Reference and Guide v. 2.09

Transcription

1 Probe for Windows Reference and Guide v By John J. Donovan (C) Copyright by John J. Donovan

2 Contents Introduction 1 Description...1 Special Thanks...1 Technical Support... 2 Analysis Concepts... 2 References... 3 Comparison to PROBE for DOS...5 Floating Point Calculations... 5 Data File Access... 5 User Interface... 5 Disclaimer... 6 Installation 7 Platform Requirements... 7 Minimum...7 Preferred...7 Installation from Floppy... 8 Modifying the AUTOEXEC.BAT File... 8 Running Probe for Windows for the First Time... 9 Files That Can be Deleted After the Installation...9 Configuration Files Constants for array declarations PROBEWIN.INI ELEMENTS.DAT...27 CRYSTALS.DAT MOTORS.DAT...30 SCALERS.DAT Overview of Programs 39 Program PROBEWIN Program STANDARD...39 Running Standard for Windows for the First Time...40 Importing Standard Compositions from PROBE for DOS Program STARTWIN Program STAGE Program JOYWIN Program USERWIN...42 STARTWIN Overview 43 Description...43 Beam and Detector Stability Spectrometer Reproducibility STAGE Overview 45 Probe for Windows Reference and Guide v Contents i

3 Description...45 Importing Standard Position Data from Probe for DOS Digitize Positions...45 Grid Minerals...46 JOYWIN Overview 47 Description...47 Feature Details...47 USERWIN Overview 48 Description...48 Creating a New User Database Calculating Hourly Usage Using the Data Cursor...49 Modifying the Custom Data Fields Standard for Windows Overview 50 Log Window Standard for Windows Menu Details 52 File...52 New...52 Open Save As Close...53 Import Export File Information...54 Print Log Print Setup...54 Exit Edit...54 Cut Copy Paste...54 Select All...55 Clear All Standard...55 New...55 Modify...57 Delete...57 Delete Selected List Standard Names List Selected Standards List All Standards Options...58 Find Match...58 Modal Analysis Interferences XRay XRay Database Emission Table Edge Table...62 Fluorescent Yield Table Probe for Windows Reference and Guide v Contents ii

4 MAC Table Analytical...62 Empirical MACs ZAF Selections Operating Conditions...63 Output Log Window Font Debug Mode Extended Format Save To Disk Log View Disk Log Help About STANDARD Help On STANDARD...64 Probe for Windows Overview 65 Log Window Menus...65 Buttons...66 Probe for Windows Modeless Window Details 67 Acquire!...67 New Sample...68 Elements/Cations...70 Analytical Conditions Locate PHA...75 Count Times Move Peak/Scan Options...80 Rate Meter...80 Acquisition Options...80 Start Peak Center...81 Peaking Start Sample Count Start Wavescan Volatile QuickScan Analyze!...84 Analyze Data KRaws Analyze Selected Line(s)...91 Delete Selected Sample(s)...91 Undelete Selected Sample(s)...92 Specified Concentrations...92 Standard Assignments...92 Name/Description Conditions Elements/Cations...98 Delete Selected Line(s) Undelete Selected Line(s) List Report Calculation Options Automate! Select Stds Select All Probe for Windows Reference and Guide v Contents iii

5 Delete All Move Digitize Plot Fiducials Peaking Conditions Setups Delete Selected Samples Delete Selected Positions Export Selected Samples Import From ASCII File Automation Actions Automation Options Run Selected Samples Plot! Select All Output Target Graph Type Output Close Probe for Windows Menu Details 120 File New Open Save As Close Import Find File File Information Print Log Print Setup Exit Edit Cut Copy Paste Select All Clear All Standard Standard Database Add Standards To Run XRay XRay Database Spectrometer Table Emission Table Edge Table Fluorescent Yield Table MAC Table Analytical Analysis Options MAN Fits Empirical MACs Empirical APFs ZAF Selections Student's "t" Table Run Probe for Windows Reference and Guide v Contents iv

