Spectra Plus Tutorial Manual M84-E00030 PDF

BRUKER ADVANCED X-RAY SOLUTIONS
SPECTRAplus
Tutorial Manual
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SPECTRA Tutorial Manual Your First Calibration
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This tutorial chapter covers the following topics to get you acquainted with calibrating:
Preparation for Calibration
Getting to know your calibration tools
Starting the Calibration
Measurement of Unknown Samples with the Low-Alloy Calibration
Using the XRF Results Manager
Drift Correction
Here, you will perform your first calibration from beginning to end, step by step. Your task will be to
calibrate low-alloy steels using a set of BCS low-alloy steels and predefined lines from the
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SPECTRA line library and scan measurements. No measurements are necessary since all samples
were measured on the Bruker AXS master SRS in Karlsruhe. But carefully follow all steps to obtain the
same results shown.
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8 Start the XRF Quantification (FQuant) program from the SPECTRA

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program folder.
8 Select File > New.
8 Select the Materials directory. A dialog window will appear and may show a list of one or more
factory-installed files.
8 In the window, select Training for Material groups and type low-alloy-steel for New material. Then
press the New File button (red circle) to create this new file and have it appear (highlighted) in the
list.
1RWH: The group might already be in your database (and the list). If so, just click on it in the list to
highlight it. No inputs will then be necessary.
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Your First Calibration SPECTRA Tutorial Manual
8 Press Next. The Orientation screen appears.

7 Select the element buttons shown, in the order shown in the list at right, to speed later entry of
their concentrations. Make sure that the Oxide button is not pressed.
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8 Press Next twice. The Standard Materials screen appears. Here, you can enter the standards and
their concentrations.
7 If no concentrations are listed, you must enter them manually. First refer to the appropriate table in
the appendix for correct standard names and concentrations. Then enter the name of each
standard in the New standard material field exactly as shown, pressing the New button (circled)
after each name entry.
Once you have entered all standard names, begin entering the concentrations as follows:
+LQW: If you are used to entering all the concentrations of one element for all standards, it is very
useful to switch the After validation button to Bottom. With the Bottom button selected, after you have
typed the concentration value and pressed New, the cursor will move down.
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Since in low-alloy steel samples the iron is not certified, you must let SPECTRA calculate the value
as balance to 100.
8 Scroll to and click on the Fe column heading so that the Fe column is highlighted.
8 Click the right mouse button, select Column Balance, and set the number of decimal places you
want to see in the list. We recommend 2 decimal places since in low-alloy steel samples the iron is
not certified.
8 Press Next. The following message appears.
8 Select Yes and the entered concentrations will be saved in the database (FLUO.MDB). For your
convenience, all concentrations are already stored in the database.
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8 Select Solid for Preparation and Method by clicking on the item in the field menu (circled arrow).
8 Press Next.The Size screen appears.
8 Select 4 cm diameter, 100g, and Fixed values for all samples.

1RWH: These settings will be used to calculate the mass absorption and other parameters
needed for correcting intensities of samples which are not infinitely thick for the X-rays. Refer
to the Theoretical section of this manual (Analyzed Layer) for more information.
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8 Press Next three times. The Standard Samples screen appears.
8 Press the Wizard button (circled above).
8 Be sure to use short names, and select OK to all.
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1RWH: In this part, we combined concentrations entered in the database with the actual
preparation to a (physical) sample which has a name. In order to distinguish between samples
of the same standard but with different preparations, you can select the long name as
highlighted above. Here, the SS_401-1 sample would be called SS_401-1-solid.
8 Press Next twice.
8 Press Launchto activate the XRF Measurement Method program, in which you will set the
measuring conditions.
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8 Press on the Elements tab to display all elements.
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8 Press the Lines tab to check the choice SPECTRA

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made for your lines and change any lines
you do not like.
8 Choose an element from the Element field menu and see which line SPECTRA
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chose (appears
in the left window).
The acquired data was collected on the master SRS using S and Mn the High Res Lines (HR-Min).
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You will now exchange the HS-Min lines that SPECTRA chose for the HR lines for S and Mn in
order to have the same conditions as for the measured data.
8 Click on the element line in the left window.
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8 Press Remove.
8 Select the HR-equivalent line in the right window, and press Add:
8 Select the element Mn and follow the same procedure for it.
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8 Click the Modes/Time Tab.
8 Select Run scan measurements, and change the Time per range to 100 seconds.
1RWH: With these settings, SPECTRA will run scans of 2Theta=10 times the collimature
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aperture of the collimator used for the line around the theoretical peak maximum with a total
time of 100 seconds and a step size of 10% of the collimator aperture.
This setting will apply to all lines. Thus, you will see global parameters for the method
checked.
8 Select Intensity reduction and Automatic calibration control to run these scans to make sure we
always remain in the linear region of the detectors. (Refer to the theoretical section Dead time of
counters.)
8 Click on the Parameters tab.
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8 Select Vacuumand 34mm as the size for the irridated sample diameter:
8 Select the Line tab again.
8 Click File > Save to save your file. Then, select File > Exit.
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8 Press Yes to save the file (method).
Now you will go back to the Quantification Editor and perform the measurements of the standards with
the Loader as follows:
8 Press Next twice to skip past Measurement Parameters and go directly to the Measurement
Standards. (You are skipping Measurement Parameters, because you do not need to check or
change any of the selected lines in that window since this method will use only library lines.)
$ We just simulated the setup for measurement of the standards, since all data is already on your
hard disk.
$ Ensure that the actual Measurement Server program is running by checking to see that the
operation icon is flashing. The icon is located in the status line at the bottom of your screen (and is
marked with a red circle two figures back). If the icon is not there, press the Windows Start button,
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select the SPECTRA program, then the XRF Measurement Program. If you do not have a
spectrometer attached, you may skip this section and go directly to page 2-16.
8 Press Launch. The Loader window appears.
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8 Click on an empty position in the Loader.

8 Select Standards > Import From Database.
8 Press Search From Database to see how many standards are actually stored for this material and
preparation.
8 Then press Import at Current Position to display the standards on the loader.
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$ You can move the cursor with the arrow keys to any of the cups, and SPECTRA will display the
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samples standard name, the method (Analytical), preparation used, and the location of the
standard file.
8 To measure these samples, you would press the Send all samples button (left circle). But since all
measurements are done, simply press the Clear new samples button (right circle) and close the
Loader.
8 Go back to the Quantification Program.
8 Select Next twice to arrive at the Calibration Method window.
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$ In this window, you see which material and preparation we selected and how many standard
samples exist.
8 Press Next.
8 Press Uncheck missing stds (standards).

