Silicate Sample Run
Introduction
This document illustrates step by step how to set up a new PROBE FOR WINDOWS quantitative run and how to analyze an unknown ten-element silicate sample. This documentation was produced on a three spectrometer JEOL 733 electron microprobe. Your particular run may look very different depending on the specific configuration of your microprobe. This document should be used in conjunction with the User’s Guide and Reference documentation, on-line help and the PFWUSERWIZARD program.
This run will demonstrate some of the powerful features of the PROBE FOR WINDOWS program. These include the use of pre-digitized standard mounts, automated spectrometer peaking, non-linear MAN (mean atomic number) background corrections, automated spectral interference corrections, automated standard acquisitions and digitizing unknown sample acquisitions.
Opening Probe For Windows
From the Desktop, double-click on the yellow PFW-E Software folder opening the EPMA Software group. Double click on the Probe for Windows … icon.
Upon launching PROBEWIN (PROBE FOR WINDOWS), the main log window appears along with the RealTimeInitInterface window as illustrated below. To collect real time data click the Yes button. The program can also be run off-line without the microprobe interface to re-process previously acquired data or on another computer.
This action causes the Confirm Motor and Crystal Positions dialog box to open. Confirm that all of the motors (stage and spectrometer positions) and crystal designations are correctly calibrated. If there is disagreement between the mechanical positions (actual) and the software values, adjust the software values. Use the <tab> key to move between the Stage and Spectrometer Positions text boxes.
Click the OK button after you have finished to close the Confirm Motor and Crystal Positions dialog box.
The main PROBE FOR WINDOWS log window is now visible as seen below.
Creating a New Run
To create a new sample run, select File from the menu bar and click New from the menu.
The Open New Probe Database File dialog box opens.
Change the Save in: location (directory) and type in an appropriate run name into the File name: text box.
The initial Save in: location is specified by the UserDataDirectory keyword in the PROBEWIN.INI file. File names longer than 8 characters are now supported.
The screen capture of the first window in this section indicates that other probe runs are already established. Any of the existing old runs maybe re-opened to acquire additional data or used as a “setup” file for starting a new run. In this example, a new file designated PYROXENE01.MDB will be created in the Kremser directory.
Close the Open New Probe Database File window by clicking the Save button. This action opens the File Information dialog box.
Enter the relevant information for the new run into the User, Title, and other Description text boxes. Use the <tab> key to move between text boxes. When finished, click the OK button.
This returns the program to the main PROBE FOR WINDOWS log window. Now the four main Probe buttons: Acquire!, Analyze!, Automate!, and Plot! become active.
Parameter Initialization
Analytical Standard Selection
Select the analytical standards to be used in the new probe run. From the main PROBE FOR WINDOWS log window click Standard from the menu bar and select Add/Remove Standards To/From Run from the menu.
This opens the Add Standards to Run dialog box.
All previously entered standards in the default standard database are accessible. Scroll through the Available Standards in Database list box to find the standards to be used in this run. Select both primary analytical standards and the MAN background standards. Some standards may be run as both. Select each and click the Add Standard To Run >> button to add each to the Current Standards in Run list box.
Click the OK button of the Add Standards to Run window when finished selecting standards. This returns the program to the main log window.
Creating a New Sample
Click the Acquire! button in the main PROBE FOR WINDOWS log window. This action opens the Acquire! dialog box. Note, not all buttons are active.
Click the New Sample button of the Acquire! dialog box.
This opens the New Sample dialog box.
Select Unknown from the New Sample Type buttons. Type an appropriate sample name and description into the New Sample Name and New Sample Description text boxes. This first sample will be used only to establish the analysis parameters.
Click the OK button of the New Sample dialog box.
The program returns to the Acquire! window. Notice that the first sample designated
Un 1 * template is now listed in the Current Sample text box. The * symbol indicates that no data has been collected for this sample yet.
Setting Analytical Conditions
Click the Analytical Conditions button to open the Analytical Conditions dialog box. Enter the appropriate numbers into the Kilovolts, Beam Current, and Beam Size text boxes for the currently Selected Sample. The Kilovolts, Beam Current, and Beam Size will need to be manually adjusted if a column digital interface is not present (all parameters other than kilovolts are simply available for documentation purposes only. If a hardware interface is supported, the user may specify a column condition string to indicate the desired analytical conditions of the instrument.
Click the OK button when done, returning to the Acquire! window.
Nominal Beam Current Measurement
The nominal beam current may be adjusted from the Count Times dialog box. Here, the nominal beam current is not the actual measured beam current but a close approximation that is used to calibrate the magnitude of the beam drift correction. If the nominal beam current is close to the actual measured beam current then the correction is close to 1.0 and the beam drift corrected counts displayed in the main log window will be close in magnitude to the counts displayed on the screen scalers. The nominal beam can be adjusted in several ways.
Open the Count Times window from the Acquire! button.
Any value desired may be directly entered into the Nominal Beam text box (30 nA value is stored in the PROBEWIN.INI file) or the user may measure the present beam current by clicking the Nominal Beam button.
The AcquireCheckNominal dialog box appears, choose the Yes button to measure the present beam current for use in the beam drift correction.
The current value of the faraday beam is measured and reported to both the Acquire! window and the Nominal Beam text box in the Count Times window as seen below.
Close the Count Times window by clicking the OK button.
Element, X-Ray Line, and Spectrometer Parameters Selection
Next, the user specifies the elements to be analyzed. Click the Elements/Cations button.
This action opens the Acquired and Specified Elements dialog box. Click on the first empty row under the Element column to enter the first element to analyze. The user may enter the analyzed elements in any order however, the analysis output will follow this order.
This opens the Element Properties dialog box. In the Element field either type in the first element to analyze or use the drop-down menu to select the element symbol. Certain default values listed in this window are based on parameters entered into the previously established configuration files.
Under the Enter Element Properties For: section (top of the Element Properties dialog box) choose the correct X-Ray Line, Cations, and Oxygens for the first element. Both alpha and beta lines are now supported as well as the ability of running the same element on all relevant spectrometers. Note: the Disable Acq and Disable Quant check boxes below the Delete button (see User’s Guide and Reference documentation for details).
There are two common methods for performing a background correction on wavelength dispersive x-ray data; off-peak backgrounds and MAN (mean atomic number) background corrections. The off-peak method entails measuring the background on each element in the sample of interest with the spectrometer adjusted to a position, typically on each side of the analytical peak. This method while somewhat time-consuming can accurately determine the background contribution for major, minor and trace element concentrations. Sophisticated modeling routines are available for precisely fitting backgrounds around analytical peaks (see User’s Guide and Reference documentation for details).
The MAN method relies on the fact that most of the background (continuum) production in the sample is directly proportional to the average atomic number of the sample. The MAN correction is an empirical calibration curve method involving the measurement of standards of known composition (hence average atomic number). If many samples are to be analyzed for their major and minor element concentrations then substantial time may be saved using the MAN method. However, if the user is required to measure high atomic number samples and/or trace concentrations, more accurate data may be obtained with off-peak background corrections.
Continue by selecting MAN
for the Background Type. Selecting MAN
deactivates the Off Peak Correction Type buttons
as well as the High and Low Off-Peak boxes. Next, click the text box under Spectrometer and enter the appropriate
spectrometer number that will be used to analyze the first element. Choosing a Spectrometer and
The next screen shows the edited Element Properties dialog box for silicon.
Click the OK button of the Element Properties dialog box to accept these element parameters for silicon.
The program returns to the Acquired and Specified Elements window with silicon now entered into the Element/Cations Parameters table.