6 List Run Summary List Sample Names List Standard Counts List Standard Compositions List Current MACs Output Log Window Font Debug Mode Extended Format Save To Disk Log View Disk Log Help About PROBE Help On PROBE Appendix A 144 Probe for Windows Import File Format Sample Import File (full version) : Sample Import File (minimal File Info section) : Appendix B 156 Problems with Light Element Analysis Physical and Chemical Effects Problems with the Measurement Techniques Appendix C 158 Use of Empirical MACs Empirical Mass Absorption Coefficients (MACs) Appendix D 162 Problems With the Analysis Glossary of Terms 164 Index 174 Probe for Windows Reference and Guide v Contents v

7 Introduction Description Probe for Windows is a complete acquisition, automation and analysis package for WDS (wavelength dispersive) EPMA (Electron Probe Micro-Analysis) running under Windows 3.1, Windows For Workgroups 3.11 or Windows95, on Intel 486 or Pentium computers. Probe for Windows can automate and acquire x-ray intensities on JEOL, ARL and Cameca microprobes with WDS spectrometers and stage motors. Probe for Windows can also import and re-process x-ray intensity ASCII data files from PROBE for DOS or other sources. Probe for Windows can also be run off-line to simply re-process previously acquired x-ray intensity data. Because Probe for Windows stores all standard, unknown and wavescan sample data and retains all experimental conditions in a single Microsoft Access relational database file, it is extremely simple to transfer Probe for Windows data to another computer for off-line reprocessing. Probe for Windows is written primarily in Visual Basic 3.0 (Professional) for Windows and utilizes several external DLLs (Dynamic Link Libraries) for data access, automation and graphics written in C++ or assembler. Special Thanks The author would like to thank John T. Armstrong for his valuable contribution of the CITZAF quantitative matrix correction routines. Also Dan Snyder for help with the mathematical codes and Mark L. Rivers for his work on the quantitative interference and iterated MAN corrections and Dan Kremser and Tracy Tingle for extensive beta testing and John Friday for help with the hardware interfacing code. And most of all, my wife Barbara, for her patience and support throughout the development of this program. Probe for Windows Reference and Guide v Introduction 1

8 Technical Support Technical support for Probe for Windows is provided by Advanced MicroBeam, Inc. Please contact Don Lesher or Dave Stanford at (330) for any questions or difficulties you may have with Probe for Windows. If an error message or software bug is seen, please note the exact error message and record as many details of the incident as you can to help us in determining a solution to your problem. Suggestions regarding new features or improvements to Probe for Windows are always welcome and every effort will be made to incorporate them in future releases. If you have an idea for a new feature, we would like to hear about it. Please write the author at the address below or call anytime. John Donovan Advanced MicroBeam 4217 C Kings Graves Road Vienna, OH (330) @CompuServe.com (John Donovan or Dave Stanford) @CompuServe.com (Don Lesher) Analysis Concepts One significant difference between Probe for Windows and other microprobe analysis programs is that Probe for Windows treats all samples, regardless of whether they are standard or unknown samples, in exactly the same manner. This begins with the data acquisition; Probe for Windows can acquire a complete analysis for every standard sample, just as it would for an unknown sample. For example, if in a particular run you are analyzing for Si, Al, Na and K, then by default, Probe for Windows can acquire data for all four elements on each standard. This means that even if a standard is only used to calibrate Si, the x-ray count data for the other three elements, Al, Na, K can also be acquired on that standard. Measuring all samples in the same manner under the same conditions can eliminate errors that may be introduced in the analysis from beam and sample interactions, especially when beam charge buildup, carbon buildup or volatile element effects are present in the samples. Although the time needed to acquire standard data is not any longer for this method when the analysis is measuring only one element on each spectrometer, it is true that acquiring more than one element on a spectrometer will increase the time required for standard calibration. This might be considered a small price to pay for the increased accuracy and flexibility of measuring both standards and unknown for the same elements. However, to save time, program Probe for Windows Probe for Windows Reference and Guide v Introduction 2