This function cancels the standards that were not measured.
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8 Press Next.
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Spectra reads all the data from your hard disk and then calculates the variable alphas for
the matrix correction.
Youve arrived at the actual calibration screen!
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In this section, you will be introduced to the calibration screen and toolbox.
Graphical
Tabular
display
Display
Toolbox
The Calibration Toolbox contains all the tools needed to perform a complete calibration without using
traditional entry techniques with the keyboard. You can access (toggle open and closed) the toolbox
with the Tool button (circled) in the menu bar, or by pressing F2.
Following are basic descriptions of the tools in the Calibration Toolbox. (For more details on the
options and buttons you can use, refer to the Software Reference Manual.)
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The Elementbutton is used to change from one element to another. You can also use the arrows to
the left of this button to change elements.
The Linebutton lets you select the actual lines you want to calibrate for the element. When you press
this button, you see all lines of your line library that have the same settings as the line(s) you used to
measure the standards. (Thus, the number of lines you see will depend on your line library.) This
feature might be a little confusing but will help you in the future.
As an example, press this button for an actual element (as shown for Si).
You can easily distinguish the standard library lines by their missing extensions. Si KA1 HS-
Min is a standard library line, whereas Si KA1-HS-Min/LAS is a copy of the HS-Min line used
for a specific material. This copy can be altered (e.g. by changing the predefined background
positions or by changing the reference sample). Whenever you change settings like kV, the
discriminator windows of the detectors on these method-specific lines will loose their property
of being a copy of the standard line and its factory calibration. Once altered, it will not be
shown together with the standard line.
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If scan measurements were made, lines with different background positions are still
displayed.The difference in background positions is not important once a scan is made.
When the line displayed is different from the line mentioned in the tutorial, change to the line
mentioned.
See the Theoretical part of this tutorial manual for more details on the line library.
The Compute and Refreshbutton forces a calculation and/or refresh of all displayed and calculated
values.
The Line Order button sets the sequence used by the interactive evaluation to evaluate each element
line. For the routine automatic evaluation, you will use only Line Order 1.
,PSRUWDQW: Throughout this tutorial, you will be using one line per element. Always make sure that this
line is set as line 1.
The Graphical Displaybutton is used to activate and switch to the Graphical Display window, which
shows a graphical representation that corresponds to the standards highlighted in the Tabular Display
window. Click on the X in the buttons upper right corner when you want to close the display window.
The Tabular Displaybutton (also called the Display Standards button) is used to activate and switch to
the Tabular Display window, which shows a text-and-numerical representation of the standards and
their theoretical and calculated concentrations. You can customize the Tabular Display window using
the customization (glasses) icon in the windows upper right corner.
The Comparisonbuttontoggles the Comparison window open and closed. In this window,
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SPECTRA logs all the settings you are applying to the current element. Here you can find out if the
correction or the new parameter you selected improved the calibration or not. It is also possible to go
back to a setting you used before (explained later and in the Software Reference Manual).
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The Standard Deviation display shows the actual deviation value derived from the calibration of the
current element (library line).A value that displays over an orange background is the standard
deviation of the precalibrated line.
The Expand button (down arrow) lets you gain access to more options in the Toolbox by expanding it
(compare figures below). The Reduce button (up arrow) shrinks the toolbox so that the commands
from the expanded area are no longer visible.
The Overlaybutton displays the overlay menu.
The Alphasbutton displays the settings for the computation of alphas.
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The Summarybutton displays the Summary window, where SPECTRA automatically creates a
short calibration summary of the actual line. This function will greatly reduce your time documenting
the working calibrations.
The Active button automatically calculates the offset of the regression curve.
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The Abs, Rel, and Stat buttons let you change between different regression weightings. (Refer to the
Theoretical section of this manual for details on the Regression Weightings.)
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You will now proceed with the calibration procedure, which takes advantage of the programs many
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built-in intellegent default settings (already included in SPECTRA ). The procedure is easy, and all
information and commands are just a mouse click away, which means you need not
wonder about alpha coefficients.
switch between applications.
provide paper for noting your comments or logging your actions.
To best explain the calibration procedure, we will guide you through sub-procedures, each calibrating
a different element line. Use the Toolbox tools to perform the calibration.
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8 Select element Si.
8 Select the Si KA1-HS-Minline.
8 Press the Compute and Refreshbutton.
8 Press the Graphical Displaybutton.
8 Select theFullScreen Display button (in the upper right corner of the Graphical Display window).
8 Select the Tabular Display button.
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$ Compare the chemical and the XRF(calculated) concentrations, note the deviations of the
standards, and see if it is a good calibration.
8 You have just completed the calibration for that line. Select 1 as a line sequence.
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8 Select element V.
8 Select the V KA1-HS-Min line.
8 Press the Compute andRefresh button.
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standards, and see if the calibration is improving.
8 Press the Active buttonto deactivate(toggle off) the Offsetfunction.
standards, and look again for improvement.
8 Check the Graphical Display window for outliers.
8 Select 1 as a line sequence.
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8 Select element Cr.
8 Select the Cr-KA1-HS-Min line.
8 Press the Compute and Refresh button.
8 Press the Active button (deactivate Offset).

8 Select the Tabular Display button.
$ Compare the chemical and calculated concentrations, and note the deviations of the standards.
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8 Select element Mn.
8 Select the Mn KA1-HR-Min line.
$ Compare the chemical and calculated concentrations, and note the deviations of the standards.
8 Delete the SS405 standard (since its deviation is too high) by double clicking on it.
This is the best that we can improve these standards.

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8 Select element Mo.
8 Select the Mo KA1-HS-Min line button.
8 Compare the chemical and calculated concentrations, and note the deviations of the standards.
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8 Select element Ni.
8 Select the Ni KA1-HS-Min line button.
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8 Select element Cu.
8 Select theCu-KA1-HS-Min line button.
8 Deselectthe Active button to deactivate Offset (if activated).
$ For a change, observe the data from the Graphical Display window. (Data here is equivalent to
that in the Tabular Display window.)
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8 Select element P.
8 Select the P KA1-HS-Minline button.
8 Press the Compute and Refreshbutton.
8 Deselect the Active button (to deactivate Offset).
1RWH: Some Standards do not fit the regression. The reason is that there could be an overlap.
8 Click the Overlaysbutton.
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All standard library lines are provided with calculated overlap factors for ease of use.
Sometimes you may see an overlay of an element which was not included in your
measurement or your actual standards.
8 To demonstrate the optimization, click on the "" button directly left of any line, then select None to
remove all the calculated overlay corrections for each line listed.
$ Notice that the standard deviation (circled) went up, indicating that the calibration got worse.
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8 Click the first ""button to display the most probable overlay (that being Mo LI).
8 Select Mo LI.
8 Press Calc (circled) to set the correction method, and note the good standard deviation.
8 In the Toolbox, set this line as line 1.
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&RQJUDWXODWLRQV! You just corrected for a very nasty

overlay!
8 Compare the chemical and calculated concentrations, and note the deviations of the standards.
8 Select element S.
8 Select the S KA1-HR-Min line button.
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$ Notice that the first standard in the list has a very big absolute deviation.
8 Delete this standard from the calibration.
$ Check the Graphical Display window to understand why we eliminated this outlier.
Now the deviation is in the range of the 95% confidence interval of the standards.
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8 Select element Fe.
8 Select the Fe KA1-Majline button.
1RWH: Here the calibration does not yield a good statistical deviation because we treat the Fe
concentrations as balance to 100.
8 Set the line as line 1.
8 Select File > Save As. (A filename will be automatically inserted.)
8 Press Save.
You have just finished the calibration of all lines. Go now to Measurement of Unknown Samples With
the Low-Alloy Calibration.
1RWH: Since default lines from SPECTRA were used, they will be automatically recalibrated when
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you run the standardless recalibration procedure.
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1RWH: Understandably, this section works only when you have a spectrometer attached.
In this section, you will use some known samples and measure (evaluate) them as if they were
unknowns to assess the quality and then to document the calibration.
8 Start the Loader program from the SPECTRA
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program folder.
$ If any samples with yellow boxes display on the Loader, select the samples (8), then select
Samples > clear all Samples done to remove them.
$ If any samples with red boxes display on the Loader, select the samples (8), then select Samples
> clear all Samples in Error to remove them.
1RWH: You can also use the toolbar icons that symbolize these commands.
In this procedure, you will reset the definition file, which controls the next input window and how the
samples are identified by the routine definition file:
8 Select Samples> Definition file.
8 Navigate to c:\specplus\libraries\Measmethods.
8 Select Routine.def and press Open.
8 Click on the first position where you want to put your sample.
8 Select Samples > Edit.
The Sample Definition Table appears. The contents and the functions of this table are
controlled by the definition file you previously loaded. You can modify this definition file to suit
your needs and save it under any filename with the tool SAMPLEDEF. (Refer to the
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SPECTRA Reference Manual, Chapter 9.)
7 In the Sample Definition Table, type SS403-unknown as a Sample name.
7 Select Low-alloy-steel for the Method.
7 Select Bulk as the Type.
7 Select Solid for the Preparation.
8 Press the Create Samples button.