Enter the next element in the run by clicking on the next
empty Element row of the Acquired and Specified Elements
window. This opens the Element Properties dialog box again.
Enter the appropriate Element,
Spectrometer,
Click the OK button of the Acquired and Specified Elements window when done entering elements in the run.
The GetElmLoadDefaultStds window opens to inform the user that standard assignments have been made based on the highest concentration of the element in the standard. The user will edit these choices shortly.
Click OK to return to the main Acquire! window.
Editing Acquisition Options
The user may change the element acquisition order of the spectrometers by clicking the Acquisition Options button in the Acquire! dialog box.
This opens the Acquisition Options dialog box.
To change the order that the spectrometer measures an element, select the User Defined Order Number button under Acquisition Order and click the row of the element to edit.
This opens the Acquisition Properties
dialog box, seen below. Here, the user
will re-define sodium (na) to be counted on the first spectrometer pass due to
its susceptibility to being volatilized by long exposure to the electron
beam. In samples containing volatile
elements the user may wish to consider running the volatile element calibration
routine (see User’s Guide and Reference documentation and/or Advanced Topics
manual).
Edit the Spectrometer Order Number for all elements to change the acquisition order. Further, the user wishes to use the same background correction method for both standards and unknowns, edit the Background Type for Standards to MAN for each element. Click the OK button returning to the Acquisition Options window. For spectrometer efficiency and element volatilization issues the user redefines the acquisition order as seen below.
Click the OK button of the Acquisition Options window to return to the Acquire! dialog box.
Modifying Standard Assignments
The standard assignments chosen by PROBE FOR WINDOWS may be inspected and edited by clicking the Analyze! button from the main log window.
The program automatically wraps element data output to eight elements per line. If the extended format menu is checked (activated from the Output menu) then the data is written out (in log window and to disk file, if enabled) as far as necessary to the right.
This opens the Analyze! dialog box.
Click the Standard Assignments button.
The Standard and Interference Assignments dialog box opens.
Click the row of the element that the user wishes to change the standard assignment for.
This opens the Assignment Properties dialog box. The default standard assignments are based on the highest concentration of the element in the standards currently in the run. In addition to standard assignments, the user may assign spectral interference corrections and volatile element calibrations from this window.
Click the Assigned Standard menu box. A scrollable list of all standards added to the current run are displayed. Select a new standard for element si.
Click the OK button returning to the Standard and Interference Assignments dialog box.
Repeat these editing steps until all necessary element standard assignments have been modified. In this example, the standard assignments for si, al, and mg are edited, resulting in the following window.
Click the OK button of the Standard and Interference Assignments dialog box returning to the Analyze! window.
Setting Count Times
Click the Count Times button of the Acquire! window.
This opens the Count Times dialog box. Here various parameters relating to counting times can be adjusted. Initially On-Peak count time is set for 10 seconds based on the configuration file defaults. Note: Real time spectrometer motion and acquisition time is graphically displayed.
To edit the count times for any element click that row in the spreadsheet. This opens the Count Time Properties dialog box.
Edit the Count Time text boxes with new times. To adjust the count times on unknowns, change the Unknown Count Time Factor. This is the multiplicity factor for acquiring unknown sample elements relative to the count times specified for the standards.
The Unknown Maximum Count text box is used to specify a statistics based count time. This feature is most useful if the user wishes to count for 30 seconds or 40000 counts whichever comes first. For samples with high count rate elements, the actual analysis time would be shorter.
Click the OK button of the Count Time Properties window.
Finally, click the OK button of the Count Times dialog box to accept any modified count times and return to the Acquire! window.
Loading Standard Position Files
To run analytical standards using automation, requires that the computer know
the physical location of all the standards for this run. Click the Automate! button from the main PROBE FOR WINDOWS log window.
This opens the Automate! dialog box shown below.
The last set of digitized standards used is visible in the Position List list box of the Automate! window. Currently, the standard block for the brass alloy run digitized previously are listed. These will be deleted and replaced by the appropriate standard position file(s).
Click the Delete All button. This opens the AutomateDeleteAll window. Click the Yes button of the AutomateDeleteAll window to clear the Position List list box of all displayed position samples.
The FiducialDeleteUnreferenced window opens. Click the Yes button to clear the fiducial coordinate set from the position database.
Click the Import from ASCII File (*.POS File) button of the Automate! dialog box to import position samples from a previously saved ASCII file.
This action opens the Open File To Import Position Data From window. The user has previously digitized all standard blocks and created STDPOS*.POS files. Three STDPOS*.POS files are typically loaded for silicate runs; STDPOS1_RECTA.POS, STDPOS2_TAYLOR.POS, and STDPOS3_RECTB.POS.
The default location for *.POS files is at C:\Program Files\Probe for Windows-E\Standard Image Files. Edit the Look in: text box if necessary.
Type in the appropriate file name in the File name: text box or simply highlight the file in the list and click the Open button.
This action opens the FiducialLoad window. Click the Yes button to do a fiducial transformation on this pre-digitized standard block to obtain an accurate set of standard positions.
The Modify Fiducial Positions window opens. Normally the user would simply accept the defaults or edit the position text boxes for each point, including the appropriate stage location number (JEOL 733 use appropriate W stage position). When done, click the OK button.
This action causes the stage motors to drive to the first fiducial coordinate in its lookup table. The FiducialVerifyFiducial window appears. Adjust the stage motors to center the first fiducial mark, click the OK button.
The computer will drive to each of the three fiducial marks for centering. Clicking the OK button after the third fiducial mark opens the FiducialsVerifyFiducials window. Click this OK button.
The program then imports and updates the position coordinates of all of the standards in the pre-digitized standard position file. The AutomateImportPositions window opens.
Click the OK button returning to the Automate! window.
The Automate! window would appear as below. The currently transformed standard position file is listed in the Position List list box.
Repeat the same loading procedure for the other two standard position files required for use in the automation. After clicking the Import from ASCII File button, the AutomateImportFile window opens.
Typically, when using more than one standard mount, the user would not delete all positions in the Position List, instead appending the additional position files to the first file. Select No and import additional standards.
All of the standards loaded are listed in the Position List list box of the Automate! window. These may now be accessed by the program during any automation action. For instance, it is now possible to have the computer drive to any standard located on the three blocks. The user may click the Move button of the Automate! window opening the Move Motors and Crystals dialog box. Then, click the Positions button.
This opens the Position Database dialog box. From here, any sample that has been digitized may be located by simply selecting it and clicking the Go button.
Once the stage motors drive the stage to the chosen standard, exit the Position Database by clicking the Close button. Likewise, the user may close the Move Motors and Crystals window by clicking its Close button, returning to the Automate! window.
Note: Double clicking from any position list will also drive the stage, highlight the row number of interest and double click.
This concludes the initial parameter setup portion of PROBE FOR WINDOWS.
Automation Actions
Confirm Standard Positions
All of the basic peak centering and x-ray count acquisition procedures may be automated. This is accomplished via the Automate! window.
Click the Select Stds button of the Automate! dialog box. All standards that have been added to the current run will now be highlighted in the Position List list box.
The user might start by checking the location and focus of each standard selected for the automated analysis. Click the box for Confirm Standard Positions under Automation Actions. Click the Run Selected Samples button.
The AutomateConfirmSelected window opens informing the user that thirteen standards were chosen and asks if you want to run these automated samples, click Yes.