9 does allow the acquisition of "quick" standards for those standards used in the primary calibration. Note that acquisition of these "quick" standards will restrict the use of some of the unique analysis features discussed below. Aside from the obvious value in keeping the analysis conditions constant for all samples, having the complete data for each standard at hand, provides the analyst with several useful capabilities. Among these is a unique standard re-assignment feature. Since all elements in the run are acquired for all standards, any standard containing a particular element can be assigned as the calibration standard for that element at any time, even when processing off-line. Another benefit to complete standard analysis is the ability to calculate each standard analysis as if it were an unknown. This means that every standard is also a secondary standard. In this way, one can easily determine the accuracy of each element in the run (and the overall accuracy of the run by noting the totals on each standard). If an element is present in a standard but is not assigned as the calibration standard for that element, then the program will calculate the relative error in the analysis based on the assigned standard. In this way one can check for agreement between various standards in the run. If the element is not present in the standard, the analysis provides a check on the accuracy of the off-peak or MAN background correction and also as a check for possible interferences. In addition, the quantitative interference correction in Probe for Windows uses this additional data to calculate the effect of an interfering element on an interfered channel. Again, since all elements are acquired for each standard and the composition of each standard is of course already known, the count to the concentration ratio of the interfering element can be calculated. This in turn can be used in the ZAF composition iteration to quantitatively calculate the interference correction in an unknown sample (Donovan, et. al., 1993). References J. T. Armstrong and P. Buseck, "Quantitative Chemical Analysis of Individual Micro-particles using the Electron Microprobe" Anal. Chem. 47: 1975, p 2178 J. T. Armstrong, "Quantitative analysis of silicates and oxide minerals: Comparison of Monte-Carlo, ZAF and Phi-Rho-Z procedures," Microbeam Analysis--1988, p J. T. Armstrong, "Bence-Albee after 20 years: Review of the Accuracy of a-factor Correction Procedures for Oxide and Silicate Minerals," Microbeam Analysis--1988, p G. F. Bastin and H. J. M. Heijligers, "Quantitative Electron Probe Microanalysis of Carbon in Binary Carbides," Parts I and II, X-ray Spectr. 15: , 1986 W. A. Deer, R. A. Howie, J. Zussman, "An Introduction to the Rock Forming Minerals", Longman, Essex, London, 1966 Probe for Windows Reference and Guide v Introduction 3

10 J. J. Donovan and M. L. Rivers, "PRSUPR: A PC-Based Automation and Analysis Software Package for Wavelength-Dispersive Electron-Beam Microanalysis" Microbeam Analysis, 1990, p J. J. Donovan and V. C. Kress, "PRTASK: A PC-Based Acquisition and Analysis Software Package for Interfacing to the Tracor TASK Automation System" Microbeam Analysis, 1991, p. 351 J. J. Donovan, M. L. Rivers and J. T. Armstrong, "PRSUPR: Automation and Analysis Software for Wavelength Dispersive Electron-beam Microanalysis on a PC" in Am. Mineral., v. 77, 1992, p. 444 J. J. Donovan, D. A. Snyder and M. L. Rivers, "An Improved Interference Correction for Trace Element Analysis" Microbeam Analysis, 2: 23-28, 1993 J. J. Donovan and T. N. Tingle, "An Improved Mean Atomic Number Correction for Quantitative Microanalysis" in Journal of Microscopy, v. 2, 1, p. 1-7, 1996 J. Z. Frazer, ISM Report 67-29, J.I. Goldstein, D.E. Newbury, P. Echlin, D.C. Joy, C. Fiori, E. Lifshin, "Scanning Electron Microscopy and X-ray Microanalysis", Plenum, New York, 1981 K. F. J. Heinrich, Proc. 11th ICXOM, 1987, p. 67. K. F. J. Heinrich, "Mass Absorption Coefficients for Electron Probe Microanalysis" in Proc. 11th ICXOM 67: 1, B. L. Henke, P. Lee, T. J. Tanaka, R. L. Shimabukuro and B. K. Fijikawa, Atomic Data Nucl. Data Tables 27, 1 (1982) B. L. Henke and E. S. Ebisu, Adv. X-Ray Anal. 17, 150 (1974) McQuire, A. V., Francis, C. A., Dyar, M. D., "Mineral standards for electron microprobe analysis of oxygen", Am. Mineral., 77, 1992, p Nielsen, C. H. and Sigurdsson, H., "Quantitative methods for electron microprobe analysis of sodium in natural and synthetic glasses", Am. Mineral., 66, p , 1981 J. L. Pouchou and F. M. A. Pichoir, "Determination of Mass Absorption Coefficients for Soft X- Rays by use of the Electron Microprobe" Microbeam Analysis, Ed. D. E. Newbury, San Francisco Press, 1988, p Press et al. (1986) "Numerical Recipes: The Art of Scientific Computing", Cambridge University Press, 818 pp. J. Ruste, J. Microsc. Spectrosc. Electron. 4, 123 (1979) Probe for Windows Reference and Guide v Introduction 4