8 Select the samples and Send selected samples.
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The measurement will start, and the sample list will display in the window below the samples.
All measurements are stored in the Measure database (Measure.mdb). To see the results, you
will use another program (XRF Results Manager), which will query the database
(Measure.mdb) and can also display online results.
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In this subsection you will:

set up a measurement Method Mapping file, which is a format file for displaying and transferring
your results from the low-alloy calibration.
start XRF Results Manager in Monitoring Mode to get an online display of results.
query the database for results measured some time ago.
transfer data from the database to Excel or Access.
8 Double-click the Results Manager icon in the SPECTRA

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folder to launch the program.
8 Select File > New Measurement Mapping Wizard.Increase the resulting window to full screen
size. Hereyou must set up a style (called a Measurement Mapping List) for the method used in
our case, low-alloy-steel.
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8 Press the button and select the method ending with low-alloy-steel.
8 Press Next.
The resulting screen lets you set various print order functions. You could set all functions to
their default values with the Default All button, or you could custom set each function to a
setting of your choice.
For instance, you could set the program with custom settings as simple as printing by Atomic
Number, Alphabetical, or Concentration order. Or you could implement a more elaborate
custom scheme of assigning numbers to the elements by clicking on each element, and
assigning a number to it that specifies its print order.
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7 Click each element in the following order and assign it a number in increasing order (to obtain this
print order):
Si, P, S, V, Cr, Mn, NI, Cu, Mo, Matrix(Fe), Sum
8 Press Next.
In this screen you can specify if you want an automatic changeover from % to PPM (parts per
million) when a certain threshold is reached. A threshold of 0.1% is good.
8 Press Next.
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In this screen you can force how you want the element printed.
PPM displays only ppm.
Auto displays as % if over the threshold (set in the previous screen). Otherwise, it will be displayed
as ppm.
Percentage displays only %.
8 Ensure that the above elements are selected, then press the Percentage button and those
elements will display at %.
8 Press Next.
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In this window, you can set the decimal places and/or significant digits to be displayed by pressing the
element (or special) button as often as needed to display the correct number of digits. Use the Decimal
places and Significant digits diagrams (circled) as guides.
8 Press the Matrix and Sum buttons as needed to set each to 2 digits (as shown, circled).
8 Press each element button shown (as needed) to set each to 3 digits.
8 Press Next.
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In this screen, you can set the printout mode of the concentration to:
only Compounds (e.g. If there would be SiO2 in our method).
only Elements (in our low-alloy-steel file, we want to have just Element concentrations)
or Automatic, which displays Compounds (displayed in %) up to a threshold, and displays
Elements when over the threshold (displayed as ppm).
8 Press the Elements button to select elements for all.
8 Press Next.
In this window, you could decide if you want to see Intensities and some special fields (Operator, etc.)
in the display and printout. Make no changes to the window, though. For now we want to specify no
intensities or special fields.
8 Press Next.
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This window prompts you for a name (usually that of the measurement method you started with).
8 Type a name after the directory shown, then press Create to make a mapping file (with your
specified name and the extension .ml) in the specified directory. Note that the mapping file should
be the same as the method used.
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8 Select File > Save As to save the Wizard settings for this mapping (.ml) file.
+LQW: You can create more than one mapping for a measurement method. Just use different names.
Always make sure that the ML files are in the MEASMETHODS directory.
7 Type a filename to match the ML file you just stored. And press Save.
8 Exit the Results Manager, and open the Results Monitor.
8 Select File > New Monitoring View.
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8 Select ORZDOOR\VWHHO in the Measurement Methodline (first data field).

8 Select ORZDOOR\VWHHO as a Mapping List in theMappingline (second data field).
8 Press the Update from Database button (circled at bottom right of display window) to see the
running measurements.
8 Press the (Printer) Setup button to set the printer, the font, and the header and footer for your
printout.
8 Set the number of results to display and print on one page (circled).
8 Leave the window open and to see when a sample is finished measuring.
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For more details on the XRF Results Program, refer to the SPECTRA Reference Manual.
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The commonly used method-specific drift correction is not necessary, since all lines used are part of
the global line library. All precalibrated lines that you use also as lines for the semiquantitative
standardless measurements are recalibrated using the four glass samples provided with your system.
Although the lines you used for the low alloy program now have new coefficients, obtained with this
calibration stored in the Low-Alloy-FCL file, the precalibrated coefficients for the standardless program
are still stored in the line library.
To perform a recalibration with these glass samples, see the tutorial in section 3 on how to recalibrate
the standardless program.
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SPECTRA Tutorial Manual Calibration of Carbonates as Fused Beads and as Wax Pellets
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This section covers the following topics:
Entering Oxidic Materials in the Standard Table.
Treating Loss on Ignition.
Defining Preparations for fused beads and Pellets with binder.
Defining variable preparation parameters.
Measuring multiple lines for one element.
Calibrating Oxides with variable alphas covering a wide concentration range.
Interactively evaluating samples using this quantitative calibration.
Mixing different preparation techniques in a calibration.
Evaluating samples with a different preparation.
This section is divided into six subsections for your convenience:

1. Getting from the Standards to the Measurement
2. Calibrating the Pressed Pellets
3. Interactively Evaluating using the Carbonates Calibration
4. Calibration of the Carbonates as Fused Bead
5. Using the Fused Bead Calibration
6. Measuring Fused Bead Samples
For each section, you will need about 20 minutes to complete the work examples.
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Calibration of Carbonates as Fused Beads and as Wax Pellets SPECTRA Tutorial Manual
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This section covers steps from entering the standard materials into the database to measuring them
with an SRS. All required data was previously measured on the master SRS and is supplied and
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installed with your SPECTRA distribution CD.
8 Start the XRF Quantification Manager program from the SPECTRA
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program folder.
8 Click File > New.
8 Click on Materials in the directory.

8 Select Trainingas the Material group.
If Training does not appear in the Material groups list, check that the training files are still
installed on your system. If they not installed, see the Troubleshooting section of this manual
for details on how to reconstruct the group (which will require entry of all the data by hand).
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8 Click on the Carbonates line of data.

8 Click Next.
In this screen, you are able to select the elements you want to calibrate, choosing between
oxides and elements.
Since we want to use the variable alphas to calibrate, we would have to input all
concentrations so that the sums of the standards are close to 100%. You would input them by
clicking on the elements that are listed in the table in the appendix (ensuring the Oxides button
is pressed to select them as oxides). In our case, however, we have already input all the
elements and concentrations in the database, so you do not have to enter them.
8 Click Next. The compounds screen appears.
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Here, you can add to your elements list those compounds which are not the usual oxides or
matrix compounds and which you could not add in the previous screen (compounds such as
LOI, CO2 or SiC, CaCO3 etc.).
8 Click on LOI, then press Add (if you had to enter also the elements).
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8 Press Next. The Standard Materials screen appears.
In this screen you would now enter the concentrations of the various standards. Again, we
have already done so for you, so no entries are needed. (However, in case your table is empty
or corrupted, see the appendix for the full list, and enter the concentrations at this time.)
Formatting of this table is like using any available spreadsheet under Windows.
8 Click any row and press the right mouse button.
+LQW: In all standard Windows-based programs, you can modify properties of an object by
clicking with the right mouse button.
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Select the number of decimal digits (3) and the unit (set to %).
8 Press Next. The Preparation screen appears.
Here you describe how you prepared the standard samples.
In our case, we have prepared the standards as pressed pellets with Hoechts-Wax C as a
binder. The binding agent is CH2 (wax). Therefore, we named the preparation WAX and used
the pressed pellet method.
Wax was declared as an additive, and the default weights were 10g sample and 0.8 of wax.
(For more information on sample preparation, see the Appendix.)
2-6 M84-E00030 -0899