The program then sends the stage motors to the fiducial transformed coordinates for the first selected standard and opens the Confirm Positions window. Clicking the two-way Pause/Continue button suspends the 10 second countdown (user defined in the PROBEWIN.INI file). Adjust the stage motors (X, Y, and Z) to a new, clean analysis position. Click the OK button of the Confirm Positions window when done, sending the stage to the next standard to confirm its position. Again, the Confirm Positions window opens, allowing the user to pause the countdown and adjust the sample position.
After the final standard is confirmed, the AcquireStop window appears. In this example standards on several standard blocks are located and confirmed. Click this OK button returning to the Automate! dialog box.
Calibrate Peak Positions
X-ray peaking may be automated from the Automate! window as follows.
The Select Stds
button from the previous step highlighted all of the standards added to the
current run. Presently the Position List list box in the Automate! window contains both the
analytical and MAN background standards for the current run. Since x-ray peak centering is only done on
the primary analytical standards, either re-select the primary analytical
standards or de-select the additional MAN background standards from the Position List list box. Under Automation
Actions click only the Peak
Spectrometers box. Under Automation Options click the Peak on Assigned Standards and Use
Confirm During Acquisition boxes.
Finally, click the Peaking
button to open the
In the
Click the Run Selected Samples button from the Automate! window.
The AutomateSave window opens, asking if you want to do a PRE-scan on each element.
The user selects Yes to do a PRE-scan.
This opens the AutomateConfirmSelected window. To run these automated samples, click Yes.
The stage motors move to the position coordinates of the first standard highlighted in the Position List list box and the Confirm Positions window opens. This window allows the user to readjust if necessary the stage motors (X, Y, and Z) to a new, clean analysis position. Click the OK button of the Confirm Positions window when done and the spectrometers go through the peaking routine to peak center the spectrometer position to the x-ray maximum for all the elements assigned to that standard. After finding a new peak position and reporting the results to the main log window, the stage motors move on to the coordinates of the next standard highlighted in the Position List list box. Once situated on this standard, the spectrometers peak center those elements assigned to it. This procedure continues until all standards are done. When all automation action is complete, the AcquireStop window appears and requests the user to click the OK button.
The following summary of the peak center automation for the primary standards is found in the main log window.
All elements were peak centered using the Parabolic fit method. The new peak locations (OnPeak) along with the start and stop intensities in counts per second and
peak-to-backgrounds are listed. The final on-peak intensities (StopI) are valuable for adjusting count time parameters for your standardizations to improve statistics.
Acquire Standard Samples
The next step is to calibrate the analytical and MAN background standards in preparation for unknown samples. The user may choose to run both types of standards together or separate them. In the latter case, the MAN background standards would normally be acquired first since backgrounds drift less than peak intensities.
Here, the user will automate the entire acquisition of x-ray counts on all standards. Click the Select Stds button in the Automate! dialog box. This selects all current standards in the run, highlighting them in the Position List list box. Next, under Automation Actions, click only on the Acquire Standard Samples box. From the Automation Options choices select the number of Standard Points To Acquire and whether to Use Confirm During Acquisition. In this example, four standard points are chosen along with a Standard X Increment of 10 um. Finally, click the Run Selected Samples button.
The familiar AutomateConfirmSelected window opens again, informing the user that thirteen standards are chosen and asks if you want to run these automated samples, click Yes.
The stage moves to the coordinates of the first highlighted standard in the Position List list box. If the Use Confirm During Acquisition box is checked then the Confirm Positions window will open. A complete analysis is acquired on all elements in the current sample, x-rays are counted on peak only for times specified in the Count Times window. Progress of the acquisition can be followed from within the Acquire! Window (far right).
Finally, the Faraday cup is measured. The stage jogs 10 um in the X direction and this procedure is repeated for the number of points specified in the Standard Points To Acquire text box of the Automate! dialog box. After completing data collection on the first standard, the stage travels to the next highlighted standard in the list box and acquires four complete analyses on that standard. This procedure is repeated for all selected standards. After finishing the automation schedule the AcquireStop window opens and requires the user to click the OK button thereby returning to the Automate! window.
The following log window illustrates typical on-peak x-ray count data (in cps) for the Taylor Quartz standard.
In addition to the four individual lines of count data, the AVER, SDEV, 1SIG, SERR, and %RSD are calculated. The AVER (average) is the average intensity reading of each element column. The SDEV (standard deviation) is the range of these results, 1SIG (one sigma) is the predicted standard deviation, and the SERR (standard error) is essentially the precision of the average. The %RSD number is the SDEV divided by the AVER times 100. See the User’s Guide and Reference documentation for exact equations. The output of the raw data counts for the remaining twelve standards are not shown here to save space.
Evaluate Standard Count Data
After all the standard data is acquired it is useful to examine the raw on-peak counts to check for and delete any obviously bad data points. Click the Analyze! button in the main PROBE FOR WINDOWS log window.
This opens the Analyze! dialog box.
The Sample List list box contains the list of the standards that data has been acquired on. To examine the raw count data acquired on any standard run under automation, first select the standard of interest and click the Data button.
The raw count data for the four automated standard analyses
of the SiO2 Quartz Taylor standard are shown below. Each individual line (49 G to 52 G) is
illustrated along with the Average, Std Dev, OneSigma, Std Err, %
Examine the raw count data for each standard. If more than one sample/standard is selected for analysis, select the Pause Between Samples check box. When this box is checked, the program will automatically pause after displaying each analysis until the user clicks the Cancel or Next (red flashing) buttons on that are located at the bottom of the log window. If there are any bad data points, use the Delete Selected Line(s) button to flag a line of data as bad. In the SiO2 Quartz Taylor standard, seen below, line 52 G (good) is deemed a bad data point since its cps value is low compared to the other three lines. Click on the line number, highlighting the line. Next click the Delete Selected Line(s) button.
This opens the SampleDeleteLines window.
Click the Yes button. The computer will flag this line with a B (bad) and ignore this data for any subsequent calculations.
Click the Data button again to re-analyze the remaining data lines for statistical parameters. Remember one can always undelete data lines with the Undelete Selected Line(s) button.
At this point, the user has collected all standardization data and is ready to make MAN background assignments.
Assign MAN Background Calibrations
From the main PROBE FOR WINDOWS log window, select Analytical from the menu bar and click Assign MAN Fits from the menu choices.
This opens the MANLoadNewElements window.
Click the OK button.
This opens the MAN Assignment and Fit dialog box. The second element, aluminum (al) in the list is shown below.
From this dialog box, the user may display and modify the MAN background assignments and fits used for the background correction of all elements in the current run. The advantage of this method is that it requires only a simple calibration of the analyzing channel over a range of atomic number. Substantial time may be saved when many samples are to be analyzed. However, if measuring high atomic number samples and/or trace concentrations, the off-peak background correction technique is usually superior.
For each element, select standards from the Standards list box that do not contain the element itself. In this way the measured background counts can be plotted as a function of the average atomic number (Z-bar). Choose at least five standards per element and compute a second-order polynomial or force a straight line fit (if deemed appropriate) between background counts and MAN for each. For further details and suggestions, see the User’s Guide and Reference documentation. Several fits (sodium, iron, and vanadium) are illustrated respectively, below.
The vanadium plot above illustrates another effect in WDS analysis; spectral
interferences. The well-known transition
metal interferences are easily visible in these types of plots. The Kb x-ray line for the
element of atomic number x interfers with the Ka x-ray line of element x+1
(Ti with V, V with Cr, Cr with Mn and Mn with Fe). Above, standard 212 is pure
TiO2 with no V2O3 but an apparent vanadium
x-ray signal is seen.