11 V. D. Scott and G. Love, "Quantitative Electron-Probe Microanalysis", Wiley & Sons, New York, 1983 K. G. Snetsinger, T. E. Bunch and K. Keil, "Electron Microprobe Analysis of Vanadium in the Presence of Titanium", Am. Mineral., v. 53, (1968) p E. W. White and G. G. Johnson, "X-Ray Emission and Absorption Edge Wavelengths and Interchange Settings for LiF Geared Curved Crystal Spectrometers", Pennsylvania State University Special Publication No. 1-70, 2nd Edition, (1979) Comparison to PROBE for DOS A quick comparison between Probe for Windows and PROBE for DOS will reveal both the improvements and tradeoffs in porting PROBE to the Windows operating system. Floating Point Calculations Probe for Windows uses native Visual Basic for the ZAF and Phi-Rho-Z calculations, while PROBE for DOS uses 32 bit FORTRAN. A benchmark comparison reveals that Visual Basic is only 20 to 30% slower than FORTRAN. This difference is easily overcome by upgrading to a faster processor. Data File Access Probe for Windows utilizes the Microsoft Access "Jet" data access engine for storing and retrieving x-ray intensity data from disk using a relational database model. PROBE for DOS uses a FORTRAN fixed record proprietary binary file format. Although the relational database model is somewhat slower than the FORTRAN binary format, the relational model is extremely flexible for modification and allows the user to easily import x-ray intensity data using a variety of commercial database products such as Microsoft Access. User Interface The most apparent difference between the two products is in the user interface, Probe for Windows uses a menu driven, point-and-click interface compared to the command line prompt of PROBE for DOS. This results in a more intuitive interface, especially for new users. Experienced users will enjoy the enhanced capabilities and flexibility of Probe for Windows for acquisition and re-processing of x-ray intensities. Probe for Windows especially benefits from a large (17" or larger) monitor, which will allow several simultaneously open windows. For example, one may have the Acquire!, Analyze! and Automate! windows open at the same time that other Windows applications such as Micro-Image, Probe for Windows Reference and Guide v Introduction 5

12 are open. Because Probe for Windows retains window size and positions during your run, the user can customize the desktop for their specific needs and requirements. Disclaimer IN NO EVENT SHALL JOHN DONOVAN OR ADVANCED MICROBEAM BE LIABLE TO ANY PARTY FOR DIRECT, INDIRECT, SPECIAL, INCIDENTAL, OR CONSEQUENTIAL DAMAGES, INCLUDING LOST PROFITS, ARISING OUT OF THE USE OF THIS SOFTWARE AND ITS DOCUMENTATION, EVEN IF JOHN DONOVAN OR ADVANCED MICROBEAM HAS BEEN ADVISED OF THE POSSIBILITY OF SUCH DAMAGE. JOHN DONOVAN AND ADVANCED MICROBEAM SPECIFICALLY DISCLAIMS ANY WARRANTIES, INCLUDING, BUT NOT LIMITED TO, THE IMPLIED WARRANTIES OF MERCHANTABILITY AND FITNESS FOR A PARTICULAR PURPOSE. THE SOFTWARE PROVIDED HEREUNDER IS ON AN "AS IS" BASIS, AND JOHN DONOVAN AND ADVANCED MICROBEAM HAVE NO OBLIGATIONS TO PROVIDE MAINTENANCE, SUPPORT, UPDATES, ENHANCEMENTS, OR MODIFICATIONS. Probe for Windows Reference and Guide v Introduction 6