number : 0 = Known Mass, Area, Rest, Dilution Because in such a case the equation system is over determined, the iteration process is adjusting the Viewed Area of the sample to correspond to the sum of the calculated concentrations, where 490.63 = 100%. Once the calculation is finished the found concentrations are displayed on the screen. All elements with a concentration below the detection limit (10 ppm in this case) are marked with a < sign. Elements for which the concentration is smaller than twice the calculated standard error are marked with <2e. Chapter 3 Semi-Quantitative Analysis WinXRF Operator Manual AA83501 3-28 Figure 3.34 In order to see the details of the light and the rare earth elements the key L has to be pressed. By setting the detection limit to 0 all concentrations will be displayed. This is done by typing P and entering 0 in the subsequently displayed entry field. If the concentration calculation was performed on an oxide basis the oxygen can be stripped off by typing O. On the print-out the amount of stripped oxygen is indicated. The result screen is left by typing F1 causing the system to display the former menu. The menu has been further extended. The function Report to client (R) displays the result screen again. The other four functions are explained hereafter. Figure 3.35 Semi-Quantitative Analysis Chapter 3 AA83501 WinXRF Operator Manual 3-29 The option Measuring order, results displays detailed information on how the final result was achieved. In this table the order in which the element lines are listed is the measuring order. The option Z order, results is similar to the option described above but in this case the order of the element lines is given in ascending atomic numbers. The last two options S and A allow you to display the result in a short form. i.e. only the elements with a concentration above the display limit (detection limit) and higher than the Standard Error are displayed, either in the order of decreasing concentrations (S), or in alphabetical order (A). Figure 3.36 Once a calculation has been performed, the Intensity table looks like shown below, i.e. most of the columns are now filled out and a new option has been added to the menu, M = Make Subset. This feature is explained in Section Convert a Subset into a measuring Program. Chapter 3 Semi-Quantitative Analysis WinXRF Operator Manual AA83501 3-30 Figure 3.37 More advanced Features in UniQuant This section has mainly been written to draw the attention to more elaborated features in UniQuant. The user is however asked to consult the UniQuant Manual or On-Line Help for supplementary details about the features explained here. Define Materials It quite often happens that there are elements in the sample that are difficult or even impossible to measure with the X-ray technique. such elements are H, Li, Be, B, C, N and O. If this is the case, it is important to include these elements in the calculation of the final result. Because, especially the very light elements have a big influence on the mass absorption it is also very important to know the composition of an unknown rest, as for instance, CH 2 has not the same effect as C 15 H 6 O 2 . The stoichiometry of such a rest or known concentration, binder or flux can be defined with the option Materials. Please note that %KnownConc is always a fixed value, but %Rest may be a fixed value or can be calculated by UniQuant. Semi-Quantitative Analysis Chapter 3 AA83501 WinXRF Operator Manual 3-31 Figure 3.38 A total of 64 different materials are available of which the first 8 are fixed and the remaining 56 are user definable. Pressing the M key displays the first 8 materials, further group of 8 materials are shown by using the Page Up and Page Down keys. Figure 3.39 A material within the group of eight materials is selected by entering its number (1 to 8). The materials can be defined in two ways: 1) Specify the stoichiometry of the material, and once the cursor is on the Wt% column, Ctrl C will automatically calculate the corresponding weight percentages. 2) Specify the elements and enter the weight percentages manually. Chapter 3 Semi-Quantitative Analysis WinXRF Operator Manual AA83501 3-32 Viewed Mass The viewed mass is an important parameter if the sample is not infinitely thick for all element lines. This is often the case for element lines of the first group (between BaKa and MoKa), especially in loose powder or liquid samples. In such a case, it is good practice to weigh the sample and to calculate the viewed mass as follows: Viewed Mass = Sample weight * (Liquid cell diameter [mm] / 25mm) 2 The found weight is then specified under Mass in General Data. This calculation can also be done in UniQuant by specifying the sample weight (Gross) and the diameter of the liquid cell (Gross). The weight corresponding to the Viewed Mass is then automatically calculated. Furthermore, UniQuant calculates the height of the sample by taking into account the specified density Rho. The height of the sample may have a big influence in case the sample is not infinitely thick. Therefore, if the density of the sample is unknown, then the height can be input directly. Area [mm2] = 490.63 Diameter [mm] = 25.00 42.0(Gross) Mass [mg] = 2657 7500(Gross) Rho [g/cm3=mg/mm3] = 1.1 Height [mm] = 4.92 Note: The viewed area with a diameter of 25 mm corresponds to the effective diameter of a standard cassette with an opening of 29 mm. A weight of 18000 mg defines an infinitely thick sample. Depending on the matrix and the viewed mass, the fluorescence yield will then be calculated correspondingly. The effect is easily observed for elements between BaKa and MoKa by comparing the result obtained with a viewed mass of 18000 and the result with the real weight. If the sample is not infinitely thick, the latter concentration of these elements is higher. Another way of detecting if a sample is not infinitely thick for all measured element lines is explained in the next section. Alternative Lines The following elements can be measured with an alternative line: Element Standard Line Alternative Line Ba Ka Lb Cs Ka La I Ka Lb Te Ka La Sb Ka Lb Sn Ka La In Ka Lb Cd Ka La Ag Ka Lb Pd Ka La Rh Ka La Ru Ka La Mo Ka Lb Nb Ka La Th Lb La Zr Ka La Semi-Quantitative Analysis Chapter 3 AA83501 WinXRF Operator Manual 3-33 Y Ka Lb Sr Ka La Pb Lb La Br Ka Lb As Kb Ka Se Ka La W Lb La Ga Ka Lb Ta La Lb Cu Ka Lb Lu La Lb Ni Ka Kb Co Ka Lb Fe Ka Lb Sm Lb La Eu La Lb Pr Lb La Ce Lb La V Ka Kb Ti Ka Kb Ca Ka Kb The alternative lines are displayed in brown colour and marked by an asterisk sign between the line number and the line name in the intensity table. When the cursor is moved to the left and then up and down it only stops at lines for which an alternative line exists. In order to select the alternative line, the asterisk is either removed by pressing the space bar if the cursor is located on the active line, or inserted if the cursor is located on the passive line. UniQuant automatically switches the corresponding lines On or Off. Figure 3.40 Chapter 3 Semi-Quantitative Analysis WinXRF Operator Manual AA83501 3-34 Figure 3.41 Please note that most of the alternative lines are L lines. This means that a comparison between the concentration calculated for the very energetic K lines with the one found for the corresponding L line may indicate that the sample is not infinitely thick. This is certainly the case if the concentration of the L line is much higher than the one of the K line for a given element. By specifying the correct weight of the sample (Mass) the concentration of the K line should not be very different from the concentration of the L line (see also Section Viewed Mass). Note: With the %Yield value in the intensity table an additional possibility exists to see whether the sample is infinitely thick for all element lines. This value indicates the relative fluorescence yield for each line. Case Numbers Because UniQuant assumes that all elements in the sample are measured and that for each element there exists a relationship between the measured intensity and the concentration (Kappa value) the system is normally over determined. This fact allows determination of an extra value if the sample is not fully determined in terms of one of the following 3 specifications: Area Rest concentration Dilution Case 0 This is the case number to start with if the sample is totally unknown. The sum before normalisation may show what other case number could improve the final result (e.g. unknown rest). Case 1 Normally, UniQuant applies implicitly this case if everything is deemed to be determined. However, if the sample is smaller than 29mm in diameter, it is meaningful to calculate the estimated area rather than the sum before normalisation. Please note that this only influences the result cosmetically. Semi-Quantitative Analysis Chapter 3 AA83501 WinXRF Operator Manual 3-35 Case 2 This case is probably the most useful case number if the sum before normalisation is far below 100%. But it is very important to know exactly the chemical composition of the unknown rest because the composition influences the sensitivity of the detected elements (see also Section Define Materials). Case 3 This case is normally seldom used because it is related to the sample preparation which should be known. If, however, a sample is analysed for which the dilution is unknown, this case is used to find the dilution of the sample preparation. Note: The two special case numbers 4 and 5 will not be explained here; the reader is asked to consult the UniQuant Manual for explanations about these. Figure 3.42 It should be quite clear that for case 2 and 3 it is essential to specify an initial concentration or dilution with the appropriate material code. The better the material code is defined the more accurate the final result will be. For the unknown rest concentration to be determined through iteration, it is not really important what is specified as initial concentration, but the correct order of magnitude may speed up the calculation, especially if the computer is not of the latest generation. Convert a Subset into a measuring Program UniQuant offers the possibility to create measuring programs with a reduced number of element lines, by simply setting the counting time of unwanted element lines to 0 in the Intensity table. These features may then be very useful if a complete category of elements are not present in a batch of samples, for example, the rare earth elements or the precious metals. On the contrary, it may also be used to improve the accuracy of important elements by increasing their counting times, or a combination of both. Note: Under Helium atmosphere the total analysis time is restricted to 15 minutes for security reasons as a long exposure to X-rays destroys the thin film and thus severe contamination of the spectrometer may occur. The option to actually create the subset program is only available after a calculation has been performed, in which case the JOB menu should look like the one below, i.e. the menu is fully extended. Chapter 3 Semi-Quantitative Analysis WinXRF Operator Manual AA83501 3-36 Figure 3.43 Some rules need to be respected when selecting the lines to eliminate, as especially neighbouring lines are important for the determination of the backgrounds (see Chapter 6, Section 8 of the UniQuant Manual or the On-Line Help for more details). First of all, it is important to notice that the appropriate function is only available after a concentration calculation has been performed. The reason for that is simple: The result after elimination of unnecessary lines should be comparable to the analysis with all lines. If this is not the case, some of the eliminated lines should be included again to improve the background calculation and thus the final result of the subset program. Secondly, the elimination of unwanted element lines should be done by measuring groups. This is because, for each group, the background calculation is done separately. This fact therefore allows all elements to be eliminated of a same group if they are of no interest. Each group of elements is shown with a different colour. Thirdly, the special background lines should not be eliminated or only, if a whole group of elements is of no interest. Finally, only the comparison between the result obtained with the complete measuring program and the restricted one gives the assurance that the choice of eliminated lines is suitable. Semi-Quantitative Analysis Chapter 3 AA83501 WinXRF Operator Manual 3-37 Figure 3.44 After the subset was defined, the option M = Make Subset creates an ASCII file, with the extension UQS. The name of this subset program can be specified in the subsequently prompted entry box. WinXRF uses then these parameters to construct a standard UniQuant measuring program. The following print-out shows the structure of such a subset file. "....,....1....,....2....,....3....,." " MgKaUQ MgKa 45.08 30 30 80 0" " GaLbUQ GaLb 50.59 30 30 80 0" " NaKaUQ NaKa 54.98 30 30 80 0" The corresponding WinXRF measuring program can now easily be created with the following steps (see Figure 3.45 and following figures): UniQuant Prepare Program Create (enter name) Retrieve (select name of subset) OK Amend (check program) OK OK The measuring program created in this way contains all element and background lines in the measuring order. This reduces the total measuring time because of minimum goniometer movements and tube condition changes. Chapter 3 Semi-Quantitative Analysis WinXRF Operator Manual AA83501 3-38 Figure 3.45 Figure 3.46 Semi-Quantitative Analysis Chapter 3 AA83501 WinXRF Operator Manual 3-39 Figure 3.47 QUANTITATIVE ANALYSIS Quantitative Analysis Chapter 4 AA83501 WinXRF Operator Manual 4-1 4 QUANTITATIVE ANALYSIS Introduction An Analysis is the operation to determine the concentration values of unknown samples from measured intensities received from the instrument. Before an analysis can be performed, the WinXRF software must be configured for the samples to be measured. This means that the following has been set up previously and where necessary the required operations performed as this is described in the WinXRF Configuration Manual: the required Setting-up Samples and Control Samples. the required Analytical Programs. the Drift Correction, i.e. Initialisation and Update. the Instrument Calibration, i.e. Line Overlap/Background corrections, Response Curve determinations, Base Curve calculations and Matrix corrections. the Analytical Tasks. the required Type Standards. an SPC Initialisation, if this option is included. In some cases it is useful to acquire only intensities of unknown samples. In this case, the intensities will not pass through the different intensity calculation stages and thus are not subject to any corrections stored in the analytical program. To perform such analyses in intensity mode, a special task is provided in the system, as explained in Section Intensity Measurements. In concentration mode, the WinXRF software offers different possibilities to analyse unknown samples. Depending on whether a quality check, a type standardisation or a quality check followed by a charge correction is required, the corresponding tasks, the type standards and the qualities need to be prepared correspondingly. The different items are linked as shown in the following diagram. This diagram shows that the Qualities are always linked to either a Type Standard, or an Analytical Program, and the Type Standard to an Analytical Program. Normally, the Qualities are linked directly to the Analytical Program. Only in special cases the variant through a Type Standard is required. Chapter 4 Quantitative Analysis WinXRF Operator Manual AA83501 4-2 Concentration Analysis The analytical tasks to analyse concentrations in unknown samples can be run in different ways: If shortcuts have been defined, then a particular task can be run directly by a double click on the corresponding shortcut, either directly from the desktop or from the WinXRF shortcut folder. Figure 4.1 By simply pressing the function key F2. Through the selection of Production / Analysis - Analysis - Concentration Analysis. Quantitative Analysis Chapter 4 AA83501 WinXRF Operator Manual 4-3 Figure 4.2 If the analysis is started through a shortcut, then the task and program that have been defined in the shortcut will be selected. On the other hand, if the analysis is started through the F2 function key or Concentration Analysis icon, WinXRF brings up the task and the program that has been run the last time. If this function is used for the first time, or if the task that was run the last time does not exist, the screen will be greyed and the operator will be asked to specify the task he wishes to run. This is done by selecting the Change Task function (see Section Change Task). Chapter 4 Quantitative Analysis WinXRF Operator Manual AA83501 4-4 Figure 4.3 Change Task There may exist many different tasks that have been prepared for various applications with different degrees of automatic operation. The degree of automatic operation can easily be selected by choosing the appropriate task. Depending on whether the chosen task was set up in manual sample mode (no sample list defined) or in pre-defined sample mode, a dialog box similar to the one shown in Figure 4.3 or in Figure 4.6 is displayed. The Change Task function brings up the screen shown below enabling the operator to select the task from the list box. Quantitative Analysis Chapter 4 AA83501 WinXRF Operator Manual 4-5 Figure 4.4 WinXRF automatically proposes the Quality, Type Standard or Analytical Program that has been defined as the default program in the currently selected task. The Analytical Program can also be changed, using the Select function. However, the Analytical Program can only be selected from the categories that have been enabled in the current task. The disabled categories will be shown with an empty and greyed list box. Change Program The program (Quality, Type Standard, Analytical Program) can be changed by either typing the new name into the corresponding entry box or by using the Select function. Only list boxes of enabled categories are activated for selection of the program to be run with the chosen task. Furthermore, only the programs of the working category are displayed in the corresponding list boxes. However, if a program from another category has to be selected, then this category has to be chosen first from within the Database Category combo box. Chapter 4 Quantitative Analysis WinXRF Operator Manual AA83501 4-6 Figure 4.5 Manual Sample Mode In manual sample mode, the sample identity together with the manual inputs, if defined in the selected analytical program, need to be entered at run time. This can be done in two different ways (see Figure 4.3) : 1) The various entry fields are selected step by step and the corresponding data entered. The Sample Details OK button is then clicked to confirm the inputs and to start the analysis. 