The 212 standard is removed and the MAN background fit updated by clicking the Update Fit button. All of these interferences will be examined shortly.
When done adjusting individual elements, click the OK button to store the updated MAN background corrections.
Analyze Standard Samples
The user will now analyze all of the standard data re-calculating the x-ray counts to compositions in oxide weight percent. Since the program treats all samples as unknowns, the results of the standards provide a valuable check on the quality of the analysis.
Click the Analyze button in the main PROBE FOR WINDOWS log window. This opens the Analyze! dialog box.
Under Sample List select the All Samples button. Click the Select All button highlighting all standards.
Click the Calculation Options button in the Analyze! window.
This action opens the Calculation Options dialog box. Under Calculations Options click the Display Results As Oxides and the radio button Calculate with Stoichiometric Oxygen. Elemental results are always calculated and output to the log window.
Click the OK button to output data in oxide form.
Analyzing all of the data on the standards will create a large amount of output, possibly overflowing the log window buffer, depending on the value specified in the LogWindowBufferSize parameter in the PROBEWIN.INI file. The size of the log window buffer is limited only by the amount of memory available. Setting this parameter to 512000 bytes is roughly equivalent to 300 pages of average density text. In some cases saving all log window output to a user specified text file for viewing with a text editor or printing to a laser printer may be best.
Select Output from the menu bar in the main log window and click Save to Disk Log.
This opens the Open File To Output Probe Data To dialog box. The Save in: location will be the directory specified for the original file name (PYROXENE01.MDB). All subsequent files created by the user will use this location. Edit the File name if desired. The default output file has the extension .OUT. Note that the raw data is always saved in the .MDB run file for future re-calculation and /or output. Click Save when finished.
Select the Analyze! button in the main PROBE FOR WINDOWS log window, to bring forward the Analyze! dialog box. Click the Select All button highlighting all standards again. Then click the Analyze button. This will analyze all selected standard data into the specified text file.
To view this data return to the main PROBE FOR WINDOWS log window and select Output from the menu bar again and click View Disk Log from the menu.
This opens the file editor. This example utilizes the Programmer’s File Editor, seen below. A number of text file viewers may be used. To utilize a specific editor such as Textpad or Word, edit the FileViewer keyword in the PROBEWIN.INI file.
The user may now scroll through the analyzed standards using the text editor or may direct the file data to a laser printer by selecting File from the Programmer’s File Editor menu bar and clicking on Print in the drop-down menu.
Since all elements were acquired on all standards, examination of the oxide weight percents will provide a check on the quality of the calibration. Several of the standard compositions will be displayed. The first example is the Orthopyroxene standard displayed in the Analyze! window below. This is the primary standard for magnesium and silicon. The average values for both elements show excellent agreement with the published standard database values.
The analysis of the Rutile standard reveals several interesting points; 1) the TiO2 concentration is close to the published value of 99.26 and 2) an apparent 1.6 weight percent concentration of V2O3 is found! This sample has no vanadium, here the user sees the notorious Ti-V spectral interference. This interference overestimates the amount of V2O3 in the sample resulting in the total exceeding 100%. This will be corrected for (shortly) using the automatic interference correction routine.
All of the data lines gathered on the standards are examined and appear close to their standard database values. To save space they will not be reproduced here.
Spectral Interference Assignments
PROBE FOR WINDOWS allows the user to select a fully quantitative correction for spectral interferences. The program can only correct for interferences if both the interfered and interfering elements are analyzed for. Further, data for an interference calibration standard must be acquired that contains a major concentration of the interfering element and none of the interfered element or any other elements that interfere with the interfered element.
Select the Standards button in the Sample List and click the Select All button in the Analyze! window. Next, click the Standard Assignments button.
Clicking this button opens the Standard and Interference Assignments dialog box.
Click on the element row to edit the Interference Assignments.
The Assignment Properties dialog box opens. Select the first interference element for this element and the corresponding standard that contains a known amount of the interfering element but none of the interfered element.
Click the OK button when finished.
The Standard and Interference Assignments window will appear as below.
Repeat these editing steps for all of the other element interferences, resulting in the following Standard and Interference Assignments window.
Click the OK button when finished returning to the Analyze! window.
Next, the user might check the analysis options that are currently assigned. From the main PROBE FOR WINDOWS log window, select Analytical from the menu bar and click Analysis Options from the menu choices.
This opens the Analysis Calculation Options window. Check that the appropriate boxes are marked.
Click the OK button returning to the main log window.
The user then reanalyzes the standards (Analyze button in the Analyze! window), utilizing the spectral interference correction routine. The results for the Rutile standard are dramatic; the apparent 1.6 wt% V2O3 concentration has been replaced with an average 0.02 wt% content (which is below the detection limit).
The user is ready to move on to unknown samples.
Unknown Sample Data Collection and Analysis
To collect x-ray data on an unknown sample, minimize the Analyze! window and/or bring forward the Acquire! dialog box to start a new sample.
Click the Move button on the Acquire! window to drive the stage to the coordinates of the first unknown sample.
Click the New Sample button to activate the New Sample dialog box. Check that the Unknown button under New Sample Type is marked. Enter an appropriate sample name and description into the New Sample Name and New Sample Description text boxes. Finally, click the OK button.
To start acquiring x-ray counts on the first unknown sample, simply click the Start Standard or Unknown Acquisition button of the Acquire! window.
Pyroxene #164, a chromium augite, is run once to obtain representative count rate information for the adjustment of element count times using the Count Times button to improve statistics and lower detection limits.
The Unknown Count Time Factor (Factor) in the Count Times window may be modified. This factor is a simple multiplication of the default count times (peak and backgrounds) on the standards. Further, the graphical spectrometer motion and acquisition time bars indicate the total time for an analysis and how efficient your usage of the spectrometers are. Here, a fourth spectrometer with an LIF crystal would substantially shorten the analytical time.
Four random spots are then acquired (a New Sample is started) on the same pyroxene.
The Start Standard or Unknown Acquisition button in the Acquire! window is clicked four times, to acquire four data points with improved count times.
Next, the Analyze! dialog box is reopened or simply brought forward. Click the Unknowns button and select Un 3 Pyroxene #164.
Click the Calculation Options button.
This opens the Calculation Options dialog box.
Make the following changes; under Calculations Options check Display Results as Oxides, Calculate Detection Limits and Homogeneity, and Calculate with Stoichiometric Oxygen. Under Formula and Mineral Calculations check the Calculate Formula Based On box. Select Pyroxene and enter 6 Atoms of Oxygen in the other two text boxes.
Click the OK button closing the Calculation Options window, returning to the Analyze! dialog box.
Clicking the Analyze button calculated the results for these four points and those values are viewed below, as copied from the text editor.