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1. Define new name

(NEW) or use
existing preparation.
2. Choose a method.
3. Choose binder
or additive.
4. Enter default
weights.
5. Click default preparation

box if you might have
variable preparations.
1RWH: Any changes you make to an existing preparation may affect calibrations and samples
used in previously made methods. If in doubt, check before changing.
8 Press Next. The Size screen (a submenu of the Preparation screen) appears.
SOXV
Here you can enter sizes and weights of the default sample so SPECTRA can acquire data
it needs for the sample thickness correction and the absorption correction.
8 Press Next three times. The Standard Samples screen appears.
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6WDQGDUGPDWHULDOV

SUHSDUDWLRQ

6WDQGDUGVDPSOH
In this window, we will now create entries in the database for any prepared standard materials we want
to use for the calibration.
$ Ensure that the correct Material group, Material, and Preparation are selected (as shown in the
dashed circle).
8 Press the Automatically create all Standard Samples button to create the samples using the
default naming convention (long names).
$ Observe what SPECTRA
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did for you in the list window.
7 Enter the actual weights of your standards in the columns for Material Mass and Additive Mass.
8 Press Next.
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You are one step away from the measurement but must first decide on a measurement
method and parameters for the lines you will use. A method defines the elements and lines
used for the measurement, the type of measurement, and all the measuring times, as well as
the atmosphere used.
8 Press Next. The Measurement Method programs launch window appears.
8 Press the Launch button to start the Measurement Method program.
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Now well let SPECTRA select some conditions for us:
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We want to measure one line per element, and SPECTRA should select the lines with the
highest intensity for our thick samples.
Included should be the Compton and the Rayleigh line.
8 Set the buttons and check the boxes as shown in the next screen, turning on One LineHighest
IntensityThick sample/high energy lines, Compton Lines, and Rayleigh Lines.
8 Press the Default line set for current material button.
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8 Click the Elements tab.

8 Deselect Carbon, since we will not measure that element. (We used wax as a binder, which
contains Carbon, so measuring that element does not make sense.)
8 Click on the Lines tab.
8 Click OK to save the changes in the element list.
M84-E00030 -0899 2-11

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8 Select the Lines tab to seewhich lines SPECTRA

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chose.
8 Select the element Si.

The only line measured so far is the HS Min Line (left window). This is perfectly OK, since we
will be using automatic current reduction and, thus, always be without a pile-up effect. When
line naming conventions seem unclear, see the Introduction to XRF section.
8 click on the related Maj line in the right window.(All lines in the right window are available in
your line library). Press the Addbutton to include that line in the active (left) window.
Repeat the above two steps for elements Al, S, Ca, and Fe, and their Maj line.
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8 Click the Modes/Time tab.
$ Make sure that the screen looks like the figure above.
You will measure scans for each element line and use them to determine the peak and the
background (to get net intensities).
The scan range for each element will be +/- 10 times the collimator aperture of the collimator
used for the specific element (e.g. Ca uses a 0.46 degree collimator, so the scan range will go
4.6 degrees 2T in both directions from the theoretical position of the peak). The total time for
that scan will be 60 seconds, and the step size of the scan will be 10% of the aperture of the
used collimator (in our example, 0.046 degrees).
Currently the program is set with global measuring conditions, meaning they apply for all
elements in your method. Since the fluorescence yield of some elements is not very high or
the concentrations are very small, you could use local parameters for some lines. We will, in
fact, use local parameters for Cl, Mn, Na, Sr, and Ti, all of them (except Na) are traces. The
scan times for these elements should be increased to 100 seconds in order to get decent
counting statistics.
+LQW: For more details on the implications of counting statistics and measuring time, see the
theoretical part of the manual.
M84-E00030 -0899 2-13

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8 Set the Local parameters for line box.

8 Select the line (from the elements list) to which you want to assign local parameters.
A warning will appear to ask you if you want to proceed.
8 Press OK.
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8 Change the Time per range to 100 seconds (to get decent counting statistics).
You have just changed the conditions for Na.
5HSHDWthe procedure to apply the same conditions to Ti, Sr, Cl, and Mn.
8 Press the Parameters tab.

8 Set the appropriate Spectrometer mode (Vacuum, if samples will be measured under vacuum) and
use the 34mm irridiated sample diameter.
8 Click File > Exit.

8 Press Yestosave the measurement method file. Otherwise, you will not save the file.
M84-E00030 -0899 2-15

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8 Now click back to Fquant. Then repeatedly press Next until you reach Measurement Parameters.
In Measurement Parameters, you could check on the individual line settings or change
background positions. But since we are using the standard lines and scans, we do not need to
check anything here.
In the Tutorial using the High-Alloy-Steel samples, you will find instructions on how to change
background positions using the Measurement Parameters program.
8 Press Next to reach Measurement Standards.

8 Click Launch to start the Loader.
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8 Click on a free position in the loader that you want to use for measuring the standards.
8 Select Standards > Import from Database.
8 Check that you have the right material and preparation (as shown), then press Search From
Database.
All standards are highlighted, and you could import them all to the Loader by pressing Import
at Current Position. But, if you only want to import some selected standard, click on the first
one you want and then Ctrl-click on the others. Once you have marked all desired standards,
press Import at Current Position.
+LQW: You can check details on a sample (including its loading sequence) by moving the cursor
(which changes to a hand) onto a sample on the loader.
M84-E00030 -0899 2-17

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You would start the measurement by pressing the Send All Samples button (circled). But,
again, we have done that for you to save you the time of preparing and measuring all the
samples.
8 Click on Clear New Samples.
8 Click File > Exit to leave the Loader.
6XPPDU\
As you can see from the following sequence, setting up a quantitative program is easy:
Define a material
Define elements to be measured (as oxides or elements)
Insert Compounds (LOI)
Insert Concentrations
Define Preparation method (if not defined in a previous program)
Make actual standard samples and input the preparation if there are differences from the default
Define a Measurement Method
Check and/or change Parameters (use method-specific lines for doing so)
Measure the actual standards
Calibrate
&DOLEUDWLQJWKH3UHVVHG3HOOHWV
In this section, you will calibrate the wax-based samples measured previously on the master SRS in
Karlsruhe.
2-18 M84-E00030 -0899

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8 Press Next until you reach the Calibration Method subdirectory.
$ Ensure that the material is Carbonates and the preparation is Wax.

8 Press Next.
M84-E00030 -0899 2-19

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8 Press Uncheck missing stds (standards) to see if any standards are missing.
$ You should find one standard missing, as shown.
8 Press Next.
&DOLEUDWLRQ6FUHHQ
The calibration screen is where you will view and perform calibration functions. You control functions
within the calibration screen from the Calibration Toolbox, which you can switch on and off by selecting
View > Calibration Toolbox Menu, clicking the Toolbox icon in the toolbar, or pressing F2.
2-20 M84-E00030 -0899

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For more details on the Calibration Toolbox and its usage, see the Stainless Steel Calibration and also
SOXV
check the SPECTRA Software Reference Manual.
Since we used the standard lines, we are shown the Std Dev and the curve of the precalibrated line.
Pressing Compute and Refresh will change to the standard deviation derived from the actual
standards. (We also changed from Element to Compound by pressing C)
8 Make sure that you see the Graphical Display and the Tabular Display.
8 Expand the Toolbox. Then close all other windows of the Toolbox by clicking the small X
associated with them.
M84-E00030 -0899 2-21