2) The analysis is started immediately by clicking onto the Analyse button. While the sample is being analysed the various fields may be completed. When the identification has been completed, you click the Sample Details OK button. Note: At least one field must be specified. Manual Inputs always need to be entered (see Figure 4.6). WinXRF only ejects the sample and prints the result after you click the Sample Details OK button. Pre-defined Sample Mode In pre-defined sample mode the samples defined in the sample register are analysed one after the other. When a task with a pre-defined sample list is called the system proposes the first sample specified in the sample register. Quantitative Analysis Chapter 4 AA83501 WinXRF Operator Manual 4-7 The analysis of each sample is started by clicking the Sample Details OK button. At the end of the analysis the next sample is automatically proposed and the same procedure applies. In case the sample details have to be changed (Identity or Manual Input Value) the procedures are the same, as described in the preceding section. Figure 4.6 Recalculate This function is used to recalculate the concentrations of already analysed samples. This may be useful if a drift correction or a type standardisation was deemed to be necessary after a batch of samples has been measured already. Please refer to Chapter Analysis Recalculation Option for details about this function. Metaverage This function allows you to invoke the metaverage operation. See Chapter Metaverage Option for details about this. Bad Sample Analysis This function allows you to create a Bad Sample result before the analysis is started, by pressing the corresponding button and confirming the subsequently appearing warning message (figure below). A dummy result is then created which indicates that the sample was unsuitable for a quantitative analysis. Please note that this option has been introduced for the purpose of optical emission analyses where it often happens that a sample can not be sparked. For statistical reasons it is necessary to keep track of such samples. For X-ray fluorescence analyses this option is seldom used. Chapter 4 Quantitative Analysis WinXRF Operator Manual AA83501 4-8 Figure 4.7 Bad analyses can also be detected automatically by checking the validity range of declared Pseudo Elements. If any of the Pseudo Elements for which a validity range was specified fails, the analysis is deemed to be bad, and a warning message is given. The Pseudo Elements that failed will be marked by { if the value is below, and } if the value is above the validity range. Furthermore, such an analysis is marked with a 'x' symbol which is also printed and sent to remote destinations set up for the telex formats. Figure 4.8 Automatic Drift Correction Control When a concentration analysis is started, WinXRF controls whether it is necessary to run the Setting-up Samples and/or the associated Type Standard (if used) to compensate for instrumental drift, by checking if the time between drift correction updates has elapsed. If this is the case, WinXRF lists the samples which need to be run (Type Standard or Setting-up Samples). Please note that normally only one type of samples is used for drift correction (Setting-up Samples) but there may be situations where you may want to perform a quick update with only one Type Standard rather than to measure all Setting-up Samples. This automatic control works for Setting-up Samples and Type Standards. Depending on whether the analysis is performed by calling an Analytical Program or a Type Standard, WinXRF prompts the user to decide whether the corresponding samples have to be run. If no time period was specified then this control is not performed. Quantitative Analysis Chapter 4 AA83501 WinXRF Operator Manual 4-9 Setting-up Samples Normally, the drift correction is controlled by Setting-up Samples. In case a time period was specified in these samples this time is checked and if it has elapsed all the corresponding samples are prompted to be run to drift correct the selected analytical program. Figure 4.9 If the decision is taken to run these samples, the system automatically sets up the Drift Correction Update task DEFAULT to acquire the actual intensities of the corresponding element lines. Figure 4.10 After the drift correction update has been performed WinXRF returns to the concentration analysis and the analysis can then be continued in the normal way. Please note that this automatic drift update only works in manual mode, i.e. Routine Analysis. Type Standards In special situations a Type Standard may not only be used to adjust the calibration curves to a specific type of samples but it may also be used for drift correction. In this case, the corresponding option was selected and a value for Hours between Updates was specified. This time period is checked and, if it has elapsed, WinXRF issues a message to warn the user that the selected Type Standard should be updated (figure below). Chapter 4 Quantitative Analysis WinXRF Operator Manual AA83501 4-10 Figure 4.11 Enter EXAN Data The devices connected to the spectrometer for the analysis of elements and components that can not be analysed by the XRF technique should normally send the required values before the XRF analysis is finished. In such a case, the values are automatically included in the final result and the system will be ready for the next analysis. On the other hand, if the results from the External Analysers are not ready by the end of the XRF analysis, the following dialog box appears. WinXRF will then wait until the data has been received, or the required data has been entered manually. Figure 4.12 Colours and Result Flags During a quantitative analysis various checks can be performed by the system. A failure of such a check is indicated by a special background colour and a result flag in front of the result value. If the option Colour for results output is selected, the results that failed a check are given on different background colours on suitable colour printers. The font style can also be selected among Normal, Bold, Italic and Bold-I talic. Flags and font styles are stored and transmitted with the results, the colour not. Therefore the flags are not changeable, but the background colour can be defined individually for each kind of result within a task (see WinXRF Configuration Manual). Each type of event on a run or average can set colours and fonts. The following figure shows the default colours and font styles defined in WinXRF, and where applicable the fixed flag assignment. Quantitative Analysis Chapter 4 AA83501 WinXRF Operator Manual 4-11 Figure 4.13 Chapter 4 Quantitative Analysis WinXRF Operator Manual AA83501 4-12 Figure 4.14 Print-out Example: 12-Apr-94 10:42:06 Sample: 1298-1 45 9967 5 final xrf 13-Apr-94 ARL/Fisons Quality: CHARGE Task: _KJ Run Co Cr Cu Mn Mo Nb Ni P S Si Ti 1> (0.41 )12.78 0.34 <1.40 5.26 0.41 >66.53 1.045 !0.000 0.06 0.041 V W Fe-DIF 1> !0.00 >2.60 9.13 Execution of Analysis Features Once the Sample Identity and the Manual Inputs (if there are) have been entered and confirmed, the system displays the screen shown in the next figure. If the Manual Run Selection has not been selected the Abort button is the only function that is enabled, and on the contrary the Deselect Runs button would be activated as well. The analysis can at all time be aborted by clicking onto the Abort button. In that case the sample currently being measured will be ejected immediately and the system returns to the former screen (Figure 4.6). To guide the operator, instructions are given dynamically on the bottom line of the screen. Quantitative Analysis Chapter 4 AA83501 WinXRF Operator Manual 4-13 Figure 4.15 Manual Run Selection Although this feature is only seldom used in X-ray analyses (but very often in optical emission spectrometry) it is nevertheless briefly explained in this section. When the analysis of all runs is terminated all runs are selected, by default. Already during and at the end of the analysis the user has the choice to remove individual measurements from the average result and the statistical calculations, provided that the appropriate options have been enabled in the task, i.e. Manual Run Selection, Display Sigma and Display Relative Sigma. The runs are selected/deselected by clicking onto the left border area where the > symbols are displayed, in front of the individual measurements (figure below). The statistical calculations are dynamically corrected whenever runs are selected or deselected. Chapter 4 Quantitative Analysis WinXRF Operator Manual AA83501 4-14 Figure 4.16 All runs are deselected by clicking onto the Deselect Runs button causing the statistical calculations to disappear. This action also causes that the function of this button is changed to Select all Runs allowing the selection of all runs again by clicking onto the same button, if necessary, or individually by clicking onto the left border area in front of the run to be selected. Figure 4.17 The individual run selection is terminated by clicking onto the Analysis Complete button and access is then given to the selected analytical options and features, e.g. Print, Quality Check, etc. as shown in the figure below. These are executed or can be executed, depending on their specified mode. For instance, if Paged Mode Deferred is set for printing, then printing will only be performed once there is enough to fill a complete page. Quantitative Analysis Chapter 4 AA83501 WinXRF Operator Manual 4-15 Figure 4.18 Analyses with Quality Check The quality checking facility permits the result to be checked against a set of upper and lower limits. This check is performed automatically at the end of the analysis under two conditions: a) The Quality Check option was selected in the current task. If this is not the case, the Quality Check button will not be enabled for selection. b) The analysis was performed through a Quality. If this is not the case, i.e. the analysis was performed through a Type Standard, or directly with the Analytical Program, the quality check is not performed automatically. It is however yet possible to perform the quality check by first selecting the quality from the list box the system displays when the Quality Check button is selected, as shown in Figure 4.20. Chapter 4 Quantitative Analysis WinXRF Operator Manual AA83501 4-16 Figure 4.19 All elements outside the quality specification are flagged '>' for over or '<' for under specification. An example of a typical result output with a quality check is shown in Figure 4.18. A table listing the elements that have failed the quality check, with the corresponding quality limits, can be obtained through the Quality Check function (figure below). The Print Result option allows you to get a hardcopy of this check. The Select Quality function allows the result to be checked against another quality, by selecting the alternative quality from the list box and the new quality check result will be displayed after having confirmed the quality selection. Figure 4.20 If the analysis has passed the quality check, the message: ***** Quality Check Successful ***** Quantitative Analysis Chapter 4 AA83501 WinXRF Operator Manual 4-17 is displayed in the scroll box. If, however, there are elements outside the charge correction limits the warning message shown in the figure below is given in addition to the indication that a charge correction might be necessary. Figure 4.21 Analyses with Quality Sort The Quality Sort facility permits the result to be checked against a set of qualities in order to find the quality that best matches with the analysed sample. The tightness of the matches is indicated by a variance value, of which the mathematics is given in the WinXRF Configuration Manual. The quality sort can be performed, if the Quality Sort option has been selected in the current task, by clicking onto the corresponding button. This causes the dialog box shown in Figure 4.22 to be displayed. In the list box on top, all Quality Sort files matching with the matrix of the analysed sample are proposed for selection. Note: Lists of qualities of similar types are defined in Quality Sort files, as explained in the WinXRF Configuration Manual. As soon as a quality sort file has been selected, by clicking onto the Select button the sort result is given in two separate lists, on the left for qualities matching with the result, and on the right where not all elements are within specification. Chapter 4 Quantitative Analysis WinXRF Operator Manual AA83501 4-18 Figure 4.22 Analyses with Charge Correction The normal charge correction procedure is interactive and it is therefore required that analyses are performed in manual mode by selecting the Concentration Analysis <F2> function (see Figure 4.2). In case one tries to perform an analysis in unattended mode or using the batch operation, a warning will be reported as shown in the figure below. Quantitative Analysis Chapter 4 AA83501 WinXRF Operator Manual 4-19 Figure 4.23 Note: Charge correction can also be used with an Automation System and, in such a case, requires no operator involvement. This procedure is described in the WinXRF Configuration Manual. Perform Charge Correction As usual, WinXRF proposes the task that was run the last time together with the Default Program (Quality, Type Standard or Program) defined in the task set-up. If the task needs to be changed, this can be done using the Change Task button (next figure). Chapter 4 Quantitative Analysis WinXRF Operator Manual AA83501 4-20 Figure 4.24 The quality can be changed either by entering its name directly into the appropriate field or by using the Select button. After having confirmed the Sample Identity, the screen in Figure 4.25 is displayed and the various options may be executed once the analysis is completed. Figure 4.25 Quantitative Analysis Chapter 4 AA83501 WinXRF Operator Manual 4-21 Note: If the analysis was performed through a quality, the quality check is done automatically at the end of the analysis (Figure 4.25) and a Charge Correction can be performed immediately. Conversely, if the analysis was not performed through a quality, the quality check has to be done manually, and a Charge Correction can then be performed. The following flow chart illustrates the steps to be executed in order to correct an existing charge. It also shows some special situations that could occur during the calculation. Please note that this applies to a charge correction at the end of an analysis and equally on a stored result: Normal Situation 1) Perform Quality check During the quality check, the analysed concentrations are compared to the Minimum and Maximum values (external limits) specified in the quality description. All elements failing the quality check are marked by '>' and '<' symbols indicating respectively above and below specification (see Figure 4.25). Chapter 4 Quantitative Analysis WinXRF Operator Manual AA83501 4-22 Note: The quality check is normally done automatically if the analysis was performed through a quality and the Charge Correction program can be started immediately. It is, however, also possible to first perform a quality check with a different quality prior to invoking the charge correction program. Figure 4.26 2) Invoke Charge Correction Depending on how the analytical task was set up, i.e. Manual, Semi-Auto or Auto, the charge correction program is either called, by using the highlighted Charge Correction button (Manual Mode), or the Continue button (Semi-Auto and Auto). The screen shown (see Figure 4.28) below will be displayed. 3) Enter Charge Weights The principle of charge correction is to correct an existing charge to yield a certain quality. This implies the initial charge weight to be entered. Because the capacity of furnaces is limited, the maximum charge weight can be specified to avoid overfilling of the furnace with material additions. Final charge weight = Initial charge weight + additions If the final charge weight is left to 0, no restriction on additions exists. Quantitative Analysis Chapter 4 AA83501 WinXRF Operator Manual 4-23 Figure 4.27 Note: If the Alternate Selection File in Charge Correction option and if the Rules for Alternate File Use is set to Manual Selection, then the dialog box shown in the next figure is displayed instead of the one shown in Figure 4.27. Figure 4.28 In addition to the inputs of the initial and the final charge weights, the material selection file to be used in the charge correction calculation can be selected. The highlighted item corresponds to the default material selection file specified in the quality. If the alternate file has itself another alternate file, then this file will also be shown in the list. 4) Dilution The charge correction is done in two passes. The first pass brings up all the elements that are below the specified minimum value to meet the Low Aim/High Aim limits (internal limits). Depending on the composition of the materials added to correct these elements, this addition may represent a dilution for elements which are initially above the specified maximum value. The effect of this addition of materials is reported for elements which are still above specification after the first pass. Chapter 4 Quantitative Analysis WinXRF Operator Manual AA83501 4-24 Figure 4.29 The user has now the choice to apply the second pass by performing a dilution. It should be noticed that a dilution may require an unexpected amount of material for only a small correction. Hence, the required amount may be impossible to add due to a final furnace weight restriction. The following example illustrates such a situation. Initial furnace weight = 1000 kg Final furnace weight = 2000 kg We assume that 25 kg are added to correct all elements below specifications. The concentration values for P after additions are: Adjusted Limit P >0.0302 % 0.012 % The amount of material (containing no P) to dilute P can be determined with the following relationship: 1025 * 0.0302 = (1025 + x) * 0.012 x = ((1025 * 0.0302) / 0.012) - 1025 Addition = 1554.6 kg In this case, the dilution can not be done successfully as the weight allowance is exceeded by more than 50% ! 5) Charge Correction Report Once the charge correction has been completed successfully the charge correction report is displayed on the screen, as shown in the figure below. This report can also be printed on the local printer or transmitted to the same TELEX destinations as the analytical result. Quantitative Analysis Chapter 4 AA83501 WinXRF Operator Manual 4-25 Figure 4.30 Special Situations 6) Uncorrectable elements found Several situations can cause WinXRF to issue this error message: - Element is missing in all materials and therefore no correction is possible. - The analysed concentration of an element is too far below specification and the amount of materials to add to correct this element would exceed the weight allowance (Final - initial weight). - An addition of the available materials to bring up an element would cause too big a correction on other elements, especially when composite materials are added. - The addition of materials would cause to high a dilution on elements within specifications. Figure 4.31 7) Undefined element in Quality Chapter 4 Quantitative Analysis WinXRF Operator Manual AA83501 4-26 If all concentration values for an element in the quality description are left at zero (refer to the Configuration Manual), WinXRF will ask you to enter these values, or to reject the element. Figure 4.32 8) Input Quality Data If the element has not been rejected (see above) the quality specifications of the element can be entered here. The charge correction program makes use of these values to correct this element. Figure 4.33 9) Charge Correction failed If all elements cannot fully be corrected, then the following message is output by the charge correction program. Nevertheless, it is recommended to have the results displayed in order to more easily detect the cause of the problem. In most cases, the failure is due to an excess of additions, especially when dilution is applied. Figure 4.34 Quantitative Analysis Chapter 4 AA83501 WinXRF Operator Manual 4-27 Result Modification If the option Results Modifiable was enabled in the current task, the operator may modify the results by selecting the Modify function. The element or sample identity to be modified is selected by moving the highlight bar onto it. The validation of the modification is done by selecting a Modification Reason and by clicking on the OK button. Figure 4.35 After having confirmed the modifications, the screen shown in Figure 4.18 is again displayed, allowing the execution of additional functions and options. Result Options As explained in the Configuration Manual three different modes of execution can be chosen in the analytical task set-up for Storage, Transmit and Send to SPC modes: Manual Semi-Automatic Automatic Similarly, for the Print mode different options allowing manual and automatic printing are also available (see next section). Chapter 4 Quantitative Analysis WinXRF Operator Manual AA83501 4-28 Options in Manual Mode All options in manual mode may be executed first by merely clicking onto the corresponding, highlighted button. The sequence of execution depends on the logic of the operations and the options to be executed. All options can be executed more than once, except Store. That means a