Un 3 Pyroxene #164
TakeOff
= 40.0 KiloVolt = 15.0 Beam Current = 40.0 Beam Size =
10
(Magnification
= 2000.) Beam Mode = Analog Spot
Four
random spots
Number
of Data Lines: 4 Number of 'Good' Data
Lines: 4
First/Last
Date-Time: 09/23/2006 11:44:50 PM to 09/24/2006 12:03:54 AM
Average Total
Oxygen: 43.823 Average Total Weight%: 99.294
Average
Calculated Oxygen: 43.823 Average Atomic Number: 12.365
Average
Excess Oxygen: .000 Average Atomic Weight: 21.725
Average ZAF
Iteration: 3.00 Average Quant Iterate: 4.00
Oxygen
Calculated by Cation Stoichiometry and Included in the Matrix Correction
Results in
Elemental Weight Percents
SPEC: O
TYPE: CALC
AVER: 43.823
SDEV: .172
ELEM: Si
Al Ti V
Cr Fe Mn
Mg Ca Na
BGDS: MAN
MAN MAN MAN
MAN MAN MAN
MAN MAN MAN
ABS%: -20.88
-28.35 -3.13 -2.04
-1.42 -.52 -.82
-32.24 -3.22 -46.88
TIME: 20.00
20.00 30.00 30.00
30.00 30.00 30.00
40.00 40.00 30.00
ELEM: Si
Al Ti V
Cr Fe Mn
Mg Ca Na
SUM
54
23.298 3.942 .309
.015 .584 3.667
.115 10.410 12.302
.617 98.857
55
23.521 3.901 .290
.011 .597 3.675
.124 10.488 12.355
.647 99.504
56
23.637 3.908 .317
.022 .567 3.695
.105 10.480
12.286 .632 99.651
57
23.520 3.895 .266
.024 .620 3.549
.127 10.465 12.273
.626 99.165
AVER: 23.494
3.912 .296 .018
.592 3.647 .118
10.461 12.304 .630
99.294
SDEV: .142
.021 .022 .006
.022 .066 .010
.035 .036 .013
SERR: .071
.010 .011 .003
.011 .033 .005
.017 .018 .006
%RSD: .6
.5 7.6 32.8
3.8 1.8 8.5
.3 .3 2.0
STDS: 206
207 212 211
224 203 205
206 210 81
STKF: .2112
.2706 .5519 .5083
.6408 .4982 .4894
.1774 .3205 .0500
STCT: 4597.1 20306.5 917.8
1665.7 2830.4 3132.6
2529.2 10126.2 10692.2 1635.7
UNKF: .1834
.0273 .0025 .0002
.0050 .0306 .0010
.0707 .1132 .0033
UNCT: 3992.1
2045.4 4.1 .5
22.2 192.5 5.0
4039.4 3777.3 106.9
UNBG: 12.8
30.0 1.1 2.2
3.5 6.9 3.8
18.7 32.2 8.6
ZCOR: 1.2810
1.4351 1.1938 1.2087
1.1797 1.1910 1.2113
1.4786 1.0867 1.9308
KRAW: .8684
.1007 .0045 .0003
.0078 .0615 .0020
.3989 .3533 .0654
PKBG: 312.32
69.09 4.80 1.23
7.27 29.06 2.31
217.21 118.38 13.42
INT%: .00
.00 .00 .00
.00 .00 .00
.00 .00 .00
Results in
Oxide Weight Percents
SPEC: O
TYPE: CALC
AVER: .000
SDEV: .000
ELEM: SiO2
Al2O3 TiO2 V2O3
Cr2O3 FeO MnO
MgO CaO Na2O
SUM
54
49.844 7.448 .516
.022 .853 4.718
.148 17.264 17.213
.831 98.857
55
50.319 7.372 .484
.017 .873 4.727
.160 17.392 17.287
.872 99.504
56
50.568 7.383 .528
.033 .829 4.754
.135 17.378 17.191
.851 99.651
57
50.318 7.360 .444
.035 .906 4.566
.164 17.354 17.172
.844 99.165
AVER: 50.262
7.391 .493 .027
.865 4.691 .152
17.347 17.216 .850
99.294
SDEV: .303
.040 .037
.009 .033 .085
.013 .058 .050
.017
SERR: .151
.020 .019 .004
.016 .042 .006
.029 .025 .009
%RSD: .6
.5 7.6 32.8
3.8 1.8 8.5
.3 .3 2.0
Results Based
on 6 Atoms of o
SPEC: O
TYPE: CALC
AVER: 6.000
SDEV: .000
ELEM: Si
Al Ti V
Cr Fe Mn
Mg Ca Na
SUM
54
1.827 .322 .014
.001 .025 .145
.005 .943 .676
.059 10.015
55
1.832 .316 .013
.000 .025 .144
.005 .944 .674
.062 10.015
56
1.836 .316 .014
.001 .024 .144
.004 .941 .669
.060 10.009
57
1.836 .316 .012
.001 .026 .139
.005 .944 .671
.060 10.010
AVER: 1.832
.318 .014 .001
.025 .143 .005
.943 .673 .060
10.012
SDEV: .004
.003 .001 .000
.001 .003 .000
.001 .003 .001
SERR: .002
.001 .001 .000
.000 .001 .000
.001 .002 .001
%RSD: .2
.9 7.6 32.7
3.9 1.8 8.6
.2 .5 1.8
Pyroxene
Mineral End-Member Calculations
Wo En
Fs
54
38.3 53.5 8.2
55
38.3 53.6 8.2
56
38.1 53.6 8.2
57
38.3 53.8 7.9
AVER: 38.2
53.6 8.1
SDEV: .1
.1 .1
Detection
limit at 99 % Confidence in Elemental Weight Percent (Single Line):
ELEM: Si
Al Ti V
Cr Fe Mn
Mg Ca Na
54
.014 .007 .041
.030 .028 .027
.025 .005 .009
.009
55
.014 .007 .041
.030 .028 .027
.025 .005 .009
.009
56
.014 .007 .041
.030 .028 .027
.025 .005 .009
.009
57
.014 .007 .041
.030 .028 .027
.025 .005 .009
.009
AVER: .014
.007 .041 .030
.028 .027 .025
.005 .009 .009
SDEV: .000
.000 .000 .000
.000 .000 .000
.000 .000 .000
SERR: .000
.000 .000 .000
.000 .000 .000
.000 .000 .000
Percent
Analytical Error (Single Line):
ELEM: Si
Al Ti V
Cr Fe Mn
Mg Ca Na
54
.4 .5 10.8
97.5 4.5 1.4
13.2 .3 .3
1.9
55
.4 .5 11.2
127.2 4.4 1.4
12.4 .2 .3
1.9
56
.4 .5 10.6
66.4 4.6 1.4
14.2 .2 .3
1.9
57
.4 .5 11.9
62.9 4.3 1.4
12.2 .2 .3
1.9
AVER: .4
.5 11.1 88.5
4.5 1.4 13.0
.2 .3 1.9
SDEV: .0
.0 .6 30.1
.1 .0
.9 .0 .0
.0
SERR: .0
.0 .3 15.1
.1 .0 .5
.0 .0 .0
ELEM: Si
Al Ti V
Cr Fe Mn
Mg Ca Na
60ci
.072 .010 .009
.001 .009 .031
.003 .017 .018
.006
80ci
.121 .017 .015
.001 .016 .052
.005 .029 .030
.010
90ci
.173 .024 .021
.001 .023 .075
.007 .042 .044
.014
95ci
.235 .032 .028
.002 .031 .102
.009 .056 .059
.019
99ci
.430 .059 .052
.003 .056 .187
.017 .103 .108
.035
Test of
Homogeneity at 1.0 % Precision (Average of Sample):
ELEM: Si
Al Ti V
Cr Fe Mn
Mg Ca Na
60ci
yes yes no
no no yes
no yes yes
yes
80ci
yes yes no
no no no
no yes
yes no
90ci
yes yes no
no no no
no yes yes
no
95ci
yes yes no
no no no
no yes yes
no
99ci
no no no
no no no
no yes yes
no
Level of
Homogeneity in +/- Percent (Average of Sample):
ELEM: Si
Al Ti V
Cr Fe Mn
Mg Ca Na
60ci
.3 .3 2.9
3.0 1.6 .9