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8 Press the Disable button in the Tabular Display window to disable all standards from the
regression which do not have any concentration listed for the actual element.
$ Lets check on some standards. Look at the absolute deviation column and then at the Graphical
Display. Lets eliminate the NIST1880 due to its deviation.
8 Double click on the point in the Graphical Display that represents the standard (or double click on
the standard in the Tabular Displaywindow) to see the change.
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$ The regression already looks better than before, but lets see if there are some overlaps that
interfere with the signal from the standard just deleted.
8 Press the Overlay button in the Toolbox.
This list already contains a lot of overlays. (Overlays are the stored correction which will be
applied if you use the line for standardless analysis).
8 Remove the stored overlay corrections by clicking the ?? button, then None
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To have SPECTRA check for an Overlay, we need to decide on the following parameters:
M84-E00030 -0899 2-23
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INFLUENCE RANGE
Minimum concentration in standards
Reflection order (see also Interference of higher reflection order in the theoretical part of the
manual)
The red vertical line represents the actual measuring position of the peak. The red horizontal
SOXV
line is the chosen influence range. SPECTRA looks now 3 or 10 times the used collimator
aperture around the peak postion.
SOXV
To detect an overlay, SPECTRA also checks the concentrations of the elements that might
interfere in your standards.
SOXV
Example: Zn has a very strong overlap on Na, but when we ask SPECTRA for possible
overlaps we will not be prompted with Zn, since it is not part of our standard materials.
8 Set a collimator aperture of 10x, a present in standards of 1%, and a reflection order of 1-2 (as
shown in the dashed area).
$ Create the overlays and notice that you get S and Mg (which are part of our standard materials),
as possible Overlays
8 Select element S.
8 Click on the S KA1,2 line button, then click on Compute and Refresh.
2-24 M84-E00030 -0899

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$ The overall standard deviation got better, and we corrected for the sulfur. You could try correcting
for Mg as well, but this will not affect the results much.
$ Make sure the active line is set to line 1 (circled) in the Toolbox.
8 Select Fe as the next element.
8 Press Compute and Refresh.

$ Check the Tabular Display and the Graphical Display windows. All standards look excellent.
8 Set this line as line 1.
8 Click on the Line button and select the next line (Maj line).
M84-E00030 -0899 2-25

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1RWH: The list may display more lines related to your element than the two you have told
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SPECTRA to measure. Do not get confused. The reason your list may vary is that
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SPECTRA looks at the actual standard measurements and then prompts you with all the
lines in your line library that have the same settings.
In this case, the Maj/High-Alloy-Steel line appears because you made a copy of the Fe-KA1-
Maj line for your high-alloy steel method (in Chapter 1, Tutorial) by pressing Insert method-
specific lines in the Measurement Method builder. Then you inserted a background position.
Since you did not change the kV and the PHA settings, this line is identical (except for different
background position) to the original line when you measure scans.
SOXV
Since we measured a scan, SPECTRA cannot detect a difference between them and, thus,
shows you this line in the selection as well. You do not need to calibrate this line, but you must
calibrate the Maj line.
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8 Press Active (Offset) and Gross (Intensity).

8 Select this line as line 2.
M84-E00030 -0899 2-27

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&DOFLXP
8 Select element CaHS-Min line.

$ Check on the absolute deviations of some standards. In this case, we exclude (delete) all
standards with an absolute deviation greater than 1% (see arrows). The reasons for excluding
standards are:
Inhomogeneous standard material
bad certified value
wrong concentration data entered
glitch in the preparation of this sample
overlay or interference due to a high concentration of another element present in this standard
2-28 M84-E00030 -0899

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8 Press Active (Offset) and make this line 2.
8 Select the Ca-KA1-Maj Line button.
8 Disable the same standards as for the HS-Min line.

8 Press Active (Offset) and Gross (Intensity).
M84-E00030 -0899 2-29

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8 Make this Line 1 and notice that the fit has improved.
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3RWDVVLXP
8 Select element K.
$ Obviously, AR4112 (like for Ca) has a problem. Disable it.

$ The Std Dev looks really good. But also check the Tabular Display window to see the individual
deviation of each standard. Make sure that you have selected line order 1.
7LWDQLXP
8 Select element Ti.
$ Highlight all standards that list no concentration, then press Disable.

$ Check the deviations of each standard. AR4112 is looking strange. and so is NIST1881.
M84-E00030 -0899 2-31

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8 Disable both these standards.

8 Make this Line 1.
0DQJDQHVH
8 Select the Graphical Display window.
$ The GBW3108 standard looks bad for this element. Check for possible overlays. The sample
might be certified wrong or there was a preparation glitch.
2-32 M84-E00030 -0899

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8 Select and disable GBW3108.
8 Disable standard An34 due to its deviation.

$ Check your overall deviation for an improvement.
$ Make this Line 1.
M84-E00030 -0899 2-33

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6WURQWLXP
8 Select the KA1-HS-Min Line.
8 In the Tabular Display window, disable all standards with trace concentration.
There is some scatter in the values but, when compared to the allowed deviation range from
the certificates, this is OK because the actual calculated values are within the 95% confidence
interval of the standards.
8 Set the HS-Min line to Line 1.
6LOLFD
8 Select the KA1-Maj Line.
8 Change to Gross (Intensity) and Active (Offset).

8 Select the Tabular Display and check on the standards.
Lets eliminate AR4112 and the NIST 1881 since they are out of their 95% confidence
intervals. Although other standards are still outside their 95% confidence intervals, we cannot
numerically make the data better.
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The deviations seen with AR4112 and NIST 1881 are mostly due to grain size effects which
are based on the preparation. (For more details, see the preparation effects in the theoretical
part of this manual.)
8 Make this Line 1.
8 Select the Si KA1-HS-Min line.
8 Select theTabular Display.
8 Delete AR4112 and NIST 1881, as mentioned above.

The same restrictions mentioned earlier apply to this line. When we look at the fused beads
(later on), we will be able to better assess the quality of the standards used.
M84-E00030 -0899 2-35

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$OXPLQLXP
8 Select element Al.
8 Select the Maj Line, and press Compute and Refresh.
$ This case looks like we need a quadratic regression.

8 Press the Alpha () button. Then press the Computed buttons below Offset and Quadratic (in the
Alphas window).
$ Except for three outliers (circled below in the Tabular window), data looks acceptable.
2-36 M84-E00030 -0899

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$ Check on the outliers for deviations.

8 Select the Graphical Display and disable the outlying samples by double-clicking them.
8 Select the Tabular Display to check again on the deviations.
8 Make this Line 1.

8 Change to KA1-HS-Min line.
8 Press the Alpha () button. Then press Quadratic (regression) in the Alphas window.
8 Select the Graphical Display.
8 Disable the three standards that you disabled earlier.
M84-E00030 -0899 2-37

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8 Make this Line 2.
3KRVSKRURXV
8 Select element P.
8 Press Compute and Refresh
8 Select the Tabular Display.
8 Disable all standards with trace composition.
8 Press Activate (Offset).
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$ Look at the Tabular Display and notice that all absolute deviations are within the limits of the
certificates.
8 Make this line 1.
6XOSKXU
8 Select element S.
8 Select the Maj line.
8 Disable standards with trace composition.
8 Disable the GBW3109 standard, which is out of the allowed range.
8 Press the Alphas tab and then the Quadratic (regression) button.
8 Press Relative (Rel.) under Regression Weighting.
8 Press Compute (Offset).
8 Press Fixed (Offset).
8 Select Absolute (Regression Weighting).
M84-E00030 -0899 2-39

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Now this does not look bad, especially if you note the large calibration range and when you
consider that the wax we used as a binder contains some sulfur.
8 Make this Line 1.
8 Select the KA1-HS-Min line.
8 Disable standards with trace composition.
8 Disable the highest GBW standard that is out of the allowed range.
8 Press Relative (Regression Weighting).
8 Press Compute (Offset).
8 Press Fixed (Offset).
8 Press Absolute (Regression Weighting).
$ See if you get the same results as we do in the next figure.
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8 Make this Line 2.
0DJQHVLXP
8 Select element Mg.
8 Disable the outlier for Mg (NIST 1881) in the Graphical Display.
8 Press the Active (Offset) button.
8 Click on the Line Overlay tab and insert the calculated S overlay.
$ Check on the deviations in the Tabular Display.
8 Make this Line 2.
M84-E00030 -0899 2-41

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&RPSWRQ3HDN
8 Click on Rh compton.
8 Press Active (Offset).
8 Make this line 1.