result may be printed before and after a modification of the result, also a Quality Check (Section Analyses with Quality Check) or Sort (Section Analyses with Quality Sort may be performed again after a modification of the result. The execution of manually selectable options is terminated by clicking onto the Continue button. Options in Semi-Automatic Mode The Storage, Transmit, Charge Correction and Send to SPC options may be specified in semi-automatic mode. Options in this mode are prompted for execution by the system after the Continue button has been clicked. Options in Automatic Mode The following options may be defined in Automatic Mode: Print (Average, All) Store Transmit (if installed) Send to SPC (if installed) Charge Correction (if installed) Options in this mode are executed without any operator interactions, except for Charge Correction. The Charge Correction program is a stand-alone program. The system only invokes this program and the control is then taken by the charge correction program which prompts for certain inputs. See Section Analyses with Charge Correction for more details. Print Mode During the set-up of the analytical task it is possible to select the option Full Headings. If selected, detailed information on how the analysis was performed in terms of what quality, type standard and analytical program was used, and full sample identity details are given. In addition to the heading information option, one of the following four printing mode options can be selected: None No printing is performed. Average Only the average of the result is printed automatically when the Continue button is clicked. All All runs, i.e. individual runs and the average result are printed automatically when the Continue button is clicked. Manual At the end of the analysis, the Print option will be enabled, allowing the operator to print the result. If the operator decides to print, and more than one run was made, the system will issue the question shown in the figure below. Figure 4.37 Quantitative Analysis Chapter 4 AA83501 WinXRF Operator Manual 4-29 Transmit Mode The results transmission is only available if at least one of the transmit options is installed. Depending on how the current analytical task was set up, one of the following four situations occurs: None No transmission can be performed, the Transmit button is dimmed. Auto All results are automatically transmitted to the remote destinations selected in the analytical task when the Continue button is pressed. The Transmit button is dimmed. Semi-automatic When the Continue button is pressed, a dialog box is displayed containing the check boxes corresponding to the available remote destinations. The destinations that have been selected in the current task are marked with a cross. If the Append Message option has been selected in the current task the default message is displayed in the corresponding entry box. Both, the proposed selection of destinations and the message can be changed before the OK button is clicked (figure below). Manual The Transmit button is available for selection. When it is pressed, a dialog box is displayed containing the check boxes corresponding to the available remote destinations. The destinations that have been selected in the current task are marked with a cross. If the Append Message option has been selected in the current task the default message is displayed in the corresponding entry box. Both, the proposed selection of destinations and the message can be changed before the OK button is clicked. Figure 4.38 Storage Mode Depending on how the current analytical task was set up for result storage, one of the following four situations occurs: None No result storage can be performed, the Store button is dimmed. Auto The result is automatically stored when the Continue button is pressed. The Store button is dimmed. Semi-automatic When the Continue button is pressed the system displays a dialog box that prompts the user to store the result or not (see figure below). Manual The Store button is available for selection. When it is pressed, the system stores the result. Chapter 4 Quantitative Analysis WinXRF Operator Manual AA83501 4-30 Figure 4.39 SPC Transfer The SPC software is an option available with WinXRF. It runs as a separate program within the Windows environment. Analytical results for product samples can be transferred from WinXRF to be available for study by the SPC Light software. Before results can be transferred, various details concerning how the study is to be performed need to be defined within the WinXRF software (see WinXRF Configuration Manual). Depending on how the current analytical task was set up for transmission of results to SPC, one of the following four situations occurs: None No transfer of the result to SPC can be performed, the Send to SPC button is dimmed. Auto The result is automatically transferred to SPC when the Continue button is pressed. The Send to SPC button is dimmed. Semi-automatic When the Continue button is pressed the system displays a dialog box that prompts the user to transfer the result or not (see figure below). Manual The Send to SPC button is available for selection. When it is pressed the system transfers the result to SPC. Figure 4.40 When a bad sample analysis is transmitted to the SPC-Light software it will be stored on that system but with an 'Ignore' status. This means that the fact that a measurement was taken will be recorded within SPC- Light but the result values will be ignored and not used in any of the calculations. Display Modes Many possibilities are available to display the results on the screen, these possibilities are set up in the analytical task used. Please refer to the WinXRF Configuration Manual for details about the available settings. Average Calculation with different Samples In special cases it is required to build the average with several sample preparations of the same material instead of a repeated measurement of the same sample. This method is very important if different factors Quantitative Analysis Chapter 4 AA83501 WinXRF Operator Manual 4-31 which are influencing the sample preparation can not be eliminated. Thus, through this method of calculating the average a certain compensation of these factors can be achieved. This way of calculating the average is invoked by a special indication of the cassette number, i.e. with a '+' symbol after the proper cassette number. The number of samples which shall be included in the average calculation is given by the Number of Runs. The symbol or the number before the '+' symbol dictates which cassette will be analysed first. This can be specified in the following three ways: ++ first cassette is the next one on the sample conveyor + first cassette is the one on the lift #+ first cassette is the one with the number # All further samples are analysed in the '+' mode, i.e. the remaining measurements are done with the n-1 following cassettes on the sample conveyor. Note: If pressed powder samples have to be used for drift correction or type standardisation updates, this method of building the average could be very useful to minimise factors which influence the intensity yield due to this sample preparation. If multiple preparation should form the average, then this way of building the average can only be specified in Manual Mode. This is done by selecting the corresponding task and changing the Cassette number and Number of Runs accordingly. Figure 4.41 Chapter 4 Quantitative Analysis WinXRF Operator Manual AA83501 4-32 Intensity Measurements The possibility to just measure intensities in unknown (or known) samples may for various reasons be of great importance. These reasons may be, for instance: Get a rough idea of the concentration levels of the different elements in the sample without having to calibrate the instrument. Stability tests. Microprocessor Background corrected net intensity measurements. The analytical tasks to measure intensities in unknown samples are run by selecting Production / Analysis - Analysis - Intensity Measurements. Figure 4.42 This induces the system to display a dialog box as shown below. The system brings up the task and the program that has been run the last time. If this function is used for the first time, or if the task that was run the last time does no longer exist, the screen will be greyed and the operator is asked to specify the task he wishes to run, by selecting the Change Task function (see Section Change Task). There may exist many different tasks that have been prepared for various applications. Depending on whether the chosen task was set up in manual sample mode (no sample list defined) or in pre-defined sample mode, a dialog box similar to the one in Figure 4.3 or in Figure 4.6 is displayed. Quantitative Analysis Chapter 4 AA83501 WinXRF Operator Manual 4-33 Please note that the sequence of operations for the execution of the selected options is exactly the same as for the concentration analysis. Options which can only be executed on concentration analysis are greyed or not presented for selection, like for instance Quality Sort or Charge Correction (if available). Figure 4.43 Note: In this mode the intensities are not passed through any of the possible correction stages (Drift Correction, Line Overlap Correction, etc.). Therefore, the intensity values correspond to the values as received from the microprocessors. DRIFT CORRECTION OF THE INSTRUMENT Drift Correction of the Instrument Chapter 5 AA83501 WinXRF Operator Manual 5-1 5 DRIFT CORRECTION OF THE INSTRUMENT Introduction The instrument is subject to long-term drift. The Drift Correction is an operation aimed at correcting for the drift and should be performed regularly. Up to three different drift correction schemes may exist on a same instrument depending on which semi- quantitative software options are installed. These are: Drift Correction for Quantitative Analyses Drift Correction for QuantAS Drift Correction for UniQuant Quantitative Analyses The drift correction for Quantitative Analyses is done by measuring Setting-up Samples (also called SUS). During the Drift Correction Initialisation the nominal or Day Zero intensities have been recorded and serve as the reference values. Each time the setting-up samples are measured during a Drift Correction Update (or Re-calibration) the actual intensities are compared with the nominal intensities. The resulting difference between the nominal and the actual intensities are used to drift correct the intensities of the analysed samples. Performing the Drift Correction Update (Re-calibration) The analysis for the Drift Correction Update is invoked by selecting Production / Analysis Analysis Standardisation / Drift Correction Update as shown in the figure below, or just by pressing the F3 function key. Chapter 5 Drift Correction of the Instrument WinXRF Operator Manual AA83501 5-2 Figure 5.1 Note: If a shortcut has been defined to perform the Drift Correction Update, then this operation can be started by clicking on the corresponding shortcut in the Shortcut folder (see next figure). If the shortcut is shown on the desktop, then a double click on the corresponding shortcut on the desktop will also start this operation. Drift Correction of the Instrument Chapter 5 AA83501 WinXRF Operator Manual 5-3 Figure 5.2 The dialog box shown in the next figure is then displayed. Chapter 5 Drift Correction of the Instrument WinXRF Operator Manual AA83501 5-4 Figure 5.3 The task in this category, which had been used previously, is automatically selected together with the analytical program(s). The name of the selected task and its description are given in the title bar. If, however, this task category is used for the first time, or if the task that has been used the last time does not exist anymore, WinXRF displays the following message in the title bar: Drift Correction - No Task selected The drift correction update task is then selected by clicking the Change Task button which causes the dialog box shown in the figure below to be displayed. Drift Correction of the Instrument Chapter 5 AA83501 WinXRF Operator Manual 5-5 Figure 5.4 After this selection, the identity of the first setting-up sample is then displayed on the screen. With the Select Program/Samples function the list of the samples to be run can be viewed and, if necessary, amended. Please note that only the programs of the working category are displayed in the corresponding list box. However, if a program from another category has to be selected, then this category has to be chosen first with the Select DB Category function. Chapter 5 Drift Correction of the Instrument WinXRF Operator Manual AA83501 5-6 Figure 5.5 If the Selective Drift Correction option has been selected in the present analytical task (see WinXRF Configuration Manual), the dialog box shown below will be displayed instead of the one shown above, allowing you to select the samples to be run on the basis of element channels. Please note that only the programs of the working category are displayed in the corresponding list box. However, if a program from another category has to be selected, then this category has to be chosen first with the Select DB Category function. Drift Correction of the Instrument Chapter 5 AA83501 WinXRF Operator Manual 5-7 Figure 5.6 If the Drift Warnings (Inform Operator) are not selected, no warnings will be issued in the event of an excessive drift and no update of the sample containing channels with excessive drifts will be performed. It is therefore recommended to select the Drift Warnings to enable the choice for updating or not. Note: In Unattended Analysis or Batch Mode (Chapter Unattended Operation) a warning is issued if elements show a drift bigger than SIGMA Factor * SIGMA. The channels are nevertheless updated. The analysis is started by clicking the Analyse button and the screen shown below is displayed. Chapter 5 Drift Correction of the Instrument WinXRF Operator Manual AA83501 5-8 Figure 5.7 The analysis can be interrupted by clicking onto the Abort button in which case the current sample will be ejected and the system returns to the former screen (Figure 5.3). Once the measurement of all element lines and runs is finished, new push buttons for the execution of analysis options will be presented at the bottom of the screen either automatically or by clicking onto the Analysis Complete button in case the Manual Run Selection option was selected. Figure 5.8 Depending on how the Print, Store and Transmit options were set up, the selected options will then be executed automatically when the Continue button is pressed or manually by clicking onto the corresponding buttons. However, if Paged Mode Deferred is set for printing, then printing will only be performed once there is enough to fill a complete page. Drift Correction of the Instrument Chapter 5 AA83501 WinXRF Operator Manual 5-9 The samples in the list will be analysed one after the other (manually) and the intensities stored according to the drift correction update scheme (see WinXRF Configuration Manual). If the corresponding options were selected in the current analytical task, a Drift Correction Report will be given after the measurement of each setting-up sample and at the end of the drift correction update an Alpha and Beta Report will be printed (see next section). The Batch Operation allows you to make this process automatic. Please refer to Chapter Unattended Operation. Drift Warnings and Reports Depending on the mode of analysis, the drift warnings and the drift update are handled slightly differently. In Unattended Analysis or Batch Mode, a warning is issued if elements show a drift bigger than SIGMA Factor * SIGMA. The channels are nevertheless updated. The Manual Analysis Mode offers the possibility to select the Drift Warnings option Inform Operator in which case a warning is given and the choice to update or not. If, however, the Drift Warnings option Inform Operator is not selected, the samples containing channels with excessive drifts are not updated. In all cases, it is possible to select different drift reports including additional drift warnings in the Analytical Tasks for Drift Correction Update. These reports can only be printed. Following options exist: Print Drift Report A report similar to the one shown next is printed. Drift Correction Report ----------------------- Channel Old New Day-Zero Drift Warning AlKa1,2 2.0000 1.4550 1.0250 CaKa1,2 210.0000 1.9205 200.5000 * FeKa1,2 3.0250 0.0037 3.0250 * MgKa1,2 0.2050 2.2901 0.2050 * SiKa1,2 19.5000 0.5000 19.5000 Print Alpha and Beta Report If the option Always was selected, a report similar to the one shown next is printed always for each analytical program for which the drift correction applies. If the option Out of Tolerance only is selected, then a report for the analytical programs is printed for which Alpha or Beta values are outside the specified tolerances. Please note that the Alpha value is not shown if a bottom standard only was used (AlKa1,2). Similarly, the Beta value is 0 if the drift correction is performed with a top standard only (FeKa1,2). Channel Alpha Beta Status ------------------------------------- AlKa1,2 -0.0126 OK CaKa1,2 1.0567 -0.0289 OK FeKa1,2 0.9474 0.0000 OK MgKa1,2 0.4964 2.2901 Alpha and Beta out of tolerance SiKa1,2 1.1034 0.0165 OK Chapter 5 Drift Correction of the Instrument WinXRF Operator Manual AA83501 5-10 QuantAS Four multi-element standards, delivered with the instrument, are used for the initial calibration of the instrument. They are stable in time and can be cleaned with alcohol. The same four standards are used to perform the re-calibration of the instrument either with the menu function or included as a step in a batch operation (see Chapter Unattended Operation) to correct for instrumental drift and compensate for any changes in the instrument hardware used for QuantAS. Performing the QuantAS Re--calibration The QuantAS option is already set up to perform the re-calibration of the instrument automatically. Prior to starting the re-calibration process the four samples, labelled QuantAS 1 to QuantAS 4, should be placed onto the specified positions or in the specified cassettes (older instruments), e.g. 1 to 4. The re-calibration procedure is started by selecting Production / Analysis Analysis QuantAS Standardisation / Drift Correction Update causing WinXRF to display the screen shown in Figure 5.10. Figure 5.9 In case the samples are to be placed onto different positions or in different cassettes, the numbers should be changed accordingly. The recalibration of the instrument is started by clicking onto the OK button. Drift Correction of the Instrument Chapter 5 AA83501 WinXRF Operator Manual 5-11 Figure 5.10 As during a normal analysis, the steps to be executed are copied into the ICS Operations Manager, which can be restored in the usual way (double-click on the corresponding icon) for examination. Figure 5.11 Note: All QuantAS Standards are automatically drift corrected during this process. This means that they can be used for future calculations. However, all analyses that were performed before a drift correction may no longer be valid, because the drift correction does not reflect the sensitivity state of the instrument at the time when the unknown samples were analysed. Chapter 5 Drift Correction of the Instrument WinXRF Operator Manual AA83501 5-12 UniQuant UniQuant uses 5 samples (also called Monitors) for drift correction. The following samples and element lines are measured: CAL.223 CAL.246 CAL.295 CAL.298 CAL.299 V Ka PdKa SiKa BaKa AlKa IrLa MgKa Y Ka NaKa PdLa CuKa F Ka BaLb The element lines have been selected in such a way that for each measuring group two lines exist close to either end of each group. The analytical conditions are the same as in the general measuring program, but the counting times have been chosen to be large enough to obtain a reasonable amount of counts for each monitored channel, typically 20-40 seconds. A special task, named RECAL-UQ, is provided to measure these monitor samples automatically. This task can be examined with the Prepare Task function (see Figure 5.13) by selecting Production / Analysis Analysis UniQuant. Figure 