2.4 .2 .1
.9
80ci
.5 .4 4.9
4.9 2.7 1.4
3.9 .3 .2
1.5
90ci
.7 .6 7.1
7.1 3.8 2.1
5.7 .4 .4
2.2
95ci
1.0 .8 9.5
9.6 5.2 2.8
7.7 .5 .5
3.0
99ci
1.8 1.5 17.5
17.7 9.5 5.1
14.1 1.0 .9
5.5
Detection
Limit in Elemental Weight Percent (Average of Sample):
ELEM: Si
Al Ti V
Cr Fe Mn
Mg Ca Na
60ci
--- --- .014
.004 .014 ---
.006 --- ---
.008
80ci
--- --- .023
.006 .023 ---
.011 --- ---
.013
90ci
--- --- .034
.009 .033 ---
.015 --- ---
.019
95ci
--- --- .046
.012 .045 ---
.020 --- ---
.026
99ci
--- --- .084
.022 .083 ---
.038 --- ---
.048
Projected
Detection Limits (99% CI) in Elemental Weight Percent (Average of Sample):
ELEM: Si
Al Ti V
Cr Fe Mn
Mg Ca Na
TIME: .31
.31 .47 .47
.47 .47 .47
.63 .63 .47
PROJ: ---
--- .670 .178
.665 --- .301
--- --- .382
TIME: .63
.63 .94 .94
.94 .94 .94
1.25 1.25 .94
PROJ: ---
--- .474 .126
.470 --- .213
--- --- .270
TIME: 1.25
1.25 1.88 1.88
1.88 1.88 1.88
2.50 2.50
1.88
PROJ: ---
--- .335 .089
.332 --- .150
--- --- .191
TIME: 2.50
2.50 3.75 3.75
3.75 3.75 3.75
5.00 5.00 3.75
PROJ: ---
--- .237 .063
.235 --- .106
--- --- .135
TIME: 5.00
5.00 7.50 7.50
7.50 7.50 7.50
10.00 10.00 7.50
PROJ: ---
--- .168 .044
.166 --- .075
--- --- .096
TIME: 10.00
10.00 15.00 15.00
15.00 15.00 15.00
20.00 20.00 15.00
PROJ: ---
--- .118 .031
.118 --- .053
--- --- .068
TIME: 20.00
20.00 30.00 30.00
30.00 30.00 30.00
40.00 40.00 30.00
PROJ: ---
--- .084 .022
.083 ---
.038 --- ---
.048
TIME: 40.00
40.00 60.00 60.00
60.00 60.00 60.00
80.00 80.00 60.00
PROJ: ---
--- .059 .016
.059 --- .027
--- --- .034
TIME: 80.00
80.00 120.00 120.00
120.00 120.00 120.00
160.00 160.00 120.00
PROJ: ---
--- .042 .011
.042 --- .019
--- --- .024
TIME: 160.00
160.00 240.00 240.00
240.00 240.00 240.00
320.00 320.00 240.00
PROJ: ---
--- .030 .008
.029 ---
.013 --- ---
.017
TIME: 320.00
320.00 480.00 480.00
480.00 480.00 480.00
640.00 640.00 480.00
PROJ: ---
--- .021 .006
.021 --- .009
--- --- .012
TIME: 640.00
640.00 960.00 960.00
960.00 960.00 960.00 1280.00 1280.00 960.00
PROJ: ---
--- .015 .004
.015 --- .007
--- --- .008
TIME: 1280.00 1280.00 1920.00 1920.00 1920.00
1920.00 1920.00 2560.00 2560.00 1920.00
PROJ: ---
--- .010 .003
.010 --- .005
--- --- .006
Analytical
Sensitivity in Elemental Weight Percent (Average of Sample):
ELEM: Si
Al Ti V
Cr Fe Mn
Mg Ca Na
60ci
.102 .014 .012
.001 .013 .044
.004 .025 .026
.008
80ci
.171 .023 .021
.001 .022 .074
.007 .041 .043
.014
90ci
.245 .034 .030
.002 .032 .107
.009 .059 .062
.020
95ci
.332 .045 .040
.002 .043
.144 .013 .080
.083 .027
99ci
.609 .083 .073
.005 .079 .264
.023 .146 .153
.049
The user may obtain a large amount of information besides elemental and oxide weight percent data; these expanded capabilities include formula and mineral end member calculations, an extended set of detection limit and statistics including homogeneity and analytical sensitivity. See the User’s Guide and Reference documentation for calculation details.
Digitized Sample Data Collection and Analysis
Next the user will perform a digitized traverse across an unknown pyroxene grain. The user can digitize standards, unknowns or wavescan positions based on random points, linear traverse or rectangular or polygon gridded areas. Check that the Unknowns button is clicked in the Automate! window.
Click the Digitize button in the Automate! window.
This opens the Digitize Sample Positions dialog box.
To create an unknown digitized sample click Unknown under Sample Type and enter a sample name in the Unknown or Wavescan Position Samples text box. Next, click the Create New Unknown or Wavescan button. The unknown sample will now appear in the Position List list box of the Automate! window.
Finally, click the Linear Traverse button to create a traverse of digitized points. Other options are rectangular and polygon grids as well as digitize clusters of random points.
The Linear Traverse Parameters dialog box opens.
Move to the start position of the linear traverse, and click the Update Start button. Move to the stop position and click the Update Stop button. The total distance is displayed.
Select the Use Number of Points Per Traverse or Use Step Size in Microns Per Step radio button and adjust the text boxes appropriately.
Click the OK button returning to the Automate! window.
Now all of the calculated analysis positions have been digitized and listed. Under Automation Actions click the Acquire Unknown Samples button.
Click Run Selected Samples button to initiate the traverse.
The AutomateConfirmSelected window opens, click Yes.
When the traverse is completed the familiar AcquireStop window appears.
Click the OK button returning the user to the Automate! dialog box.
To analyze the data obtained from the traverse, the user opens the Analyze! window and selects the Un 4 Pyroxene Traverse unknown sample in the Sample List.
Again, save the log window output to the text editor. Click the Analyze button to calculate compositions and finally view the disk log in the text editor. A portion is shown below.