8 Click File > Save and name the calibration Carbonates.
The calibration is now finished. Test (evaluate) it, as explained in the next section.
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To check the calibration made in the previous subsection, you can use some files provided in the
Tutorial Directory and also some measured standards used in the calibration by:
using the XRF Interactive Evaluation Program
printing with the XRF Interactive Evaluation Program
8 Close the Quantification program if still active.

8 Select the Interactive Evaluation program from the SPECTRA
SOXV
folder.
8 Select File > Next Sample.
8 Press the Browse button ().
8 Go to \Libraries\Materials\Carbonates\WAX\.
8 Select sample Kalkstein1b_WAX.
8 Press Open.
M84-E00030 -0899 2-43

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8 Press Open.
8 Select Carbonates.FCL as a calibration file.

8 Select Preparation WAX.
$ Check to see that Material Mass is 10g, that Additive is 0.8g, and that Mass is 10.8g.
8 Press OK.
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8 Press Matrix (circled). The Insert Matrix dialog box appears, where you will enter a non-measured
compound (needed to get an exact analysis).
8 Enter CO2. Note that if you had no value, you would set the remainder of the total to that
compound.
8 Press OK. A new CO2 line will appear in the data window.
M84-E00030 -0899 2-45

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8 Double-click on the CO2 line to display the Compound Property dialog box.
8 Select Fixed.
8 Under Concentration (%), enter the LOI of the sample (37.6) from the table in the appendix.
8 Press OK.
8 Compare the concentration values for the different lines with the values for the certified material.
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8 Mg line 1 is Mg KA1-HS-Min. To use line 2 for the sample, double-click on Mg.
8 Click on the other line (Mg KA1-Maj) and press OK.

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Every time you change from one line to another line of the same element, SPECTRA
recalculates the whole matrix correction based on the new intensity.
$ Compare the elements with the table, and note those which are a little off.
8 Press Print Result, and note the actual certified concentrations on that page.
5HSHDW the same procedure with some other standards from the same group and compare them to the
table.
$ Note the elements which show values that are off. Go back to the calibration in the Quantification
and try to optimize the element where the values were not satisfactory. Be aware that your
calibration can never be better than the standard you used and that even good standards might
look bad whenever the preparation is not optimal.
+LQW: Invest most of your time and effort in choosing good standards ad even more in the optimal
preparation.
M84-E00030 -0899 2-47

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&DOLEUDWLRQRIWKH&DUERQDWHVDV)XVHG%HDG
The same standards used in the previous calibration (for wax samples) have been prepared as fused
beads to illustrate the difference between these two calibrations. You will perform the same calibration
process as before, by using the fused samples instead of the wax samples.
This calibration method offers three advantages:

Relatively long preparation time is required for fused beads if you desire optimum results for
analysis of different materials, especially regarding reproducibility and accuracy. The prerequisite
for this reproducibility is total homogeneity of the samples. This reproducibility cannot be reached
with pressed pellets because they can differ even with the same element concentrations both in
their mineralogical composition and in their grain sizes.
Besides homogeneity, sample dilution can be a further advantage of the fused bead method,
because interelement effects are reduced while the intensity losses of most of the elements stay in
the low range.
The third big advantage of fused beads is the possibility to synthetically prepare standards from
purely oxidic materials.
In this example, we used a fixed-amount ignited sample material to prepare the beads. In order to
calibrate back to the original concentration, we had to determine the Loss on Ignition (LOI) for each
sample. This value was included as CO2 in the standard table.
Since we loose the CO2 during fusion, we have to increase the weight of the original material by the
percentage of loss to end up with our desired weight of ignited sample.
Example of a fixed dilution preparation: 1g of ignited material is fused with 6g of flux. The calibration is
then done with the LOI corrected concentrations or the LOI has to be inputted together with the sample
in order to use the original concentrations. Another option is when the original material is weighted, so
that after the fusion the ignited original is always a constant. In order to use the 1g of ignited material
per 6g flux ratio of a substance with an LOI of 12%, the amount of 1,12g has to be weighted in as
original material together with 6g of flux.
SOXV
The terms used by the manual and SPECTRA are:
LOI Loss on ignition
Original material Unignited sample material or the original material (dried at 105 deg C)
Ignited material Ignited material
Flux Amount of flux used
This section contains the step-by-step guide for calibrating a quantitative method using fused bead
preparation.
The same standards were used as in the previous section. Only now well change the preparation, and
then well be able to compare the results of both calibrations.
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6WDUWLQJ)48$17DQG'HILQLQJD1HZ3UHSDUDWLRQIRU&DUERQDWHV
8 Launch XRF Quantification (Fluorescence) from the SPECTRA
SOXV
folder.
8 Click File > New.
8 Click on Materials in the directory.
8 Select Training for the Materials group.
8 Select Carbonates for the Material.
8 Click on Preparation in the directory.
8 Select IgnSam for the Preparation. If this does not exist, create this preparation with the
parameters shown above.
8 Tick the Default values for sample specific input.
The preparation method that was used for these standards is fusing the previously ignited
material with 7.5 g of Lithiumtetraborate. The LOI was determined after the ignition process
and entered as CO2 (LOI) in the standard table.
SOXV
This method takes full advantage of the variable input parameters support by SPECTRA
8 Press Next.The Size screen appears.
M84-E00030 -0899 2-49

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8 Check that the diameter is set to 4cm, the Mass to 9g, and all other settings are as shown. Press
Next, and save the current preparation when asked to do so.
8 Click on Standard Samples in the directory. The Standard Samples window displays.
$ Check to see if the standards already exist. If not, select (8) the sample wizard (the following
window displays) to create all standard samples using long names. Then press OK. The Standard
Samples window reappears.
7 In the Standard Samples window, click into the desired field and enter the values for the original
material and the flux from Preparation table in the appendix. (Scroll to access columns with this
data.)
2-50 M84-E00030 -0899

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$ Double check the values to ensure their accuracy.
$ Your Standard List should now look like the above.

8 Press Next.
8 When asked to save the standard data, press Yes.
The standard samples are stored with their respective weights in the database.
M84-E00030 -0899 2-51

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8 Click the Calibration subdirectory.

8 Click on Calibration Method.
$ Check that Carbonates and IgnSam are selected.
8 Press Next and check that all standard samples are present.
8 Press Uncheck missing standards to check that all standard samples are present.
8 Press Next to go to Compute Coefficient (the actual calibration screens).
7 Make sure the toolbox is active (F2).
For this material, make sure to be in Compound Mode (C is pressed on the toolbox, Oxide of
the element displayed on the Element button).
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&DOLEUDWLQJWKH(OHPHQWVIRU7KLV0DWHULDO
&DOLEUDWLRQRI)H
8 Select the Fe KA1-HS-Min line.
8 Make it Line 1.
8 Select Compute and Refresh to calculate.
8 Disable the standardKH, due to its deviation.
8 Press Active (to activate Offset).
8 Press the C in the toolbox to switch to compound mode (if not already set).
$ Check the standard concentrations and deviations.
8 Click on Overlays.
8 Make these settings: range set to 10* of collimature aperture, 1% present in standards and 1-3
order lines. Then press ??.
Since there are no Overlays, we cannot get better results with these standards.
Most of the data for Fe2O3 in the standards are certified to two decimal places.
M84-E00030 -0899 2-53

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5HSHDW the same procedure for the second line measured (Fe KA1-Maj) and make it Line.2.
2-54 M84-E00030 -0899

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6WURQWLXP
8 Select Sr.
8 Press Disable all standards with Trace in the Tabular Display.
8 Click the Overlay tab and disable all stored overlays.
$ Compare your results with the next screen.
8 Make this Line 1.
M84-E00030 -0899 2-55