5.12 Drift Correction of the Instrument Chapter 5 AA83501 WinXRF Operator Manual 5-13 Figure 5.13 Measure the Monitor Samples The measurement of the monitor samples is done by selecting the Measure Intensities function in the UniQuant folder, as shown in Figure 5.12. This causes the dialog box shown in the next figure to be displayed. Figure 5.14 The task to be run can then be selected in the list box (normally RECAL-UQ) and the measurement started by confirming with OK. The intensities will be stored in the file called MONITOR.UQR. Import Measured Intensities The measured intensities have then to be imported into UniQuant. The importing works in the same way as for JOBs (see Chapter Semi-Quantitative Analysis) except that the intensity data are all written into one and the same file with the name MONDATA. While in the menu JOBS, the function I for Import of intensities has to be selected first. Chapter 5 Drift Correction of the Instrument WinXRF Operator Manual AA83501 5-14 Figure 5.15 The following dialog box is then displayed. Figure 5.16 The function I for Import has to be selected again, causing the following dialog box to be displayed from which the Monitor data has to be selected to be imported. Drift Correction of the Instrument Chapter 5 AA83501 WinXRF Operator Manual 5-15 Figure 5.17 Examination of the Drift After the new intensities have been imported, the details of the drift correction can be examined in the following way: While in the menu JOBS, the function I for Import of intensities has to be selected first. (see Figure 5.15). This causes a new menu to be displayed from which the function to check the drift correction data can be selected (M). Chapter 5 Drift Correction of the Instrument WinXRF Operator Manual AA83501 5-16 Figure 5.18 Please note that the system shows the drift range at the bottom of the screen. The details of the drift are given in the table shown below which looks similar for all UniQuant versions. Figure 5.19 CONTROL SAMPLE ANALYSIS Control Sample Analysis Chapter 6 AA83501 WinXRF Operator Manual 6-1 6 CONTROL SAMPLE ANALYSIS Introduction Control Samples can only be configured and analysed if the SPC Option (basic or full version) is installed. They are used to measure the instrumental performance on a regular basis. Before the WinXRF software can be used for Control Sample analyses, the following preparation work has to be performed, as described in the WinXRF Configuration Manual: Set-up of the required Control Samples. Allocation of the required Control Samples to Analytical Programs for unknown sample analysis and/or to the Global Control Samples List. Set-up of the required Analytical Program for Control Sample analysis. Set-up of the required Analytical Task for Control Sample analysis. SPC Initialisation. The Control Sample Analysis can be performed when required, or WinXRF requests the analysis after a certain time has elapsed, as explained below: When you try to analyse an unknown sample with an analytical program which includes Control Samples and the time allowed between analysis for the associated Control Samples has elapsed. When you try to analyse an unknown sample and the time allowed between analysis for the Control Samples in the Global Control Samples List has elapsed. At the end of the analysis of a control sample, the result of the analysis is transferred to the SPC software for storage and checking against the limits and trends that have been defined. When any violations occur, messages are then transferred back to WinXRF and displayed on the screen. Chapter 6 Control Sample Analysis WinXRF Operator Manual AA83501 6-2 Analysing Control Samples A Control Sample analysis can be started in three ways: 1) Through selection of Production / Analysis Analysis Control Sample Analysis. Figure 6.1 2) Through a click on a dedicated Shortcut in the Shortcut folder or on the desktop. Control Sample Analysis Chapter 6 AA83501 WinXRF Operator Manual 6-3 Figure 6.2 3) Automatically from within the Concentration Analysis function when the time for control sample analysis has elapsed. Figure 6.3 The screen similar to that shown below will then be displayed, which shows the previous analytical task that was used for analysis (1), or the task that was set up in the shortcut (2), or the default task for automatic measurement of the control sample (3). Chapter 6 Control Sample Analysis WinXRF Operator Manual AA83501 6-4 Figure 6.4 Pressing the Change Task button allows you to select another Control Sample task. The screen shown in the next figure is then displayed and the required task can be selected from the list and the selection confirmed by pressing the OK button. Figure 6.5 Pressing the Select button allows you to choose different Analytical Programs from which different Control Samples can be selected to be analysed using this task. By default, the task will run the Control Samples that were defined when the Analytical Task was created. The following window is displayed. Control Sample Analysis Chapter 6 AA83501 WinXRF Operator Manual 6-5 Figure 6.6 You can select another analytical program by clicking on its name. You can also select a group or many groups or even all programs, by using the s and c keys (Windows rules), as shown in the example below. When a new or an additional program is selected, the Update List button becomes available. Note: Only the Analytical Programs of the working category are displayed in the corresponding list box. However, if a program from another category has to be selected, then this category has to be chosen first with the Select DB Category function. Chapter 6 Control Sample Analysis WinXRF Operator Manual AA83501 6-6 Figure 6.7 Control Sample Analysis Chapter 6 AA83501 WinXRF Operator Manual 6-7 Press on the Update List button, and the control samples belonging to the selected programs are listed in the Available Samples list box, as shown in the figure below. Note that global control samples are always available, even if no program is selected. Figure 6.8 Chapter 6 Control Sample Analysis WinXRF Operator Manual AA83501 6-8 To select a control sample, you just double click on it. Repeat this operation for all control samples you want to analyse. The sample order is the order in which you selected them (see the example shown in the figure below). Figure 6.9 Note that you can also remove a selected sample in the same way (double click on it). When the OK button is pressed, WinXRF returns to the screen shown in Figure 6.4. Note: The Analytical Program that is used to analyse a Control Sample is not necessarily the same as the one that was used to set up the Control Sample, although, probably in most cases, they will be the same. The Sample Identifier will show the first Control Sample to be analysed. The Number of Runs is as specified in the analytical task and the Cassette Number as specified when the Control Sample was created. The analysis of this sample is started by pressing the Analyse button or you can move to the next sample selected by pressing the Skip button. Note: The Inform Operator check box has no effect and will disappear in a future software release. The Control Sample is analysed in the same way as an Unknown Sample. Control Sample Analysis Chapter 6 AA83501 WinXRF Operator Manual 6-9 Figure 6.10 At the end of the analysis, the Control Status of the sample is updated to OK, Out-of-Control or SPC Error and the Time-To-Next Analysis is reset only if the Control Status is OK. Note: The Recalculate button allows you to reprocess the analysis of selected control samples without having to measure them again. This is especially useful if a Control Sample analysis has been performed and an Out-of-Control situation has been reported, requiring a drift correction to be performed. After the drift correction has been performed, the involved Control Samples could just be recalculated to check whether the process is again in control. Please refer to Figure 6.4 and Chapter Analysis Recalculation Option for more details about this function. Chapter 6 Control Sample Analysis WinXRF Operator Manual AA83501 6-10 Transfer to SPC At the end of the Analysis, when the Continue button is pressed, the results are transferred to the SPC-Light package. The way the results are transferred depends on how the SPC Transfer Mode was set up. If the transfer mode is Auto, the result will be transferred directly to the SPC package without further operator involvement. If the transfer mode is Semi-Auto, a dialog box is displayed allowing the operator to choose whether to send the result to the SPC-Light Software. If the operator presses the Yes button, the result will be transferred to the SPC-Light package. If the transfer mode is Manual, the Send to SPC button will be available on the final result screen which has to be pressed to transfer the result to SPC. Bad Sample Transmission Control Samples can be given a Bad Sample status. This can occur after an analysis because a certain test on the result has failed, like the sum calculated by a Pseudo element is too far away from the specified range. When a bad sample analysis is transmitted to the SPC-Light software, it will be stored on that system but with an 'Ignore' status. This means that the fact that a measurement was taken will be recorded within SPC- Light, but the result values will be ignored and not used in any of the calculations. SPC Messages This section lists the messages that can appear during analysis of Control Samples with an explanation of the meaning and the action to take when appropriate. Failed to run SPC This message will appear if the SPC-Light software is in a wrong directory or is not installed. Failed to communicate with SPC This message will appear if an error occurs when a result is sent to SPC-Light. You should ensure that all the settings are as described in the Readme file SPC.WRI and that the dongle is properly installed. Do you want to create a study file for the current sample This message will be output when the first analysis for a Control to SPC-Light is sent and there is no study file with this sample name available. You should press the OK button to create the study file automatically. No SPC Statistics available for sample This message appears when there are insufficient measurements, less than twenty, carried out for the sample and control limits cannot be calculated for the elements in the sample. Sample and study file elements dont match The elements in the result being sent to SPC-Light do not match those defined in the study file. The result will not be stored in SPC-Light. You will need to change the elements defined for the Control Sample or in the Storage section of Print Orders to match those stored in the study file. This error can also appear if an element name is changed in the program. Control Sample Analysis Chapter 6 AA83501 WinXRF Operator Manual 6-11 SPC Automatic Batch Management not selected, defaulting to batch name ARL This message appears when the automatic batch management by SPC is selected in WinXRF, but is not defined in SPC. SPC Alarms Warnings and out of control alarms for SPC test failures are reported in a scrolling window as shown below. Figure 6.11 Fatal alarms are reported in red. Warnings are reported in blue or black; they are blue if no limits have been established for an element. SPC This button remains greyed with SPC Basic and is available with SPC Full. The SPC button restores the SPC window. First a message Display failed chart lets the user choose to display or not the failed chart(s) within SPC. This message will not appear when the concerned analytical task has the option Auto Display SPC Charts selected. The following control samples need to be measured ........ Analyse control samples now? This message can appear when an analytical program is used which has had control samples defined for it or when a Global Control Samples list is configured. If one or more of these control samples have expired or were outside the limits when previously measured, then this message appears. If you press the Yes button, you can analyse these samples using the Default analytical task. If you press the No button, you can continue to use the analytical program in the normal manner. The following SPC flags are set when the results are not within control limits: [ Result above SPC control limit ] Result below SPC control limit # Failed SPC Test UNATTENDED OPERATION Unattended Operation Chapter 7 AA83501 WinXRF Operator Manual 7-1 7 UNATTENDED OPERATION Introduction In general, an Unattended or Batch Operation is an execution of a list of instructions in a pre-defined sequence, referred also to as automatic operation. In WinXRF, this list of instructions consists of a list of operations, like Scans or Energy Profiles, and Tasks to perform various analytical measurements, like recalibration or analyses of a series of unknown samples etc. The WinXRF Software offers two ways of unattended operations: Unattended Analysis Batch Operation The Unattended Analysis mode allows execution of analytical tasks without operator interactions, or if a task was not set up for a fully unattended operation, with a minimum number of operator interactions. This is especially useful if a sequence of pre-defined samples needs to be run rapidly. As explained in the WinXRF Configuration Manual, the unattended analysis can be combined easily with the Batch Operation. The Unattended Analysis mode is restricted to the execution of Analytical Tasks (i.e. Analysis) whereas the Batch Operation works with the following instrument operations: Analysis Scan Energy Profile Batch Delay Set Environment UniQuant QuantAS QuantAS Recalibration Goniometer Position Calibration Goniometer High Voltage Calibration Monochromator High Voltage Calibration Terminal Script Mode In Batch Operation, the list of operations and tasks is stored in a named file. This mode of analysis is therefore very powerful for sequences that need to be executed periodically, like running the Setting-up Samples to recalibrate the instrument. It is quite obvious that the tasks and other operations, like Scans or Energy Profiles (Parameter Files) have to be prepared before they can be included in the step list of operations. The next sections explain the two modes of unattended operations in more details. Note: There exists a third automatic or unattended operation mode called Automatic Mode. This mode allows you to control the X-ray instrument from a remote computer in conjunction with an Automation System. This automatic mode is an option and is treated in Chapter Automation Mode. Chapter 7 Unattended Operation WinXRF Operator Manual AA83501 7-2 Unattended Analysis This mode of analysis is invoked by selecting Production / Analysis Analysis Unattended Analysis, or by pressing the key F5. Figure 7.1 The next screen is then displayed, allowing the operator to select the category of tasks from which the task to be executed can then be chosen from. Unattended Operation Chapter 7 AA83501 WinXRF Operator Manual 7-3 Figure 7.2 Three cases exist depending on how the chosen task has been set up: 1. The task was set up with a pre-defined sample list In this case, the displayed screen looks like in the Figure 7.2, i.e. only the Category and the Analytical Task, the OK and the Cancel buttons are enabled for selection and the rest of the screen is greyed. After the OK button is pressed, the list of samples (or the single sample) is entered in the ICS Operations Manager list. The execution of the first step in the list is then started unless an elapsed time period is detected among the Setting-up Samples (or Type Standard or Control Samples) used for drift correction of the selected analytical program (see figure below). Figure 7.3 2. The task was set up without an Analytical Program In this case, the displayed screen looks like in the figure below, i.e. in addition to the Category and the Analytical Task only the Analytical Program can be selected either by using the Select button and the screen shown in Figure 7.5 is displayed, or by writing the name directly into the entry box. Chapter 7 Unattended Operation WinXRF Operator Manual AA83501 7-4 Figure 7.4 When such a task is chosen, the operator must select the Analytical Program he wishes to run with this task first before the sample identity and the Manual Inputs (if present) can be specified and the analysis started. Only the program categories (i.e. Qualities, Type Standards, Analytical Programs) that have been enabled in the current task are offered for selection. Figure 7.5 Note: Only the programs of the working category are displayed in the corresponding list boxes. However, if a program from another category has to be selected, then this category has to be chosen first from within the Database Category combo box. Please note that the option Bad Sample will be enabled for selection after the Analytical Program has been chosen. Unattended Operation Chapter 7 AA83501 WinXRF Operator Manual 7-5 After the OK button is pressed, the single sample is entered in the ICS Operations Manager list. The execution of this step is then started unless an elapsed time period is detected among the Setting-up Samples (or Type Standard or Control Samples) used for drift correction of the selected analytical program (see Figure 7.3). 