Un 4 Pyroxene Traverse
TakeOff
= 40.0 KiloVolt = 15.0 Beam Current = 40.0 Beam Size =
10
(Magnification
= 2000.) Beam Mode = Analog Spot
Number
of Data Lines: 10 Number of
'Good' Data Lines: 10
First/Last
Date-Time: 09/24/2006 12:16:49 AM to 09/24/2006 12:50:11 AM
Average Total
Oxygen: 43.864 Average Total Weight%: 99.347
Average
Calculated Oxygen: 43.864 Average Atomic Number: 12.362
Average
Excess Oxygen: .000 Average Atomic Weight: 21.721
Average ZAF
Iteration: 3.00 Average Quant Iterate: 3.90
Oxygen
Calculated by Cation Stoichiometry and Included in the Matrix Correction
Results in
Elemental Weight Percents
SPEC: O
TYPE: CALC
AVER: 43.864
SDEV: .186
ELEM: Si
Al Ti V
Cr Fe Mn
Mg Ca Na
BGDS: MAN
MAN MAN MAN
MAN MAN MAN
MAN MAN MAN
ABS%: -20.86
-28.33 -3.13 -2.04
-1.42 -.52 -.82
-32.23 -3.22 -46.87
TIME: 20.00
20.00 30.00 30.00
30.00 30.00 30.00
40.00 40.00 30.00
ELEM: Si
Al Ti V
Cr Fe Mn
Mg Ca
Na SUM
58
23.592 3.885 .278
.032 .581 3.656
.133 10.432 12.290
.645 99.412
59
23.527 3.844 .345
.016 .577 3.666
.125 10.405 12.209
.638 99.115
60
23.579 3.894 .343
.029 .597 3.731
.133 10.398 12.226
.635 99.465
61
23.437 3.893 .248
.031 .544 3.558
.120 10.457 12.365
.631 98.975
62
23.282 3.861 .314
.004 .571 3.639
.120 10.437 12.221
.634 98.569
63
23.631 3.916 .309
.031 .579 3.632
.141 10.496 12.309
.642 99.710
64
23.641 3.888 .288
.019 .545 3.648
.100 10.402 12.261
.643 99.322
65
23.670 3.889 .336
.030 .581 3.652
.145 10.473 12.240
.631 99.667
66
23.701 3.923 .360
.034 .534 3.649
.110 10.519 12.298
.659 99.924
67
23.535 3.894 .290
.050 .548 3.619
.095 10.465 12.334
.634 99.310
AVER: 23.559
3.889 .311 .028
.566 3.645 .122
10.448 12.275 .639
99.347
SDEV: .124
.023 .035 .012
.021 .043 .017
.041 .052 .008
SERR: .039
.007 .011 .004
.007 .014 .005
.013 .017 .003
%RSD: .5
.6 11.4 44.1
3.7 1.2 13.6
.4 .4 1.3
STDS: 206
207 212 211
224 203 205
206 210 81
STKF: .2112
.2706 .5519 .5083
.6408 .4982 .4894
.1774 .3205 .0500
STCT: 4597.1 20306.5 917.8 1665.7
2830.4 3132.6 2529.2 10126.2 10692.2 1635.7
UNKF: .1840
.0271 .0026 .0002
.0048 .0306 .0010
.0707 .1130 .0033
UNCT: 4004.4
2033.9 4.3 .7
21.2 192.5 5.2
4034.7 3768.2 108.4
UNBG: 12.8
30.0 1.1
2.2 3.5 6.9
3.8 18.7 32.2
8.6
ZCOR: 1.2806
1.4349 1.1938 1.2087
1.1797 1.1910 1.2114
1.4786 1.0867 1.9305
KRAW: .8711
.1002 .0047 .0004
.0075 .0614 .0021
.3984 .3524 .0663
PKBG: 313.41
68.70 4.99 1.35
6.99 29.05 2.36
216.96 118.13 13.60
INT%: .00
.00 .00 .00
.00 .00 .00
.00 .00 .00
Results in
Oxide Weight Percents
SPEC: O
TYPE: CALC
AVER: .000
SDEV: .000
ELEM: SiO2
Al2O3 TiO2 V2O3
Cr2O3 FeO MnO
MgO CaO Na2O
SUM
58
50.471 7.340 .464
.047 .850 4.704
.172 17.299 17.196
.869 99.412
59
50.332 7.262 .576
.024 .844 4.717
.162 17.255 17.083
.860 99.115
60
50.443 7.357 .572
.042 .873 4.800
.172 17.243 17.106
.856 99.465
61
50.140 7.357 .413
.046 .795 4.577
.155 17.342 17.301
.851 98.975
62
49.809 7.296 .524
.006 .834
4.681 .156 17.308
17.100 .855 98.569
63
50.556 7.400 .516
.046 .846 4.672
.182 17.405 17.222
.865 99.710
64
50.576 7.346 .480
.028 .797 4.694
.129 17.249 17.155
.867 99.322
65
50.638 7.349 .560
.044 .850 4.698
.187 17.367 17.126
.850 99.667
66
50.704 7.413 .600
.049 .781 4.695
.142 17.444 17.208
.888 99.924
67
50.350 7.358 .484
.073 .801 4.656
.122 17.354 17.257
.854 99.310
AVER: 50.402
7.348 .519 .041
.827 4.689 .158
17.327 17.175 .861
99.347
SDEV: .266
.044 .059 .018
.031 .055 .021
.068 .073 .011
SERR: .084
.014 .019 .006
.010 .017 .007
.022 .023 .004
%RSD: .5
.6 11.4 44.1
3.7 1.2 13.6
.4 .4 1.3
Results Based
on 6 Atoms of o
SPEC: O
TYPE: CALC
AVER: 6.000
SDEV: .000
ELEM: Si
Al Ti V
Cr Fe
Mn Mg Ca
Na SUM
58
1.837 .315 .013
.001 .024 .143
.005 .939 .671
.061 10.010
59
1.838 .312 .016
.001 .024 .144
.005 .939 .668
.061 10.008
60
1.836 .316 .016
.001 .025 .146
.005 .936 .667
.060 10.008
61
1.834 .317 .011
.001 .023 .140
.005 .945 .678
.060 10.015
62
1.830 .316 .014
.000 .024 .144
.005 .948 .673
.061 10.016
63
1.835 .316 .014
.001 .024 .142
.006 .942 .670
.061 10.011
64
1.841 .315 .013
.001 .023 .143
.004 .936 .669
.061 10.007
65
1.838 .314 .015
.001 .024 .143
.006 .940 .666
.060 10.007
66
1.835 .316 .016
.001 .022 .142
.004 .941 .667
.062 10.009
67
1.835 .316 .013
.002 .023 .142
.004 .943 .674
.060 10.012
AVER: 1.836
.315 .014 .001
.024 .143 .005
.941 .670 .061
10.010
SDEV: .003
.001 .002 .001
.001 .002 .001
.004 .004 .001
SERR: .001
.000 .001 .000
.000 .001 .000
.001 .001 .000
%RSD: .2
.4 11.2 44.1
3.8 1.1 13.5
.4 .5 1.1
Pyroxene
Mineral End-Member Calculations
Wo En
Fs
58
38.3 53.6 8.2
59
38.2 53.6 8.2
60
38.1 53.5 8.4
61
38.4 53.6 7.9
62
38.1 53.7 8.1
63
38.2 53.7 8.1
64
38.3 53.5 8.2
65
38.1 53.7 8.2
66
38.1 53.8 8.1
67
38.3 53.6 8.1
AVER: 38.2
53.6 8.1
SDEV: .1
.1 .1
Detection
limit at 99 % Confidence in Elemental Weight Percent (Single Line):
ELEM: Si
Al Ti V
Cr Fe Mn
Mg Ca Na
58
.014 .007 .041
.030 .028 .027
.025 .005 .009
.009
59
.014 .007 .041
.030 .028 .027
.025 .005 .009
.009
60
.014 .007 .041
.030 .028 .027
.025 .005 .009
.009
61
.014 .007 .041
.030 .028 .027
.025 .005 .009
.009
62
.014 .007 .041
.030 .028 .027
.025 .005 .009
.009
63
.014 .007 .041
.030 .028 .027
.025 .005 .009
.009
64
.014 .007 .041
.030 .027 .027
.025 .005
.009 .009
65
.014 .007 .041
.030 .027 .027
.025 .005 .009
.009
66
.014 .007 .041
.030 .027 .027