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3RWDVVLXP
8 Select element K.
8 Disable all Overlays.
8 Disable all the Kalkstein and KH standards.
8 Compare your results with the next screen.
8 Make this Line 1.
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0DQJDQHVH
8 Remove all stored Overlays.
8 Disable all Standards with Trace composition.
8 Make this Line 1.
M84-E00030 -0899 2-57

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&DOFLXP
8 Select element Ca.
8 Select the KA1-Maj line.
8 Disable all Standards with an absolute deviation greater than 0.8%.
8 Compare your results with the next screen and make it Line 1.
5HSHDW the procedure for the KA1-HS-Min line and make it Line 2.
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7LWDQLXP
8 Select element Ti.
8 Select the KA1-HS-Min line and make it Line 1.
8 Disable all Standards with trace composition.
8 Disable NIST1881 and AR4112.
0DJQHVLXP
8 Select element Mg.
8 Make this Line 2.
8 Disable all overlays.
8 Press ?? in the Overlay menu and check for possible overlays.
8 Select S and set it to calculated correction in the Overlay menu.
As an alternative, you can try to correct with the Intensity (Measured).
Click on measured and select the S-KA1-HS-Min line.
Compare the effect on the Std Dev.
$ Check the deviations of the standards in the Tabular Display.
You might disable the AN34.
8 Press Active (activate Offset) and see if it gives you an improvement.
M84-E00030 -0899 2-59

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8 Make it Line 1.
8 Select Compute and Refresh.
8 Click the Line Overlays tab, disable all Overlays, and select the Overlay for S.
8 Select calculated Overlay.
8 Disable the An34 standard from the Tabular Display window.
2-60 M84-E00030 -0899

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6XOSKXU
8 Select element S.
8 Select the S KA1-Maj line.
8 Click the Line Overlays tab and disable all Overlays.
8 Press Active (activate Offset).
8 Disable all Standards withTrace composition.
8 Click the Alphas tab and enable the Quadratic (regression).
8 Make it Line 1.
M84-E00030 -0899 2-61

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5HSHDW the steps for the KA1-HS-Min line (except for the Quadratic Regression), looking for the
following results.
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3KRVSKRURXV
8 Select element P.
8 Select the KA1 HS-Min line.
8 Disable all standards with trace composition.
8 Click the Line Overlays tab and disable all stored Overlays.
8 Press the ?? button, Query for an Overlay, and select it as calculated.
8 Make it line 1
M84-E00030 -0899 2-63

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6LOLFD
8 Select the Si KA1-Maj line.
8 Click the Alphas tab and enable Quadratic (Regression).
8 Disable standard AR4112 in the Tabular Display window.
8 Make it Line 1.
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5HSHDW the same procedure for KA1-HS-Min, looking for the following results.
$ You might also try to disable both the Kalkstein standards.
M84-E00030 -0899 2-65

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$OXPLQLXP
8 Select element Al.
8 Click the Alphas tab and enable Quadratic Regression.
8 Disable standard AR4112 in the Tabular Display window.
8 Make it Line 1.
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5HSHDW the same procedure on the KA1-HS-Min line (except for the quadratic regression), looking for
the following results.
8 Make it Line 2.
M84-E00030 -0899 2-67

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6RGLXP
8 Select element Na.
8 Disable all Standards with Trace composition.
8 Press the ?? button, Select Overlays on S and Mg.
8 Set Overlay calculation to calculated.
8 Disable all Standards with a deviation greater than 0.6%.
2-68 M84-E00030 -0899

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8 Make it Line 1.
M84-E00030 -0899 2-69

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&RPSWRQDQG5D\OHLJK3HDN
8 Select element Rh Compton.
8 Deselect Active (to deactivate Offset).
5HSHDW the same procedure for Rayleigh.
8 Click File > Save, and save the calibration as Carbonates-FB.

8 Close FQuant.
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8VLQJWKH)XVHG%HDG&DOLEUDWLRQ
,QWHUDFWLYH(YDOXDWLRQ8VLQJ)XVHG6DPSOHV
8 Launch the Interactive Evaluation program.
8 Select File > Next SSD.
8 Navigate to Specplus\Libraries\Materials\Carbonates\IgnSam.
8 Select NBS188 as a sample and press Open.
8 Select Carbonates-FB as Calibration (FCL).
8 Select IgnSam as the Preparation.
8 Enter the original weight = 1.5182.
8 Press OK. The following window appears.
8 Press LOI, then enter CO2 as the compound for LOI, and enter 1.25 (%) as a fixed value.
8 Tick Auto Update, then press the View button (circled) to display the View Line window.
8 Click on the Si line in that window, then press Update.
8 Look at the lines displayed for the element and compare the differences by clicking at the line
shown in the lower part of the View Line window.
8 The line currently used is marked with a filled circle.
8 Double-click the highlighted line for use in the evaluation.
8 Press Print Result and document the results.
M84-E00030 -0899 2-71

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(YDOXDWLQJD*\SVXP6DPSOHDV)XVHG%HDG
8 Select File > Next SSD.
8 Navigate to Specplus\Libraries\Materials\Carbonates\IgnSam.
8 Select GBW3109 as a sample and press Open. The EVAL window displays.
8 Select Carbonates-FB as calibration.
8 Select IgnSam as preparation.
8 Enter 1.4521 as original weight. Note this Material has a GAIN on Ignition.
8 Leave flux at 7.5 and weight at 9g. (where do these display?)
8 Press OK.
8 Double-click on the CaO line (circled). A dialog box appears.
8 Modify CaO to CASO4.
8 Press OK.
8 If Auto Update is not ticked, press Recalculate button (circled), which blinks when AutoUpdate is
not ticked.
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0HDVXULQJ)XVHG%HDG6DPSOHV
If you want automatic evaluation of samples prepared as fused beads, you must remember two
important aspects:
Whenever you work with variable dilution, you need a Loader sample definition which contains
these variable parameters.
If you work with fixed dilution, you can work with the routine definition where just the name of the
preparation is entered.
Whenever you work with an LOI or GOI, you have variable dilution when you calibrate against the
original material. In this case, you have to use a Loader Definition file which includes the orig-g and
LOI field.
5RXWLQH0HDVXUHPHQWRIDVDPSOHZLWK/2,DVIXVHGEHDGZLWKYDULDEOHGLOXWLRQ
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SPECTRA needs the LOI, the amount of original material, and the amount of flux used to calculate
the dilution of the bead.
Included in the distribution are a number of Loader sample input definition files (also called DEF files)
which should cover nearly all needs. In our case, we use the OrigLOI.Def.
8 Launch the Loader. (Note that the Measurement Server must be active on your system, or on the
network, for the Loader to start.)
8 Select Sample > Definition File. The following window appears.
8 Select ORIGLOI.DEF and press Open.