3. The task was set up with an Analytical Program only. In this case, the displayed screen looks like in the figure below, i.e. all dialog box options and inputs are enabled and the specified Default Program is proposed in the corresponding entry box. The operator has however the possibility to select another Analytical Program, if required, by using the Select button and the screen shown in Figure 7.5 is displayed. Only the program categories that have been enabled in the current task are offered for selection. Note: Only the programs of the working category are displayed in the corresponding list boxes. However, if a program from another category has to be selected, then this category has to be chosen first from within the Database Category combo box. Figure 7.6 Before the analysis can be started, at least one sample identity has to be specified and Manual Inputs (if present) given. Please note that the option Bad Sample is also enabled for selection in this case. After the OK button is pressed, the single sample is entered in the ICS Operations Manager list. The execution of this step is then started unless an elapsed time period is detected among the Setting-up Samples (or Type Standard or Control Samples) used for drift correction of the selected analytical program (see Figure 7.3). Chapter 7 Unattended Operation WinXRF Operator Manual AA83501 7-6 ICS Operations Manager The ICS Operations Manager handles the execution of the required operations. Each time an Unattended Analysis, a Step Scan, an Energy Profile etc. is launched, a step is added to the list of operations. Normally, the ICS Operations Manager works in the background, but the icon can be restored, by double-clicking on the icon, for examination and step list manipulations. Various options and functions are offered by the ICS Operations Manager, as shown in the figure below. Figure 7.7 While the manager is busy working through the list of operations, the operator has the possibility to queue up additional operations, like Scans, Energy Profiles, Analyses, Batches etc. with the Insert Steps option. Note: The list of operations in Unattended Analysis Mode together with steps added later are only stored temporarily. Once the sequence is finished, the list will be lost unless it is stored in a named Batch with the Copy Active Steps function (refer to the Configuration Manual). Step List Manipulation In order to manipulate the list of operations, the execution of operations has to be interrupted first either with the Abort option for an immediate interruption, or with the Halt option, in case the current operation has to be finished first. As soon as the operation is stopped, the Step List Manipulation options will be enabled. These options are described in the WinXRF Configuration Manual. Unattended Operation Chapter 7 AA83501 WinXRF Operator Manual 7-7 Batch Operation In principal, this mode of unattended operation looks very similar to the Unattended Analysis mode. The difference, however, consists in the fact that all steps of operations are stored in so called Batches. Before a Batch Operation can be launched, the implied Batches need to be prepared, as explained in the Configuration Manual. Running Batches A Batch Operation is invoked by selecting Production / Analysis Batch Operation. Figure 7.8 and the screen shown below is displayed. After the selected Batch has been started, by clicking the OK button, the list of operations is copied into the ICS Operations Manager. Chapter 7 Unattended Operation WinXRF Operator Manual AA83501 7-8 Figure 7.9 As explained in Section ICS Operations Manager, the ICS Operations Manager can be displayed by double- clicking the corresponding icon. Then, the current operation can also be halted or aborted and the step list manipulated, if required (Figure 7.7). The Halt and Abort functions are used to interrupt the currently running operations in case a more urgent analysis needs to be done: Halt The execution of the step list is interrupted at the end of the current step. Abort The execution is interrupted immediately by resetting the instrument. RESULTS RETRIEVAL & STATISTICS Results Retrieval & Statistics Chapter 8 AA83501 WinXRF Operator Manual 8-1 8 RESULTS RETRIEVAL & STATISTICS Introduction All results that have been stored through various store actions offered in the different analytical tasks are stored in the active results database. The number of results is only limited by the disk space. Each result holds the Measured Raw Intensities and Concentrations for up to 100 elements. The retrieval function allows retrieving thousands of results using various selection criteria, like Task name, Sample Identity or a Time Period. However, the number of retrieved results that can be retrieved at any one time is limited by the value entered under Retrieval Limit in the Results Database Generator dialog box (see WinXRF Configuration Manual). The following actions, described in the next sections, may then be performed on retrieved results: Modification of the result values and identifier Statistics Deletion Transmission (if option installed) Export into ASCII or special format files Export to Report Generator (if option installed) Print Quality Check Quality Sort Charge Correction (if option installed) Send to SPC (if option installed) Chapter 8 Results Retrieval & Statistics WinXRF Operator Manual AA83501 8-2 Retrieval & Statistics There are three ways to start the results retrieval process: Using a pre-defined shortcut (if one has been defined) Using the Results Database icon Pressing the F8 function key All these ways are essentially the same, but the shortcut allows the pre-selection of some of the sorting parameters, in order to control or ease the operator's choices. Selection Criteria for Results Retrieval The retrieval function is started by clicking on the Results Database icon which is part of the Results Processing folder of the Production / Analysis menu or by pressing the function key F8. Figure 8.1 Note: Alternately you may start the results retrieval process by clicking on a pre-defined shortcut, if such a shortcut has been defined. The screen shown below is then displayed, allowing the operator to specify the various selection criteria. Please note that if the results retrieval function has been initiated through a shortcut, then some sample selection criteria may already be filled in. Results Retrieval & Statistics Chapter 8 AA83501 WinXRF Operator Manual 8-3 Figure 8.2 In order to understand the many possibilities offered by the selection criteria, it is recommended to follow the procedures described in the next section. Once acquainted with the possibilities, some of the steps may be omitted or executed in a different way. Procedure for Results Retrieval We recommend the following step-by-step procedure: 1. Select database 2. Select task 3. Select analytical program 4. Select sample identity 5. Select time period 6. Select result type 7. Terminate selections These steps are explained chronologically in the next sub-sections. Database Selection If you want to make the retrieval operation on the currently active results database, you can skip this section. Otherwise you can change the currently active results database by pressing on the Results DB button (Figure 8.2). The following dialog box is displayed. Chapter 8 Results Retrieval & Statistics WinXRF Operator Manual AA83501 8-4 Figure 8.3 Select the path from the list box. When the displayed path is correct press the OK button. You are returned to the Define Sample Selection window (Figure 8.2). Task Selection The Change Task button is used to select the category of tasks that were used to obtain the results. Furthermore, a particular task of the selected category can then be selected. Figure 8.4 After the category has been selected, the tasks available are then displayed in the right-hand list box and any one of these may be selected. All results obtained with the selected task name may be retrieved. If no task name from the selected category is entered, then all results obtained with this category of tasks will be available for further selection. If the [All] category is selected then all results will be available for further selection. The Save as Defaults function is used to store the selected task category and name as the default set-up. This default will then be used for all future retrievals and it will not be necessary to use the Change Task function to choose this category and name of task each time. However, the Change Task function is still used to select other tasks or to change the default set-up. Results Retrieval & Statistics Chapter 8 AA83501 WinXRF Operator Manual 8-5 The OK button validates the selection and causes WinXRF to return to the screen shown in Figure 8.2, and the task category and name is displayed in the window title bar. Analytical Program Selection With the Select button (see Figure 8.2), the Quality, Type Standard or Program that was run with the task(s) specified in Section Task Selection can be selected. Figure 8.5 Please note that only the programs of the working category are displayed in the corresponding list boxes. However, if a program from another category has to be selected, then this category has to be chosen first with the DB Category button, as shown in the next figure. Chapter 8 Results Retrieval & Statistics WinXRF Operator Manual AA83501 8-6 Figure 8.6 The OK button validates the selection and WinXRF returns to the screen shown in Figure 8.2, but this time, the selections made are indicated on the title bar (task) and in the Analytical Program box as shown below. Figure 8.7 Results Retrieval & Statistics Chapter 8 AA83501 WinXRF Operator Manual 8-7 Sample Identity Filter Every sample identity field defined in the system is displayed with a pair of Low and High text boxes as shown in Figure 8.7. These pairs of text boxes may be used in two different ways: If the sample selection for a certain identity field is made on a name, this name may be entered in either box. The Wild Card characters "*" and "?" may be used to select a group of samples with similar identifications. If the sample selection for a certain identity field is made by specifying a range, then the range is defined by the limits entered in the Low and High text boxes of that identity field. The system checks the range in an alpha-numeric order by comparing the ASCII values of the characters in that field with the ASCII values of the limits. Note: The ASCII values of numbers are smaller than the ASCII values of letters. The ASCII values of small letters are greater than the ASCII values of capital letters. Wild Card characters only should not be used in the specification of the range limits. The following examples illustrate various possibilities of sample identity selection: 1) Low BAS401 All samples with this name in the corresponding field. High (empty) 2) Low (empty) Same as 1. High BAS401 3) Low (empty) All samples with a name starting with BAS40 High BAS40? in the corresponding field. 4) Low B* All samples with a name starting with B High (empty) in the corresponding field. 5) Low 100 Numeric Field: All samples with a number High 125 between 100 and 125 in the corresponding field. 6) Low 100 Alpha-numeric Field: All samples starting High 1250 with a number between 100 and 1250 , e.g.: 100, 102A, 119, 12CD, ..... 7) Low A All samples with a name starting with a capital letter High Z in the corresponding field. 8) Low 0 All samples with a name starting with a High z number or a letter in the corresponding field. Time Period Filter A Period may be specified by entering the Time or the Date of the beginning and the end time in the From and To text boxes of the Date and Time box. A Daily Period is specified by selecting the corresponding check box and by entering the date of the first day together with the time of the beginning of the daily period, and the date of the last day together with the time of the end of the daily period. If the Daily Period check box is not selected, then all results between the date and time limits will be retrieved. Chapter 8 Results Retrieval & Statistics WinXRF Operator Manual AA83501 8-8 The Time has to be specified as set for the Windows short format (Regional Settings item in the Control Panel). The values for hours, minutes and seconds are floating values, i.e. they can be entered as real values. The seconds need not be specified. For example: 14:30:25 = 14 hours 30 minutes 25 seconds 14.5:25 = 14 hours 30 minutes 25 seconds 00:30.5 = 30 minutes 30 seconds The date and time complies with year 2000 and follows the selected Windows format. Therefore, the Date has to be specified as set for the Windows short format (Regional Settings item in the Control Panel). Beside the "/" symbol the "\ . -" symbols may be used as separators, but both separators must be the same. If the month is entered using alphabetical characters, the Spacebar or no separator may be used. If the year is omitted, it defaults to the current year. For example: 20/12/01 = 20 December 2001 20-12-2001 = 20 December 2001 20.12.2001 = 20 December 2001 20\DEC\01 = 20 December 2001 20dec = 20 December (current year) 20 DECEMBER 2001 = 20 December 2001 20J01 Not valid, J could be JULY, JUNE or JANUARY The time and date in a Daily Period is separated by a space: 20dec01 14:30 or 14:30 20/12/01 Examples: 1) From 1-JUL-00 All samples with a date equal or higher than the low limit. To (empty) 2) From 12:00 All samples between the two limits. To 20:00 (No date restriction). Daily Period checkbox has no effect. 3) From 1-Jul All samples of the month of July of the current year. To 31-Jul Daily Period checkbox has no effect. 4) From 1-Jan-00 12:00 Only samples between 12:00 and 20:00 of every day To 31-dec-00 20:00 in 2000. (Recurring range). Daily Period 5) From 1-Jan-00 12:00 All samples from January 1 st , 2000, from 12:00 To 31-dec-00 20:00 to December 31 st , 2000, to 20:00 (Absolute range). Daily Period Result Type Filter The type of results to be retrieved may be specified by selecting one of the four following Result Type options, as shown in Figure 8.7: All All results will be retrieved (individual runs and averages). Results Retrieval & Statistics Chapter 8 AA83501 WinXRF Operator Manual 8-9 Individual runs Only results of individual runs will be retrieved. Average Only average results will be retrieved. Metaverage Only metaverage results will be retrieved. Terminating Selections Pressing the OK button terminates the input of the selection criteria and WinXRF then displays all results that match the specified selection. All results that are matching the selection criteria are then displayed, and depending on the number of results to be checked, the progress of result retrieving is shown in an intermediate window. Actions to be carried out on Retrieved Results After the OK button has been pressed (Figure 8.7), the matching retrieved results are displayed on a HTLM page as is shown in the example below. The path of the selected results database is indicated in the windows title bar. The report page is divided into four parts: The first part displays general information concerning the selected sample (when more than one sample is selected, it displays the data concerning the first one of the selection). The second part is a list box showing the sample identifiers and date and time of analysis. The third part displays the result values of the selected sample (when more than one sample is selected, it displays the data concerning the first one of the selection). The fourth part contains action buttons. Depending on the activated options and the configuration, some of the buttons may be greyed or even not displayed. The action buttons are described in the following section. Chapter 8 Results Retrieval & Statistics WinXRF Operator Manual AA83501 8-10 Figure 8.8 Before using the action buttons, a sample or a group of samples (i.e. results) must be selected as follows. Single Sample Selection A click on the sample (result) line selects (highlights) the sample. Clicking on another sample selects the new one and deselects the previous one. Multiple Sample Selection You can select a group of samples with the left mouse button and with the s or c key pressed according to the Windows rules: Keeping the s key pressed allows selection of a consecutive group of samples (all samples between the first and the second selection click are highlighted). Keeping the c pressed allows selection of an additional individual sample (at each click a sample is added and highlighted). Note: When more than one sample is selected, the details of the first sample in the list of selected samples are displayed. Results Retrieval & Statistics Chapter 8 AA83501 WinXRF Operator Manual 8-11 Action Buttons Once an individual sample or a group of samples is selected, various actions can be carried out on the selected samples. Some of the actions depend on the activated and available options. Set Selection The selection criteria for results retrieval may be re-defined. Modify Sample The sample identifier and the result values of the selected sample may be changed. If more than one sample is selected, only the first one will be available for modification. This function is subject to permission, see Section Modification of Results. Print The selected samples (results) are printed. Delete This will delete the selected sample(s) from the retrieved list. This function may be restricted by the Result Modification Scheme. Export The selected samples (results) are exported in the selected format (ASCII, dBase, Lotus) and stored in a named file or can be displayed on screen. This is also used to transfer results to the Report Writer when the report option is available (see Section Export Results). Transmit The selected samples are transmitted to remote destinations. This function is subject to the availability of a transmission option (see Section Transmission of Results). Statistics The Average, Standard Deviation (Absolute and Relative), Minimum and Maximum values are computed with the results of the selected samples (minimum two). See Section Statistics. Quality Check The selected result may be checked against a set of upper and lower limits stored in a Quality. This function is only available if the selected result was obtained through a quality. Quality Sort The values of the selected sample are used to determine the quality of the sample, using a Quality Sort List which holds a set of suitable Qualities. If more than one sample is selected, only the first one will be used for sorting (see Section Quality Sort). This function is only available if the selected result was obtained through a quality. Charge Correction The values of the selected sample are used to calculate the charge correction, using Materials and Selection. If more than one sample is selected, only the first one will be used for charge computation. This function is only available if the selected result was obtained through a quality and the Charge Correction option is installed. See Section Charge Correction. Send to SPC Transfers the results of the selected sample(s) to the SPC software. Only available if the SPC option is installed (see Section Send to SPC). Exit The results retrieval function is left. Modification of Results The Modify Sample function allows the modification of the result values (Intensities and Concentrations), the Compound name and the Sample Identity. This function is only available if it has been enabled under System Options (see WinXRF Configuration Manual). Chapter 8 Results Retrieval & Statistics WinXRF Operator Manual AA83501 8-12 After the sample has been selected, pressing the Modify Sample button causes the screen shown below to be displayed. Figure 8.9 On leaving the screen by clicking on the OK button, all modifications will be stored. Note: You cannot exit without giving a modification reason to be selected from the Modification Reason combo box. Export Results The Export function allows the conversion of a selected list of results, defined as a group, in various formats. The converted results will be stored in a named file or sent to the selected output. After a group of samples has been selected, pressing the Export button causes the dialog box shown in the next figure to be displayed. Results Retrieval & Statistics Chapter 8 AA83501 WinXRF Operator Manual 8-13 Figure 8.11 The Export Format group box allows selecting the results file format. The following options are available: dBase IV The results are exported in dBase IV format. Lotus The results are exported in Lotus format. Analysis Reports - No. of Channels The results are exported for use with the Analysis Report option. The maximum of channels (32, 64 or 100) needs to be selected with the corresponding radio button. Include flags When selected, the results are exported with their quality flags (<, > etc.). Append to existing file When selected, the results are appended to the existing file. Otherwise the file is overwritten. Export Print Order This is used to choose print order of the elements when exporting the results. The print orders are as defined in the analytical program at analysis time. File name This is used to define the destination directory and file for the results export. The details specified here can be stored with the Save as Default Path option in case the same destination is used again later. As an alternative, the user can select the directory of the destination file in the Directories list box and then the file name in the Files list box. In this case, the selected file will be overwritten. Additional formats are available within the Special Options function and are explained after the next figure. Note: Most of the functions are tools only. No warranty can be given on the export formats. These may change with the mode level of any software version. Chapter 8 Results Retrieval & Statistics WinXRF Operator Manual AA83501 8-14 Figure 8.12 Readable This produces a printable text file (*.RD). The content is in ASCII format with field identification names. Import(.src) This produces a text file (*.SRC) suitable for re-importation via the import database function. The content is in ASCII format without field identification names. Binary only This produces a file (*.BIN) where the exported data is simply packed binary. Binary + Import Info This produces a file (*.BIN) where the exported data is simply packed binary. Binary + Full Info This produces a restricted form of information file which is only worthwhile for re- importing data exported in this format. UniQuant 1 UniQuant measurement results (version 1 only) have to be exported in this format. Transform This produces a file using a transformation file (*.TRF) which generates output lines as it wishes. The transformation files available are displayed in the list box. Among the files listed, only ASCII, RTXT_FLG and RTXT_NFG may be of interest. Other files may be present if special export formatting is required by software options or software specials. Note: The suffix FLG stands for 'with flags' meaning that the result flags <, >, (, ), ! etc. should be considered as well. The suffix NFG stands for 'no flags' meaning that the result flags should be ignored. Lotus 123 (WK1) This provides a method of exporting any data in Lotus format in a file (*.WK1). Results Retrieval & Statistics Chapter 8 AA83501 WinXRF Operator Manual 8-15 Lotus 123 (WK1) Transform This produces a Lotus format file (*.WK1) using a transformation file. Two transformation files (R123_FLG and R123_NLG) are available for this purpose. FLG extension means that the results will be transformed with their flags and NLG extension means without flags. The exported data can be combined with an existing file. dBASE IV (.DBF) Transform This produces a dBASE format file (*.DBF) using a transformation file. Two transformation files (RDB4_FLG and RDB4_NFG) are available for this purpose. FLG extension means that the results will be transformed with their flags and NFG extension means without flags. The exported data can be combined with an existing file. This file format is also used for the export of results to the Report Generator option. Five transformation files are available for this. These are RR100.NFG, RR64.FLG, RR64.NFG, RR32.FLG, RR32.NFG. The user is asked to refer to the WinXRF Configuration Manual for additional information. The output destination can be selected through the following options: User Directory The results in the selected format are stored in the database directory in a file for which the name is specified in the Output file name box. Other Directory This option is used to select the directory from the list box. This selection is done in the standard Windows manner, i.e. double-click on a drive and/or directory to expand, or on [..] to go back one level. The selected directory is displayed next to the header Directory. The results in the selected format are stored in a file for which the name is specified in the Output file name box. Device The results in the selected format are sent to the selected output device. This should be a 'receive only' device. Warning: Do not select ICS Show on Screen Results that are exported in the Readable, Import (*.SRC) or Transform format can be displayed on the screen. Transmission of Results The Transmit function allows the transmission of a selected list of results, defined as a group, to the various destinations configured. After a group of samples has been selected, pressing the Transmit button causes the dialog box, shown in the figure below, to be displayed. Chapter 8 Results Retrieval & Statistics WinXRF Operator Manual AA83501 8-16 Figure 8.13 The configured destinations are displayed and the destinations for the transmission can be selected by checking the corresponding check boxes. The Full Sample Headings check box allows addition of sample heading information for the transmission to telex destinations. Also, for the transmission to telex destinations, a message can be added to the transmission. Its text has to be entered in the Append Message text box. The transmission to the selected destinations is performed by clicking the OK button. Statistics The Statistics function allows the computation of the average, standard deviation, relative standard deviation, minimum and maximum of a group of selected results. At least two results (samples) have to be selected to use the Statistics function. The samples to be included in the statistical calculations can be chosen in the normal way (see beginning of Section Actions to be carried out on Retrieved Results). After a group of samples has been selected, pressing the Statistics button causes the dialog box, shown in the figure below, to be displayed. All samples of the selected group are listed in the list box and may be examined. The Statistics works only if: the elements match for all results there are no bad sample results Results Retrieval & Statistics Chapter 8 AA83501 WinXRF Operator Manual 8-17 Figure 8.14 At this time, the only enabled buttons are Set Details and Exit. The Weight edit box is used to give more or less importance for a sample. When the statistics are calculated, each element concentration (or intensity) will be multiplied by the Weight associated to the corresponding result. The average for an element will then be the sum of all weighted concentrations (intensities) for this element divided by the Total Weight (see Figure 8.16), as usual for a weighted average calculation. This can be useful for calculating a pseudo charge from various charge scraps. Sigma (Sd), relative sigma (Sd%), Min and Max values will not be affected by this Weight. Before the statistical calculation can be performed, the Statistics Details have to be specified by using the Set Details button, which causes the dialog box shown below to be displayed. Chapter 8 Results Retrieval & Statistics WinXRF Operator Manual AA83501 8-18 Figure 8.15 The following items can be defined: Sample Name If the average result has to be stored, a new sample identification may be entered for the statistical results. Field Widths The length of the result headers (Compound names) can be defined here. Print Orders The print orders for the local and the remote results can be defined here. Compound The result name can be changed in this entry box. Local Accuracy The number of decimal places for the local statistical result can be specified in this entry box. Remote Accuracy The number of decimal places for the remote statistical result can be specified in this entry box. Average Type Selects if the statistical calculations are to be made on intensity or concentration values. Four check boxes allow the user to select what must be calculated and displayed in addition to the mean value. This selection can be stored with the Set as default button for a later use. These check boxes are the following: Sigma The absolute standard deviations will be calculated and displayed. Relative Sigma The relative standard deviations will be calculated and displayed. Results Retrieval & Statistics Chapter 8 AA83501 WinXRF Operator Manual 8-19 Minimum The minimum values found will be displayed. Maximum The maximum values found will be displayed. After the Statistics Details have been defined and confirmed by clicking on the OK button, WinXRF returns to the previous dialog box (see below). But this time, the Get Statistics option has now become enabled. Clicking on this button causes WinXRF to calculate the desired statistical values, which will then be displayed. Figure 8.16 The statistical results are displayed at the end of the list box shown in Figure 8.16 after the analytical results of the group of selected samples. After the statistical calculations have been performed the following buttons are available: Print Average The statistical results are printed. Transmit Average The statistical results are transmitted to the selected remote destinations. Store Average The statistical results are stored in the result file. Print All All analytical and statistical results are printed. Transmit All All analytical and statistical results are transmitted to the selected remote destinations. Exit Causes the WinXRF to return to the dialog box shown in Figure 8.8. Chapter 8 Results Retrieval & Statistics WinXRF Operator Manual AA83501 8-20 Quality Check The Quality Check function allows the selected retrieved result to be checked against a set of upper and lower limits defined in a Quality. Depending on how the sample has been analysed, the following two cases exist: If the sample has been analysed with a quality, then pressing the Quality Check button displays the dialog box shown in Figure 8.17 showing the result of the quality check. If the sample has not been analysed with quality, then pressing the Quality Check button displays first a dialog box requiring a quality to be selected (see Figure 8.18) and then the dialog box showing the result of the quality check (see Figure 8.17). Figure 8.17 Another quality can then be selected by pressing the Select Quality button. This causes a new dialog box to be displayed and the user is asked to select the required quality from the list box. Results Retrieval & Statistics Chapter 8 AA83501 WinXRF Operator Manual 8-21 Figure 8.18 On confirmation of the choice, the new quality check result is then displayed and yet another check can be performed or the result be printed. When leaving the quality check function by clicking on the OK button, the user is prompted with the options shown in the figure below, before returning to the screen shown in Figure 8.8. These are: Discard Quality Checked Result Replace Original Stored Result Store New Result and Retain Original The last two features might be of interest if a Charge Correction has to be done with a different quality than the one the sample was originally analysed with. Because, prior to performing a new charge correction, the result has to be checked with the desired quality and the result stored with one of the two store options. Figure 8.19 After selecting one of the three options, WinXRF returns to the dialog box shown in Figure 8.8. Quality Sort The Quality Sort facility permits a retrieved result to be checked against a set of qualities in order to find the quality that best matches with the selected sample. The tightness of the matches is indicated by a Chapter 8 Results Retrieval & Statistics WinXRF Operator Manual AA83501 8-22 variance value, of which the mathematics is given in the WinXRF Configuration Manual. However, this option is only enabled if the highlighted sample has been analysed through a quality. When the Quality Sort button is pressed, the dialog box shown below is displayed. Figure 8.20 In the list box on top, all Quality Sort files matching with the matrix identifier of the selected sample are proposed for selection. The desired group of qualities can be selected from that list and as soon as the Select button is pressed, the sort result is given in two separate lists, on the left for qualities matching with the retrieved result and on the right where not all elements are within specification. The quality sort result can be printed with the Print Sort option and with the Quality Check function, a quality check of the retrieved result is directly performed from this dialog box (see Section Quality Check). Pressing Exit brings back the dialog box shown in Figure 8.8. The Quality Sort procedure is also described in Chapter Quantitative Analysis. Charge Correction It is also possible to perform a charge correction on a stored result, however only, if the selected sample has been analysed through a quality, if not, an appropriate warning message will be given. In order to do this, the required result has to be selected in the upper list box. The charge correction can be performed directly by clicking onto the corresponding button or after a new quality check was performed and works in exactly the same way as after an analysis. A complete explanation of the charge correction can be found in Chapter Quantitative Analysis and in the WinXRF Configuration Manual. Results Retrieval & Statistics Chapter 8 AA83501 WinXRF Operator Manual 8-23 Send to SPC Analytical Results for Control Samples or Unknown Samples (Product Qualities) that have previously been analysed and stored can also be transferred to the SPC software. The results can be transferred either individually or as a group. The Send to SPC function allows the transfer of a selected group of results to the SPC software. Results for Setting-up Samples, Control Samples and Unknown Samples can be transferred. Note: No SPC alarms are returned when retrieved results are transmitted. AUTOMATION AND REMOTE SAMPLE DEFINITION MODES Automation and Remote Sample Definition Modes Chapter 9 AA83501 WinXRF Operator Manual 9-1 9 AUTOMATION AND REMOTE SAMPLE DEFINITION MODES This chapter describes the two Automatic Operation Mode options available with WinXRF: Automation Mode In this mode, WinXRF is under the control of a Host Computer. This is typically the case when a SMS Automation System is used. Remote Sample Definition Mode In this mode, the parameters necessary to perform an analysis (i.e. Task, Program, SIDs, Manual Inputs, etc.) on a unknown sample (production sample) are received from a Host Computer, but the operator still has the control over the analysis progress. This chapter describes how WinXRF has to be set up in order to operate in the two automatic modes and the features that are available when running in these modes. Automation Mode In this mode WinXRF is under the control of a Host Computer. This is typically the case when a SMS Automation System is used. Setting Automatic Mode In order to set WinXRF into Automatic Mode so that it can operate under the control of a Host Computer, you click on the Automation icon of the Production / Analysis as shown in the figure below. Chapter 9 Automation and Remote Sample Definition Modes WinXRF Operator Manual AA83501 9-2 Figure 9.1 The automatic mode starts in the same way as when it was left the last time. That means that either the dialog box in the following figure or the Results window shown in Figure 9.3 is displayed. Figure 9.2 Automation and Remote Sample Definition Modes Chapter 9 AA83501 WinXRF Operator Manual 9-3 Figure 9.3 Test Link Pressing this button checks whether communication with Host Computer has been established. It causes the enquiry Are you there to be sent and waits for the reply I am here. If this test is successful the following message is displayed. Automation. I am Here If communication cannot be established then the following error message is displayed. Timeout, automation system failed to reply. Some of the more likely causes of this message are as follows. 1) The Host Computer has not been set to operate in Automatic Mode. 2) The network software on the Host Computer is not operational. 3) The Host Computer is not physically connected to the network. 4) The WinXRF computer is not physically connected to the network. 5) The network software is not running on WinXRF. Display Results Selecting this button puts WinXRF into a mode where it can display the analytical results in a window. It initially displays a blank window as shown in Figure 9.3. As information is received from the Host Computer, the Analytical Task, Analytical Program and Sample Identifier will be displayed in the window. Then, as each analysis run is performed, the result values are displayed in the window in the same way as for standard WinXRF analysis. However, it is not possible to interact with this window. The average of runs is made according to rules defined within the Host Computer. Exit Results Display This button puts WinXRF automation back to the mode where results are not displayed. The dialog box shown in Figure 9.2 is displayed. Exit Automatic Mode This exits Automatic Mode and returns to the standard WinXRF. Similarly, the automation mode can also be left by clicking on the Exit automation mode icon of the Production / Analysis menu as shown in the figure below. Chapter 9 Automation and Remote Sample Definition Modes WinXRF Operator Manual AA83501 9-4 Figure 9.4 Using WinXRF in Automatic Mode When in Automatic Mode you can still use a few facilities within standard WinXRF. The facilities that are available are restricted, as access is only allowed to those items that will not affect the automatic operation. For example the Configuration Report menu can still be used as well as Results Processing and Alarms and Status Monitoring. The icons and options that are available can be seen by examining the various menus and folders while in automation mode. Automation and Remote Sample Definition Modes Chapter 9 AA83501 WinXRF Operator Manual 9-5 Remote Sample Definition Mode In this mode the parameters necessary to perform an analysis (i.e. Task, Program, SIDs, Manual Inputs, etc.) on an unknown sample (production sample) are received from a Host Computer, but the operator still has control over the analysis progress. Setting Remote Sample Definition Mode In order to set WinXRF into the Remote Sample Definition Mode so that it can receive the necessary parameters from a Host Computer, the Remote Sample Definition icon of the Production / Analysis menu has to be clicked (see figure below). Figure 9.5 The dialog box shown in the following figure is then displayed. This shows that WinXRF is in the Remote Sample Definition Mode. Chapter 9 Automation and Remote Sample Definition Modes WinXRF Operator Manual AA83501 9-6 Figure 9.6 The window is empty if there is no sample definition list available and both, the Sample Definition List and the Start Analysis buttons remain greyed. Otherwise the dialog box will contain a sample definition and the Start Analysis is available in order to measure the sample. Bad Sample Pressing this button creates a bad sample of the selection. Test Link Pressing this button checks whether the communication with Host Computer has been established. It causes the enquiry Are you there to be sent and waits for the reply I am here. If this test is successful the following message is displayed. Automation. I am Here If communication cannot be established then the following error message is displayed. Timeout, automation system failed to reply. Some of the more likely causes of this message are as follows. 1) The Host Computer is not in Remote Sample Definition Mode 2) The network software on the Host Computer is not operational. 3) The Host Computer is not physically connected to the network. 4) The WinXRF computer is not physically connected to the network. 