.025 .005 .009
.009
67
.014 .007 .041
.030 .028 .027
.025 .005 .009
.009
AVER: .014
.007 .041 .030
.028 .027 .025
.005 .009 .009
SDEV: .000
.000 .000 .000
.000 .000 .000
.000 .000 .000
SERR: .000
.000 .000 .000
.000 .000 .000
.000 .000 .000
Percent
Analytical Error (Single Line):
ELEM: Si
Al Ti V
Cr Fe Mn
Mg Ca Na
58
.4 .5 11.6
47.5 4.5 1.4
11.7 .3 .3
1.9
59
.4 .5 10.0
89.7 4.5 1.4
12.3 .3 .3
1.9
60
.4 .5 10.1
53.2 4.4 1.3
11.7 .3 .3
1.9
61
.4 .5 12.6
48.9 4.7 1.4
12.8 .2 .3
1.9
62 .4 .5
10.7 349.9 4.6
1.4 12.7 .3
.3 1.9
63
.4 .5 10.8
49.1 4.5 1.4
11.2 .2 .3
1.9
64
.4 .5 11.3
78.2 4.7 1.4
14.7 .3 .3
1.9
65
.4 .5 10.2
51.0 4.5 1.4
11.0 .2 .3
1.9
66
.4 .5 9.8
45.7 4.7 1.4
13.6 .2 .3
1.9
67
.4 .5 11.3
32.3 4.7 1.4
15.4 .2 .3
1.9
AVER: .4
.5 10.8 84.6
4.6 1.4 12.7
.2 .3 1.9
SDEV: .0
.0 .9 94.7
.1 .0 1.5
.0 .0 .0
SERR: .0
.0 .3 30.0
.0 .0 .5
.0 .0
.0
ELEM: Si
Al Ti V
Cr Fe Mn
Mg Ca Na
60ci
.036 .007 .008
.001 .005 .012
.003 .012 .014
.002
80ci
.056 .010 .012
.001 .008 .018
.004 .019 .022
.003
90ci
.074 .014 .016
.002 .011 .024
.006 .025 .029
.005
95ci
.091 .017 .020
.002 .013 .030
.007 .031 .036
.006
99ci
.131 .024 .029
.003 .019 .043
.010 .045 .052
.008
Test of
Homogeneity at 1.0 % Precision (Average of Sample):
ELEM: Si
Al Ti V
Cr Fe Mn
Mg Ca Na
60ci
yes yes no
no yes yes
no yes yes
yes
80ci
yes yes no
no no yes
no yes yes
yes
90ci
yes yes no
no no yes
no yes yes
yes
95ci
yes yes no
no no yes
no yes yes
yes
99ci
yes yes no
no no no
no yes yes
no
Level of
Homogeneity in +/- Percent (Average of Sample):
ELEM: Si
Al Ti
V Cr Fe
Mn Mg Ca
Na
60ci
.2 .2 2.5
3.2 .9 .3
2.2 .1 .1
.3
80ci
.2 .3 4.0
5.0 1.4 .5
3.4 .2 .2
.5
90ci
.3 .3
5.3 6.6 1.9
.7 4.5 .2
.2 .7
95ci
.4 .4 6.5
8.1 2.3 .8
5.6 .3 .3
.9
99ci
.6 .6 9.4
11.6 3.3 1.2
8.1 .4 .4
1.3
Detection Limit
in Elemental Weight Percent (Average of Sample):
ELEM: Si
Al Ti V
Cr Fe Mn
Mg Ca Na
60ci
--- --- .013
.004 .008 ---
.006 --- ---
.003
80ci
--- --- .020
.007 .012 ---
.009 --- ---
.005
90ci
--- --- .026
.009 .016 ---
.012 --- ---
.006
95ci
--- --- .032
.011 .019 ---
.015 --- ---
.008
99ci
--- --- .047
.016 .028 ---
.022 --- ---
.011
Projected
Detection Limits (99% CI) in Elemental Weight Percent (Average of Sample):
ELEM: Si
Al Ti V
Cr Fe Mn
Mg Ca Na
TIME: .31
.31 .47 .47
.47 .47 .47
.63 .63 .47
PROJ: ---
--- .372 .129
.224 --- .176
--- --- .089
TIME: .63
.63 .94 .94
.94 .94 .94
1.25 1.25 .94
PROJ: ---
--- .263 .091
.158 --- .125
--- --- .063
TIME: 1.25
1.25 1.88 1.88
1.88 1.88 1.88
2.50 2.50 1.88
PROJ: ---
--- .186 .064
.112 --- .088
--- --- .045
TIME: 2.50
2.50 3.75 3.75
3.75 3.75 3.75
5.00 5.00 3.75
PROJ: ---
--- .132 .045
.079 --- .062
--- --- .032
TIME: 5.00
5.00 7.50 7.50
7.50 7.50 7.50
10.00 10.00 7.50
PROJ: ---
--- .093 .032
.056 --- .044
--- --- .022
TIME: 10.00
10.00 15.00 15.00
15.00 15.00 15.00
20.00 20.00 15.00
PROJ: ---
--- .066 .023
.040 --- .031
--- --- .016
TIME: 20.00
20.00 30.00 30.00
30.00 30.00 30.00
40.00 40.00 30.00
PROJ: ---
--- .047 .016
.028 --- .022
--- --- .011
TIME: 40.00
40.00 60.00 60.00
60.00 60.00 60.00
80.00 80.00 60.00
PROJ: ---
--- .033 .011
.020 --- .016
--- --- .008
TIME: 80.00
80.00 120.00 120.00
120.00 120.00 120.00
160.00 160.00 120.00
PROJ: ---
--- .023 .008
.014 --- .011
--- --- .006
TIME: 160.00
160.00 240.00 240.00
240.00 240.00 240.00
320.00 320.00 240.00
PROJ: ---
--- .016 .006
.010 --- .008
--- --- .004
TIME: 320.00
320.00 480.00 480.00
480.00 480.00 480.00
640.00 640.00 480.00
PROJ: ---
--- .012 .004
.007 --- .006
--- --- .003
TIME: 640.00
640.00 960.00 960.00
960.00 960.00 960.00 1280.00 1280.00 960.00
PROJ: ---
--- .008 .003
.005 --- .004
--- ---
.002
TIME: 1280.00 1280.00 1920.00 1920.00 1920.00
1920.00 1920.00 2560.00 2560.00 1920.00
PROJ: ---
--- .006 .002
.004 --- .003
--- --- .001
Analytical
Sensitivity in Elemental Weight Percent (Average of Sample):
ELEM: Si
Al Ti V
Cr Fe Mn
Mg Ca Na
60ci
.051 .009 .011
.001 .007 .017
.004 .017 .020
.003
80ci
.079 .014 .018
.002 .011 .026
.006 .027 .031
.005
90ci
.105 .019 .023
.003 .015 .034
.008 .036 .041
.006
95ci
.129 .024 .029
.003 .018 .042
.010 .044 .051
.008
99ci
.186 .034 .041
.005 .027 .061
.014 .063
.073 .011
Plotting Analysis Data
The use may wish to examine the traverse data in a graphical presentation. Click the Plot! button in the main PROBE FOR WINDOWS log window. This opens the Plot! dialog box.
First, choose the pertinent samples from the Sample List list box. Select the required X-Axis, and Y-Axis items from the axis lists. Choose a Graph Type and the button Send Data to Plot Window. Finally, click the Output button.
Here the user selects the X-Stage Coordinates for the X-Axis and multi-selects the TiO2, V2O3, Cr2O3 and MnO Oxide Percents for the Y-Axis. This graph is displayed below. Furthermore, the weight percent concentration of any point may be read directly off the plot using the two-way Hot Hit On/Zoom On button. Any graph maybe directly output using the Print button.
Closing the Current Run and Probe for Windows
The user ends the analysis session from the main PROBE FOR WINDOWS log window. Select File from the menu bar and click Close from the menu selections.
This opens the ProbFormCloseFile window, click Yes to close this file.
Close PROBE FOR WINDOWS by selecting File from the menu bar and clicking Exit.