5) The network software is not running on WinXRF. Sample Definition List This function is used to select the sample to perform the analysis from the list of sample definitions received from the host computer, as this is described in Section Using WinXRF in Remote Sample Definition Mode. Please note that this function remains greyed as long as the list is empty. Start Analysis This function is used to start the analysis using the selected sample definition. Please note that this function remains greyed as long as no sample definition is selected. Automation and Remote Sample Definition Modes Chapter 9 AA83501 WinXRF Operator Manual 9-7 Metaverage By pressing the Metaverage button, the WinXRF checks if there is any metaverage process ongoing. If this is not the case, an information message is displayed and once acknowledged, the WinXRF returns to the previous dialog box. The button is present only if the corresponding system option is enabled. See Chapter Metaverage Option. Exit Remote Sample Definition Mode This exits the Remote Sample Definition mode and returns to the standard WinXRF. Similarly, the remote sample definition mode can also be left by clicking on the Exit Remote Sample Definition icon of the Production / Analysis menu as shown in the figure below. Note: The list of available samples is not lost when exiting Remote Sample Definition Mode or WinXRF. Figure 9.7 Using WinXRF in Remote Sample Definition Mode As soon as a sample definition is received from the computer, or if the sample definition list is not empty, the option Sample Definition List is enabled, and when selected, the dialog box shown in the next figure will be displayed. Chapter 9 Automation and Remote Sample Definition Modes WinXRF Operator Manual AA83501 9-8 Figure 9.8 The samples that can not be deleted are shown in blue, and if such a sample is selected, the Clear button will be greyed. Following options are available: Sample Signature This is used to define a sample signature using the components available in this dialog box. Figure 9.9 Components The selected components compose the sample signature. Delimiter The delimiter is 1 character long. Any character with an ASCII code above 31 can be used, no character is interpreted as a space. Default If pressed, the default sample signature applies: Components: SID1 Delimiter: , (comma) Automation and Remote Sample Definition Modes Chapter 9 AA83501 WinXRF Operator Manual 9-9 Insert (End of Batch) after selection This is used to mark the end of the batch of samples that are to be analysed automatically. Clear This is used to clear the selected sample definition. Clear All This is used to clear all sample definitions in the list, except the ones marked in blue. OK If the OK button is pressed, but no component was selected, then a warning message that at least the component SID1 must be selected is displayed. After one or several samples have been selected and confirmed with OK, the former dialog box (see Figure 9.6), will be displayed again with the button Start Analysis enabled. When the analysis is started, the screen shown below will be displayed. Figure 9.10 When in Remote Sample Definition Mode you can still use a few facilities within standard WinXRF. The facilities that are available are restricted, as access is only allowed to those items that will not affect the automatic operation. For example the Configuration Report menu can still be used as well as Results Processing and Alarms and Status Monitoring. The icons and options that are available can be seen by examining the various menus and folders while in automation mode. METAVERAGE OPTION Metaverage Option Chapter 10 AA83501 WinXRF Operator Manual 10-1 10 METAVERAGE OPTION The Metaverage option is used to perform an average on different results of currently analysed samples. Note: The average on stored averaged results can be done with the Statistics function of the results retrieve facility. This chapter describes how WinXRF is used with the metaverage option and the features that are available when using this particular averaging mode. The chapter Metaverage Option of the WinXRF Configuration Manual explains how to set-up WinXRF in order to work with the metaverage facility. Manual Operation on Metaverage Process The metaverage process is monitoring every result to see if it is part of a metaverage scheme. If this is the case, it is stored for the future metaverage calculation. If the current result is the last one expected, then the WinXRF automatically goes to the metaverage creation function as described below. At any time (except when in Automation Mode), the operator can manually check, process or delete a metaverage state by pressing the Metaverage button as described by the next figures. If the system option Average of Analysis Results is not enabled, results are not scanned to see if they belong to a metaverage scheme. Chapter 10 Metaverage Option WinXRF Operator Manual AA83501 10-2 Figure 10.1 An additional button Metaverage is present. By pressing the Metaverage button, WinXRF checks if there are any metaverage processes ongoing. If this is not the case, an information message is displayed and once acknowledged, WinXRF returns to the window shown above. Another way to call the Metaverage function is to click on the Metaverage icon of the Results Processing folder in the Production / Analysis menu, as shown in the figure below. Metaverage Option Chapter 10 AA83501 WinXRF Operator Manual 10-3 Figure 10.2 If more than one metaverage process is ongoing, the user will be prompted to select one in the dialog box shown in the figure below. Figure 10.3 The metaverage scheme is selected by highlighting it and pressing the Select button. After this selection, the window shown in the next figure is displayed, similar as for a normal analysis. Chapter 10 Metaverage Option WinXRF Operator Manual AA83501 10-4 Otherwise, you may decide to delete one or all on-going metaverage operations. Deleting does not create a Bad Metaverage. Figure 10.4 The title bar indicates the current metaverage scheme operation. At the top of the window you can see the metaverage status. Pressing the button Proceed with Average forces the average creation after the OK button has been pressed in the following dialog box. Figure 10.5 You press on OK and you are returned to the Metaverage Operation window, but now the buttons at the bottom have changed as shown below. Metaverage Option Chapter 10 AA83501 WinXRF Operator Manual 10-5 Figure 10.6 Note: Some of the above buttons may be greyed, depending on the analytical task and available options. The buttons are following exactly the same rules as for a standard sample analysis. The availability of these buttons depends on the set-up of the UCN task selected for the metaverage processing. As mentioned above, the Metaverage Operation window for a specific process is also automatically displayed after reception of the final result analysis and when a manual operation is required from the operator. If the task used for the metaverage process is set for full automatic operation, then this Metaverage Operation window is displayed with only the Exit button active. In the previous window you can check or clear the check boxes to select or deselect averages when the analytical task allows it. If you just place the mouse pointer in the same area, a tooltip as shown in the next figure is displayed, indicating the full identity of the concerned average. This lets you check samples identities that can be very different from one sample to another. Chapter 10 Metaverage Option WinXRF Operator Manual AA83501 10-6 Figure 10.7 Quality Control of the Metaverage When the task selected for metaverage has the checkbox Quality Check enabled, you can use the Quality Check button while in the metaverage operation window. There are some cases where a quality control can be applied automatically to a metaverage without any operator action, both in manual or in automatic mode. The condition is that the task selected for metaverage processing allows quality checking and a quality is available as described below: First, the system uses the quality selected in the analytical category of the metaverage task. In this case, the metaverage identity will indicate this quality. If the metaverage task does not have any quality defined, WinXRF uses the quality defined in the metaverage identity (quality coming from the first result average in the process). If neither the metaverage task nor the identity indicates a quality, then no automatic quality check can take place. Metaverage Option Chapter 10 AA83501 WinXRF Operator Manual 10-7 Behaviour with Automated Modes Metaverage with Automatic Mode In automatic mode, the metaverage result is automatically processed as defined within the task. In automatic mode, the metaverage result is displayed directly after the last results analysis. The display is the same as the one used for standard results and the keyword ANALYSIS_DONE is sent to the host computer only once the metaverage is totally processed. Any error during the metaverage process is reported to the host computer through LOG_MESSAGE keywords only. In automatic mode, the user cannot force the access to the metaverage process as for the manual mode. If this is necessary, the user must exit the automatic mode and go to the manual mode of analysis. Metaverage with Remote Sample Definition Mode In remote sample definition mode, the user can also access the metaverage process as for the manual mode. The access to metaverage operation is done either through the standard Sample % window (see Figure 10.1) or as shown in the next figure. Figure 10.8 Note that the Metaverage button is available when this option is activated. Once the last result is analysed and if the metaverage scheme task requires it, the Metaverage Operation window is also automatically displayed for the operator to perform the necessary operation before exiting this window and returning to the remote sample definition window. ANALYSIS RECALCULATION OPTION Analysis Recalculation Option Chapter 11 AA83501 WinXRF Operator Manual 11-1 11 ANALYSIS RECALCULATION OPTION The main object of this function is to be able to recalculate concentrations of a particular sample some time after the analysis. This can be useful in cases such as: Recalculate a type standard update or a control sample analysis after a drift correction. This is used, for example, to check if the control sample is OK, without having to physically re-analyse it. Recalculate some production samples results after a drift correction. Recalculate production samples to test a calibration modification. It is possible to recalculate amongst the last 100 samples. It is clear that the main purpose to recalculate an analysis is to obtain new values after having made some modifications on drift correction parameters or on the calibration data. If this is not the case, then the result of the recalculation is going to be exactly the same as the original analysis. Another purpose of recalculation is to allow the user to add one or more physical measurements to a previous analysis. Finally, this recalculation can also be used for other purposes such as selecting different rules for creating an average or to reprocess a result with an alternative quality check. This system option must be activated. Refer to Section Set-up System Options in Chapter System Configuration of the WinXRF Configuration Manual. When activated, this option can be configured through the Recalculation Scheme icon that is described in Section Set-up Recalculation Scheme in Chapter Analytical Programs of the WinXRF Configuration Manual. Figure 11.1 According to the configuration of the option, the recalculation may be allowed for the following tasks: Concentration Analysis Type Standard Update Control Samples When the permission is checked for a task, a Recalculate button is added in the analysis preparation window, as this can be seen in Figure 11.2 below. Chapter 11 Analysis Recalculation Option WinXRF Operator Manual AA83501 11-2 Using Analysis Recalculation An analysis recalculation is initiated by pressing the Recalculate button, see figure below. Figure 11.2 When the button is pressed, the system checks if at least one sample is available for recalculation. If not, the message box shown in the figure below is issued and no other action is taken. Figure 11.3 Analysis Recalculation Option Chapter 11 AA83501 WinXRF Operator Manual 11-3 If one or more samples are available, a dialog with the list of available samples is displayed as shown in the next figure. Figure 11.4 The list shows the sample definition according to a sample signature defined earlier by the operator. Clear All Clears all samples available in the list. Clear Clears the selected sample in the list. Sample Signature The sample signature may be changed when you press this button. This calls another dialog box that is described in Section Changing Sample Signature. Redefine This button allows you to redefine the sample identifier, as well as the task, program (or type standard or quality) and manual inputs, of the selected (highlighted) sample. It calls the analysis preparation windows as shown in Section Redefining Recalculation Parameters. Recalculate This button starts the analysis recalculation process. It has the same effect as double clicking on a sample signature. OK This button becomes only available to validate changes made with the Clear or Clear All buttons. Cancel This button exits the function without validating changes made with the Clear or Clear All buttons. This does not affect the recalculation process itself. Chapter 11 Analysis Recalculation Option WinXRF Operator Manual AA83501 11-4 Changing Sample Signature When pressing the Sample Signature button (Figure 11.4) the following dialog box is opened. Figure 11.5 Components The checked components will be used to compose the signature. SID1 to SID10 check boxes remain all greyed when the sample signature dialog is called from a fixed sample name analysis mode (control sample or type standard). For this kind of samples, the fixed name is always displayed. Delimiter Enter the delimiter you would like between components. Characters below ASCII code 032 are not allowed. Default Recalls default dialog box values, as shown above. See Section Recalculation Process. Analysis Recalculation Option Chapter 11 AA83501 WinXRF Operator Manual 11-5 Redefining Recalculation Parameters When pressing the Redefine button (Figure 11.4) the following dialog box is opened. Figure 11.6 The window is similar to the normal analysis window, but notice the change in the title bar. It indicates that you are in an Analysis Recalculation process and all items that are not relevant here are hidden. You can modify the task, the program, the sample identifier, the manual inputs, the number of runs and the cassette number, as required. Within Concentration Analysis, you may change the quality, type standard or analytical program. Before an analytical program change is accepted, WinXRF checks that the channel list remains compatible between the new program and the original one. The analytical conditions of the two programs must also be equivalent, except the counting times. If the programs are not equivalent, WinXRF issues an error message and reselects automatically the original quality, type standard or analytical program. It is allowed to choose: a program with less elements. a program that uses different counting times. Chapter 11 Analysis Recalculation Option WinXRF Operator Manual AA83501 11-6 Recalculation Process When pressing the Recalculate button (Figure 11.4) the recalculation process is started. You can also start the recalculation by a double click on a sample signature. The sample result is recalculated instantly as if it was being analysed, according to the task category and the task configuration. If the number of runs has been increased, then WinXRF will analyse the sample as many times as given by the difference between the new and the former Number of Runs. The following message is also issued in this case. Figure 11.7 On confirming the warning message, the window shown in the figure below is then displayed. Figure 11.8 Analysis Recalculation Option Chapter 11 AA83501 WinXRF Operator Manual 11-7 When the Analysis Complete button is pressed the window shown in the next figure is displayed, allowing the actions that have been pre-defined in the selected task to be carried out. Figure 11.9 After pressing the Continue button, WinXRF returns to the window shown in Figure 11.4. You may then recalculate another sample or exit with the Cancel button. Results Retrieval The results retrieval function indicates when a result has been recalculated, beside the task category, on top of the first panel of the window, as shown in the next figure. Chapter 11 Analysis Recalculation Option WinXRF Operator Manual AA83501 11-8 Figure 11.10 Transmission to SPC It must be possible to indicate to SPC that a WinXRF result is a recalculated one. This can be done in the Set-up SPC Fields Definition dialog box. You can assign the Contents entry Recalculation Flag to any of the SPC fields, as shown in the figure below. However this item is only available in the combo box if the Analysis Recalculation system option is ON. Refer to Chapter SPC Option in the WinXRF Configuration Manual for directions on how to get the dialog box shown in the figure below. Analysis Recalculation Option Chapter 11 AA83501 WinXRF Operator Manual 11-9 Figure 11.11 Properties of Recalculated Results Recalculated results are treated as standard results. However, in order to differentiate them, they are qualified as Recalculated. Recalculated results are flagged in the result retrieval window (see Figure 11.10) and indicated in the different relevant transmission formats. Compac Format Type CMP?0_0? A recalculated sample is indicated by adding 100 to the Result type item as shown in the next table. 100 is chosen to be compatible with DBase and Lotus formats described next. Result Type Sample Analysis Recalculated Analysis Average 0 100 Bad Sample 1 101 Run in Average 2 102 Run not in Average 3 103 Run is Bad Run 4 104 Bad Analysis 5 105 Other Compac Formats Other Compac formats are left unchanged. Chapter 11 Analysis Recalculation Option WinXRF Operator Manual AA83501 11-10 DBase and Lotus Formats These formats have the run qualifier that gives either the run number or the negative run number when it is not included in an average. A run qualifier equal to 0 indicates either the average or a bad run. As run number can go up to 99, recalculated results are indicated by adding either 100 (good run, average) or 100 (run not selected) to the run qualifier. This also applies to Report formats. Telex A and Telex B Formats When transmitting a result using these formats the indication that the result has been recalculated is also transmitted. Printed Results Printed results on the local printer are indicated as recalculated when applicable. ASCII Format Recalculated results transmitted in ASCII format are reported in the following way (in comparison with the normal analysis). Run Number Sample Analysis Recalculated Analysis Average Average of n Recalculated average of n Bad Sample Is bad sample Is bad recalculated sample Run in Average m (in average) of n m (in recalculated average) of n Run not in Average m (not in average) of n m (not in recalculated average) of n Run is Bad Run m (is bad run) of n m (is bad recalculated run) of n Bad Analysis Is bad sample see note Is bad recalculated analysis Where m is the run number and n is the total number of runs in the average. ABOUT THE WINXRF SOFTWARE About the WinXRF Software Appendix A AA83501 WinXRF Operator Manual A-1 A ABOUT THE WINXRF SOFTWARE This section provides a basic explanation of actions to be carried out when using the WinXRF software. As WinXRF is a Windows based program, most functions and options are executed in the standard Windows way, only the graphics (i.e. MVR and Scan Graphics) make use of some particular non-standard Windows actions. It is not intended to explain the Windows environment in full details here, the user is therefore asked to consult the corresponding manual delivered with the system. The Mouse All WinXRF functions and options may be carried out using the mouse. Especially, for graphic treatments, the use of the mouse is the most efficient way of working. The mouse has either two or three buttons, which are used as follows: Left button This button is used for most functions with the WinXRF software. It carries out all selections, actions and functions. Middle button This button is not used with the WinXRF software, but can be programmed for double-click action on some systems (e.g. DEC). Right button This button is used for reverse zooming of the graphic displays (MVR, Scans) and for labelling peaks in Scan Graphics. Note: The actions of the left and right button can be switched with the Windows Control panel. The following terms are used in the manuals to describe actions carried out with the mouse: Click Quickly press and release the mouse button. Double-click Click the mouse button twice in rapid succession. Drag Hold down the mouse button while the mouse pointer is moved. Point Move the mouse pointer until the tip is on the desired item. Highlight Move the mouse pointer to the desired item in a list box and click the left mouse button. Select Choose an action by clicking the mouse button while pointing at the desired push button. Choose an option by clicking the left mouse button while pointing at the desired Check box or Radio button. Special Keys The following keys and key combinations help to execute the most frequently used operations rapidly and without use of the mouse. The + sign indicates that the keys must be pressed simultaneously. <ALT> or <F10> Selects (highlights) or cancels the selection of the first menu in the menu bar. Appendix A About the WinXRF Software WinXRF Operator Manual AA83501 A-2 <ESC> Cancels the menu selection or closes the open menu or dialog box. <ALT> + <ESC> Activates (selects) windows and icons (i.e. applications). <ALT> + <TAB> Switches between the present applications. <ALT> + <F4> Closes the activated window or icon (i.e. application). <ALT> + <SPACE> Opens the system menu in an application window. <CTRL> + <F4> Closes the active group window. <ALT> + <ENTER> Changes the window of a non-window application (e.g. UniQuant) from full screen to a window. <TAB> Selects the options presented in a dialog box from left to right and from top to bottom. <SHIFT> + <TAB> Selects the options presented in a dialog box from right to left and from bottom to top (reversed TAB). <CTRL> + <ALT> + <DEL> Is used to cancel active tasks that are no longer responding. <V> Displays the license box. <Print Screen> Copies the screen into the Clipboard. <ALT> + <Print Screen> Copies the active window into the Clipboard. <CTRL>+<TAB> Moves selection between group windows and icons in the Program Manager. <F2> Invokes the Concentration Analysis function. <F3> Invokes the Drift Correction Update function. <F4> Invokes the Type Standard Update function. <F5> Invokes the Unattended Analysis function. <F6> Displays the dialog box to Reset and Initialise the ICS. <F7> Reads and displays the Instrument Status. <F8> Invokes the Results Retrieval & Statistics function. <F9> Invokes the SPC program. Selection of a Group of Items A group of items, such as elements and channels in MVR (see next figure) are easily selected with the mouse. However, these items can also be selected using the keyboard. About the WinXRF Software Appendix A AA83501 WinXRF Operator Manual A-3 Figure A.1 1. Individual selection: Move with the t and/or s +t keys and the direction keys w x y z to highlight the item in the Available list box e.g., Elements, and press the } key. This item is then copied into the Selected list box. 2. Group selection: Move with the t and/or s +t keys and the direction keys w x y z to highlight the first item of the desired group in the Available list box e.g., Samples. Then move with the t key onto the Group command button and press the } or e key, come back to the Available list box with the t and/or s +t keys and the direction keys w x y z to select the last item of the desired group. Now press the } or e key twice rapidly (to simulate a double-click) and this group of items is then copied into the Selected list box. Appendix A About the WinXRF Software WinXRF Operator Manual AA83501 A-4 Windows Terminology The figure below shows the principal components of an Application Window. A short description follows. Figure A.2 Application Window This is the main window of an application such as Windows Explorer or WinXRF. Mouse Pointer The arrow-shaped mouse pointer appears if a mouse is installed. It moves in synchronism with the mouse movements performed on the table or the mouse pad. When the system is busy the arrow-shaped mouse pointer is changed to an hourglass and the mouse button clicks are inhibited until the current operation is completed. Control Menu Box This box is located in the upper-left corner of every window and most dialog boxes. The Control Menu (also called the System Menu) is most useful if you prefer to use the keyboard instead of the mouse to resize, move, maximize, minimize, close a window or dialog box. With the mouse the same operations can simply be performed by clicking and dragging. About the WinXRF Software Appendix A AA83501 WinXRF Operator Manual A-5 Title Bar The name of the application is shown on this bar. If more than one window is open, the title for the active window is in a different colour or intensity than the other title bars. Window Title Depending on the type of window, the window can be the name of the application or the name of the document. Menu Bar This bar contains the available menus. They consist normally of pull-down menus, e.g. by clicking on one of the menu items a list of sub-menus opens. Further sub-menus may be presented in the same way depending on the complexity of the menu structure. Maximize and Minimize Buttons These buttons enlarge the active application window to fill the entire desktop or shrink the window to an icon. After a window has been enlarged, the Maximize button changes to a Restore button, i.e. both arrows are combined in the same little square box. By clicking onto the Restore button the window returns to its previous size. Window Border This is the outside edge of a window. When the mouse pointer is moved onto this border, the pointer symbol changes to indicate that the size of the window can be changed by a dragging action in the corresponding left/right or up/down direction. Window Corner When the mouse pointer is moved onto one of the corners, the pointer symbol changes to indicate that the size of the window can be changed by a dragging action in a diagonal direction. Workspace This is the area limited by the window border. Most WinXRF windows and dialog boxes have a fixed size that is big enough to display all the information presented in the window. Therefore, the size of such windows can not be changed. Desktop This is the background of the screen on which the different windows, symbols and dialog boxes appear. Dialog Box A dialog box is an area (or window) in which input information is requested, to define further actions and parameters or, for the execution of operations. It may also contain relevant information for guidance. The main components of a dialog box are: Push (Command) Buttons A click on these buttons initiates an immediate action or displays a new dialog box. Edit (Text) Boxes An edit box is used to enter specific information. If the box already contains text, the entire string is automatically highlighted when the edit box is selected with the TAB key. List Boxes A list box contains a list of available choices. If there are more choices than can fit in the list box, scroll bars are provided so that the mouse can be used to move quickly through the list. As an alternative, an item can be quickly located by pressing its first letter. This is most useful for long lists, like the Line Library. Combo Box This is an extendable list box, i.e. in order to choose an item, it has to be opened by clicking onto the corresponding symbol. Radio Buttons (Option Buttons) Appendix A About the WinXRF Software WinXRF Operator Manual AA83501 A-6 Radio buttons are grouped, but mutually exclusive, choices of an option. Only one of the available options can be selected at one time. They got their name because of old radio receivers, which had a range of push buttons to select the wavelength band. Check Boxes Check boxes allow selection of options which are not exclusive. None, a few or all of the presented options may be selected. A X in the corresponding square indicates the selection of an option. WINXRF ICONS WinXRF Icons Appendix B AA83501 WinXRF Operator Manual B-1 B WINXRF ICONS Icon Composition and Colours Commands and functions are represented by graphical icons or shortcuts. Each icon is composed by a base background, called a polygon, and one or two specific symbol(s) called element(s), like the examples below. Main element Secondary element Shorcut sign Polygon Figure B.1 Meaning of the Colours The colours used are limited to six. 0,0,0 RGB code Name 255,255,255 133,163,206 12,71,144 254,23,28 255,255,0 Black White Light Blue Dark Blue Red Yellow Figure B.2 Black is used as outline only, for elements and yellow polygons. White is used in the design of elements only. Light Blue is used as outline only, for dark blue polygons. Dark Blue is used for general polygons only. Appendix B WinXRF Icons WinXRF Operator Manual AA83501 B-2 Red is used in the design of elements only. Yellow is used for check polygons only. Meaning of the Polygons There are seven base polygons. They give information on the general operation concerned. Generic Icon Instrument General Analysis Task Instrumental Check Check Task QuantAS Figure B.3 WinXRF Icons Appendix B AA83501 WinXRF Operator Manual B-3 Meaning of the Elements The elements used by WinXRF are summarised below. Automatic Status (action and measurement result) Manual operation on instrument Report and display Production, Home Drift (raw data) Unattended batch analysis Results database Status, Alarm state Algorithm, Computation Deleting Quality Type Standard (calculated/organised data) Calibration (calibrated data) Control sample Detector High Voltage Permission Security access Transmission destinations Import (world) Export (world) Edition Initialisation, Reset Update Materials Configuration database Import (ARL) Manual input Exit Icon / Tree mode Export (ARL) SPC R & R Short-cut Environment X-Rays Theta Report and display scans Selection, Choice, Sorting Figure B.4 Appendix B WinXRF Icons WinXRF Operator Manual AA83501 B-4 Other Symbols The other symbols used are shown below. Folder (closed) Folder (open) Folder up Figure B.5 WinXRF Icons Appendix B AA83501 WinXRF Operator Manual B-5 All WinXRF Icons and Shortcuts Icons The icons used by WinXRF are shown below. Menu Function Frame and Log In Home (back to shortcuts) Log off Exit Tree / Icon mode (toggle) About WinXRF Figure B.6 Generic Icons These icons may be used several times. Analysis: - Import old format Database Report and Edition report: - External Analysers - Firmware Status - Instrument - Sample Identity Scheme Deleting: - Clear External Analysers Data Selection: - System Options - Change Language Edition: - Monochromator Line Library - Analytical Conditions - Recalculation Scheme - Sample Identity Scheme - Absolute Tolerance for Metaverage Initialisation: - Instrument Emulator - Reset Instrument - Instrument - Printer Modes - Inclusion - Firmware Status - External Analysers - Report Alpha Factors - Monochromator Line Library - Monochromators - Monochromators - Primary Beam Device - Headers and Footers Figure B.7 Appendix B WinXRF Icons WinXRF Operator Manual AA83501 B-6 Instrument Icons With one element: Automation (mode) Instrument (configuration) Concentration Analysis (also shortcut) Send Instrument Configuration Read Instrument Status Terminal Mode View Scans Run Scans Unattended Analysis Set X-Rays Set Environment Figure B.8 With two elements: Remote Sample Definition (mode) Intensity Measurement Calibration Standard Measurement Analytical Programs (report) Measure Intensities (UniQuant) Report Scan Parameters Energy Profile Graphics Report Energy Profile Figure B.9 WinXRF Icons Appendix B AA83501 WinXRF Operator Manual B-7 Analytical Programs (preparation) Set up Monitoring Status Channel Alarms (configuration) Program Choice Position Calibration Parameters Eco Mode Parameters HV Graphics (Goniometer Calibration) HV Parameters (Gonio. Cal. report) HV Parameters (Mono. Cal. report) Instrument Configuration Report Run Energy Profile Batch Operation Metaverage 2 Theta Angle Calculation Position Calibration Coefficients Position Calibration Scan Parameters Set Energy Profile Set Batches Status Monitoring Status Channel (Configuration) Alarm Monitoring Alarms (Configuration) HV Calibration Coefficients HV Calibration Calibration Standards (report) Figure B.10 Appendix B WinXRF Icons WinXRF Operator Manual AA83501 B-8 Calibration Standards (preparation) Status Reporter (initialisation) Initialise Alarm and Status Logger Terminal Mode Script Exit Automation mode Exit Remote Sample Definition (mode) Eco Mode Setting HV Calibration Parameters Metaverage Scheme Goniometer (Instrument Config.) Position Calibration Parameters Prepare Programs (UniQuant) Zero Goniometer Figure B.11 General Icons With one element: Results Database (retrieve) (also shortcut) SPC Offline Analysis Figure B.12 WinXRF Icons Appendix B AA83501 WinXRF Operator Manual B-9 With two elements: Report 1 to 4 (on display) Report 1 to 4 (on printer) MVR Qualities (report) Alloy / Quality Sort (report) Clear (results) Control Samples (report) Result Transmission Properties Password (report) Delete Configuration Files Remote Destinations (report) Device Parameters (report) Select / Create (results database) Charge Correction Materials (report) Correction Material Selection (report) Alloy / Quality Sort (preparation) Manual Inputs (report) Correction Material Selection (preparation) SPC Rules and Actions (report) SPC Transmission (report) Merge (results) Statistics (on display) Statistics (on printer) Virtual Elements (report) Line Library (report) Mask (Configuration Database) Figure B.13 Appendix B WinXRF Icons WinXRF Operator Manual AA83501 B-10 CSV Output Calibration Standards Select (configuration database) Layout Configuration Manual Inputs (preparation) Qualities (preparation) Set Shortcuts Create Calibration File SPC Rules and Actions (preparation) Permissions (configuration Revive (results database) Password (configuration) Update / Create (configuration database) Remote Destinations (configuration) Charge Correction Materials (preparation) Result Modification SPC Transmission (preparation) CSV Input Calibration Standards Calibration Modification Logging Virtual Elements (preparation) Alpha factors (preparation) Line Library (preparation) Figure B.14 WinXRF Icons Appendix B AA83501 WinXRF Operator Manual B-11 Import Calibration Standards Export (configuration database) R & R Report Generator Export Calibration Standards Figure B.15 QuantAS Icons With one element: View Scans Standardisation / Drift Correction Update Run Scans QuantAS Standards Figure B.16 With two elements: Report QuantAS Standards Figure B.17 Analysis Task Icons With one element: Concentration Analysis (automation task) Concentration Analysis (manual task) Calibration (task) Figure B.18 Appendix B WinXRF Icons WinXRF Operator Manual AA83501 B-12 With two elements: Intensity Measurement (task) Prepare Tasks (UniQuant) Figure B.19 Instrumental Check Icons With one element: Standardisation / Drift Correction Update (also shortcut) Control Sample Analysis (also shortcut) Type Standard Update (also shortcut) Figure B.20 With two elements: Setting-Up Sample (report) Type Standards (preparation) Type Standards (report) Define Control Samples Standardisation / Drift Correction Initialisation Type Standard Initialisation Define Global List Setting-Up Samples (preparation) Figure B.21 WinXRF Icons Appendix B AA83501 WinXRF Operator Manual B-13 Check Task Icons With one element: Standardisation / Drift Correction Update (preparation manual task) Control Sample Analysis (preparation manual task) Type Standard Update (preparation manual task) Figure B.22 With two elements: Standardisation / Drift Correction Update (preparation automation task) Type Standard Update (preparation automation task) Control Sample Analysis (preparation automation task) Standardisation / Drift Correction Initialisation (preparation task) Type Standard Initialisation (preparation task) Figure B.23 Appendix B WinXRF Icons WinXRF Operator Manual AA83501 B-14 Shortcut and Desktop Icons The shortcuts used by WinXRF are shown below. Results Database (retrieve) Concentration Analysis Standardisation / Drift Correction Update Control Sample Analysis Type Standard Update Run Scans Batch Operation Run Scans (QuantAS) Figure B.24 And the corresponding desktop icons Results Database (retrieve) Concentration Analysis Standardisation / Drift Correction Update Control Sample Analysis Type Standard Update Run Scans Batch Operation Run Scans (QuantAS) Figure B.25 INDEX Index AA83501 WinXRF Operator Manual I INDEX A Abort Instrument Operations, 1-25 Air, 1-18 Alarm Reporter, 1-21 Alpha and Beta Report, 5-9 Alternative Lines, 3-32 Analysis Bad Sample ~, 4-7 Concentration ~, 4-2 Control Sample ~, 6-1 Menu, 5-3 Quantitative ~, 4-1 Semi-quantitative ~, 3-1 Unattended ~, 7-2 UniQuant ~, 3-17 Append Message, 8-16 Application Window, A-4 Area Viewed ~, 3-27 Automatic Mode, 4-28 Set ~, 9-1 Peak Identification, 2-14 Sample Definition Mode, 9-5 Scan Identification, 2-2, 2-13 Automatic Drift Correction Control, 4-8 Average Calculation, 4-30 B Bad Sample, 7-4 Analysis, 4-7 Result, 4-7 Transmission, 6-10 Bar Identification ~, 2-18 Batch Operation, 7-1, 7-7 Binary Format, 8-14 C Calculation Average ~, 4-30 Case Numbers, 3-34 Change Program, 4-5 Task, 4-4, 6-4, 8-4 Charge Correction, 4-18, 8-22 Weight, 4-22 Check Quality ~, 4-15, 8-20 Communication Instrument ~, 1-23 Complete QuantAS Analysis, 3-10 Concentration Analysis, 4-2 Condition X-Ray Tube ~, 1-19 Configure Instrument, 1-17 Control Sample Analysis, 6-1 Global ~, 6-1 Correction Charge ~, 4-18, 8-22 Drift ~, 5-1 Criteria Results Retrieval ~, 8-2 D dBase Format, 8-15 Default, 4-9 Program, 7-5 Save as ~, 8-4 Define Materials, 3-30 Device Export to ~, 8-15 Differential Graph, 2-21 Dilution, 4-23 Display Instrument Status, 1-21 Mode, 4-30 Display Results Automation, 9-3 Documentation Software ~, 1-2 Index WinXRF Operator Manual AA83501 II Drift Correction, 5-1 Automatic ~, 4-8 Selective ~, 5-6 Update, 5-1 Report, 5-9 Warning, 5-9 E EJOB, 3-21 Element Show ~, 2-11 Environment Spectrometer ~, 1-18 EXAN, 4-10 Exit (WinOE), 1-31 Export Format ~, 8-13 Results, 8-12 External Analysers, 4-10 F Flags Result ~, 4-10 SPC ~, 6-11 Format Binary ~, 8-14 dBASE ~, 8-15 Export ~, 8-13 Lotus 123 ~, 8-14 Readable ~, 8-14 Full Headings, 4-28 G Global Control Samples List, 6-1 Goniometer Zero ~, 1-19 Graph Label, 2-17 H Helium, 1-18 I ICS Operations Manager, 1-25, 7-6 Identification Bar, 2-18 Manual ~, 3-9 Peak ~, 2-12 Scan ~, 2-11 Tag, 2-18 Inform Operator, 5-9 Initialisation Instrument ~, 1-16 Instrument Alarms, 1-21 Communication, 1-23 Configure, 1-17 Initialisation, 1-16, 1-23 Reset ~, 1-23 Intensity Measurement, 4-32 Interactive QuantAS Analysis, 3-5 J JOB, 3-24 K Keys Special ~, A-1 L Log Off, 1-31 Log on, 1-15 Logging into WinXRF, 1-12 Lotus 123 Format, 8-14 M Manipulation Step List ~, 7-6 Manual Identification, 3-9 Mode, 4-28 Run Selection, 4-13 Sample Mode, 4-6 Scan Identification, 2-11, 2-14 Mass Viewed ~, 3-32 Materials Define ~, 3-30 Measurement Intensity ~, 4-32 Measuring Task UniQuant ~, 3-19 Index AA83501 WinXRF Operator Manual III Menus Routine Analysis, 5-3 Message Append ~, 8-16 SPC ~, 6-10 Mode Automatic ~, 4-28 Display ~, 4-30 Manual ~, 4-28 Print ~, 4-28 Semi-Automatic ~, 4-28 Storage ~, 4-29 Transmit ~, 4-29 Mode ~ Automatic Sample Definition, 9-5 Modification of Results, 8-11 Result ~, 4-27 Monitor Samples, 5-13 Moseley, 2-7, 2-21 Mouse, A-1 Pointer, A-4 Multiple QuantAS Analyses, 3-5 N NJOB, 3-21 O On-Line Scanning, 2-2 Operation Batch ~, 7-1, 7-7 Unattended ~, 7-1 Options Result ~, 4-27 P Parameter Scan ~, 2-1 Password Protection, 1-15 Peak Identification, 2-12 Automatic ~, 2-14 Pre-defined Sample list, 7-3 Sample Mode ~, 4-6 Print Mode, 4-28 Procedure Transfer ~, 6-10 Program Change ~, 4-5 Default ~, 7-5 Protection Password ~, 1-15 Q Quality Check, 4-15, 8-20 Select ~, 8-20 Sort, 4-17, 8-21 QuantAS, 3-1 Analysis Complete ~, 3-10 Interactive ~, 3-5 Multiple ~, 3-5 Single ~, 3-1 Recalibration, 5-10 Quantitative Analysis, 4-1 R Readable Format, 8-14 Recalibration, 5-1 QuantAS ~, 5-10 Report Alpha and Beta ~, 5-9 Drift ~, 5-9 Reset Instrument, 1-23 Result Bad Sample ~, 4-7 Export, 8-12 Flags, 4-10 Modification, 4-27, 8-11 Options, 4-27 Transmission, 8-15 Results Retrieval, 8-2 Actions, 8-9 Criteria Daily Period, 8-7 Result Type, 8-8 Sample Identity, 8-7 Time and Date, 8-7 Procedure for ~, 8-3 Retrieve Results Procedure for ~, 8-3 Selection Criteria, 8-2 Routine Analysis Menu, 5-3 Run Selection Manual ~, 4-13 Index WinXRF Operator Manual AA83501 IV S Sample List Pre-defined ~, 7-3 Mode Manual ~, 4-6 Monitor ~, 5-13 Samples Setting-up ~, 4-9 Save as Defaults, 8-4 Scan Graphics, 2-4 Identification, 2-11 Automatic ~, 2-2, 2-13 Manual ~, 2-11, 2-14 Parameter, 2-1 Select Quality, 8-20 Selection Criteria, 8-2 Selective Drift Correction, 5-6 Semi-Automatic Mode, 4-28 Semi-quantitative Analysis, 3-1 Set Automatic Mode, 9-1 Setting-up Sample, 4-9 Show Element, 2-11 Single QuantAS Analysis, 3-1 Software Documentation, 1-2 Sort Quality ~, 4-17, 8-21 SPC Flags, 6-11 Message, 6-10 Transfer, 4-30 Transfer to ~, 8-23 Special Identifications, 2-15 Keys, A-1 Spectrometer Environment, 1-18 Statistics, 8-16 Step List Manipulation, 7-6 Storage Mode, 4-29 Subset Program UniQuant ~, 3-35 T Tag Identification ~, 2-18 Task Change ~, 4-4, 6-4, 8-4 Terminology Windows ~, A-4 Transfer Procedure, 6-10 SPC ~, 4-30 to SPC, 8-23 Transmission Bad Sample ~, 6-10 Transmit Mode, 4-29 Results, 8-15 Type Standards, 4-9 U Unattended Analysis, 7-2 Operation, 7-1 UniQuant Analysis, 3-17 Export Format, 8-14 Measuring Task, 3-19 Subset Program, 3-35 Update Drift Correction ~, 5-1 User name, 1-15 Utilities Log Off, 1-31 V Vacuum, 1-18 Viewed Area, 3-27 Mass, 3-32 W Warning Drift ~, 5-9 Weight Charge ~, 4-22 Wild Card, 8-7 Windows Application ~, A-4 Index AA83501 WinXRF Operator Manual V Terminology, A-4 WinXRF Automatic Mode, 10-1 Logging into ~, 1-12 X X-Ray Tube Condition, 1-19 Z Z - Scale, 2-20 Zero Goniometer, 1-19 Zooming Scan Graphs, 2-16 Thermo ARL ARL Applied Research Laboratories S.A. 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