8 Press Sample > Edit. The Sample Definition Table appears.
M84-E00030 -0899 2-73

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8 Enter data as shown.
In the OrigLOI.def file you enter Samplename, Method, Preparation, the amount of original
material, the amount of flux, and the LOI. These values will be automatically stored with the
Samplename and a unique identifier in your database, so that you can also reevaluate the
sample without looking up these values.
+LQW: In the tutorial, you must enter all these since your system database is empty when the
system gets delivered and does not contain these values for the tutorial samples.
8 Press Create Samples. (If you have a system, you could now measure a sample.)
8 After the measurement is finished, SPECTRA
SOXV
will automatically evaluate the sample.
If there is an FCL with the same name as the Method, this will be used.
If there is no FCL with the same name as the Method, the calibration in the line library will be
used.
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SPECTRA Tutorial Manual Calibration of a Set of Stainless Steels
&DOLEUDWLRQRID6HWRI6WDLQOHVV6WHHOV
The Tutorial section is made up of eight parts of approximately 20 minutes each for convenience:
Creating the Program and Methods (and setting the measurement conditions)
Performing the Actual Calibration (of the high-alloy-steel method)
Documenting the Calibration
Testing the Calibration
Setting up a Recalibration
Setting up a Recalibration Definition File for the Loader
Using the DumpSSD
Errata
The section is based on the material high-alloy-steel from the Material Group Training.
All needed files are located in the directory Specplus\Libraries\Materials\high-alloy-steel\solid.
M84-E00030 -0899 3-1

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Calibration of a Set of Stainless Steels SPECTRA Tutorial Manual
&UHDWLQJWKH3URJUDPDQG0HWKRGVDQGVHWWLQJWKHPHDVXUHPHQW

FRQGLWLRQV
)URPWKH0DWHULDOWRWKH0HDVXUHPHQWRI6WDQGDUGV
8 Start the Quantification Manager program from the SPECTRA
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folder.
8 Select File > New. Then click the Materials subdirectory.
8 Select Training for Material groups.
8 Select the high-alloy-steel line under Materials.
8 Click Next.
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$ Ensure that the elements shown are selected (if not, select them at this time).
8 Press Next twice.
7 Enter the concentrations from Appendix 3 for these standards.
M84-E00030 -0899 3-3

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7 Right-click the Fe column and format it as Column Balance with two digits. Then do the same with
elements Cr, Ni, and Mn, And format P, S, and Si as Column Balance with three digits.
You do not need to enter the preparation, since the SOLID preparation is already part of the
distribution.
8 Click on the Standard Samples subdirectory.
$ Check that Material and Preparation match the screen below.
8 Check the Short names box.

8 Press Automatically create all Standard Samples.
8 Press Next, and save the modifications.
8 Press Next again to go to Measurement Method.
SOXV
With help from SPECTRA , you will now set up a method for measuring the steel samples.
1
8 Press Launch to start the Measurement Method program .
If you get prompted with the above error message, do not worry. It is OK!
1
The Measurement Method program needs an active Measurement Server Meas3p on your system or on
the TCP/IP Network. It will run also without an SRS attached.
3-4 M84-E00030 -0899
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The Measurement Method supplied with this tutorial already includes the method-specific lines
you will be creating next. But these lines are not yet part of the line library, so they are deleted
from of the method.
8 Press Default line set for current material.
A warning will appear.
8 Press OK to proceed.
8 Press the Elements tab.
M84-E00030 -0899 3-5

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8 Check that all elements involved are pressed.
8 Click the Lines tab.

7 Check the library lines of each element listed in this table and ensure that the corresponding line listed
here is selected in the library. If not selected/listed, remove the selected one and add the line listed in
the next table.
(OHPHQW /LQH
Si KA1-HS-Min
P KA1-HS-Min
S KA1-HR-Min
Cr KA1-HS-Min
Mn KA1-HR-Min
Fe KA1-Maj
Ni KA1-HS-Min
Mo KA1-HS-Min
3-6 M84-E00030 -0899

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8 Select the Modes/Time tab.

7 Select Global parameters for method (which automatically sets Scan, Automatic optimization, Intensity
reduction on, Automatic Dead time control on, Scan range +/-10 times the collimator of the desired
element, 100 sec Measurement time for the scan, 10% Collimator aperture step size).
7 Now select Local parameters for line and select line P.
The following message appears.
8 Press OK.
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7 Change the settings to Measure (Peak) at fixed positions, Measure (Background) at fixed Positions,
Fixed (measuring time) = 10 seconds, Background = Same as Peak.
5HSHDW the procedure for Si.
8 Click on the Parameters tab, and check Vacuum and 34 mm.
M84-E00030 -0899 3-9

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8 Click on the Lines Selection tab.

8 Click on Insert and select method specific lines.
8 Click back on the Lines tab to see what happened.

$ Select any element from the drop down menu, and look at the selected line.
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$ You should note three things:

the line now has an extension /high-alloy-steel
the (c), which means calibrated, is still there
you can see that P is not using global modes/times
8 Click File > Save, and save the method as high-alloy-steel.
8 From the XRF Quantification program, click Nextto get to the Measurement Parameters program.
8 Launch Measurement Parameters.
8 Select the P KA1-HS-Min/high-alloy-steel line.
M84-E00030 -0899 3-11

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3URFHGXUH$ZLWKDQ656DWWDFKHGWR\RXU3&
With an actual SRS attached to your PC, you could now really run a sample and check on the line position
and background position by selecting the Immediate Scan tab.
Identify Lines
option on/off
Theory button.
Reset to theory
position
Position of
sample in
loader Press for new
Bkg Pos and
drag it where
you want it to
be
Bkg box. Drag

no-longer-used
Bkg lines into
this box
8 Press the Immediate Scan tab to display the peak and background positions window. Press the Reset
to Theory button to set the peak position to the theoretical value. Remove the two stored background
(Bkg) positions by dragging them into the Bkg box. Set a new bkg position at 2Theta=86.576.
8 Select any other line.
8 Click Write Changes in Library. And press OK.
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To perform these steps without an SRS, select View > Line positions. The next window appears. Make the
changes by typing.
5HSHDW the procedure for Si KA1-HS-min/high-alloy-steel, setting its background position as follows. Then
click Write Changes in Library and press OK.
Done. You changed the background positions for two lines of the measurement method high-alloy-steel.
3URFHGXUH%IRU6LPXODWLRQ
For those without a steel sample and an SRS, try the following:
8 From Measurement Parameter, select the Scan File tab. Select previously stored SSD file SS_402-1
to check line positions and background positions.
8 Press on the Search Files () button and select the file SS_402-1from the Material Low-Alloy.
8 Remove both existing background positions by dragging each of them to the Bkg waste bin.
M84-E00030 -0899 3-13

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8 Select a new background by pressing on the New Bkg button and dragging the vertical line for the Bkg
position to the 2theta 86.576. Or select View > Positions from the menubar, and change the 2thetas
there.
$ After the change, your screen should look like the next screenshot.
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8 Select the Si KA1-HS-Min/high-alloy-steel line. You will be prompted to write changes to library.
8 Select the Immediate Scan tab, then check Write Changes in Library in the appearing dialog box.
7 Select the View > Positions and change the Bkg position to 105.957 2Theta.
8 Select any other line in the MeasParameters screen.

8 Check Write Changes in Library, and press OK
The Lines for Si KA1-HS-Min/high-alloy-steel and for P-KA1-HS-Min/high-alloy-steel have been

changed to have new background positions different from the original lines used to make these
copies. The associated calibration is NOT LOST due to this difference.
8 Close the MeasParameters program.
You do not need to actually save the library since all changes are written (or not) into the library
whenever you get prompted to decide between Restore and Write.
8 Back in FQuant, click on Next and then Launch (the Loader, if this is not yet activated). Launch from
FQuant (level 1 in Explorer) or from Measurement Standards (level 4).
8 Click on a free loader position.
8 Click on Standards > Import From Database (since we do not want to type in anything).
8 Select high-alloy-steel for Material and Solid for Preparation.Then press Search From Database. All
standards that use this material-preparation combination appear highlighted in the list window.
+LQW: Whenever you are unsure where to place Background positions for a material for some (or all)
elements, you can first make the measurements and then off line select or verify the Background positions
as follows.
Measure the samples for the calibration with the actual select lines as scans overnight. Then go to
Measmethod and use the Scan File option to look at them and check peak and background positions.
M84-E00030 -0899 3-15

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8 Press Import at Current Position to import into the Loader all standards from the highlighted list.
In reality you would now have to place your samples accordingly into the SRS/S4 Loader. (You
can check which sample is on a position by moving the cursor onto that sample.) After the above
measurement, all samples should be flagged OK. If not flagged, you would have to remeasure the
sample.
Since all measurements are already done and stored, we can proceed to Section 2 of this tutorial:
Calibration of High-Alloy-Steel Method.
1RZLWVWLPHIRUDVKRUWEUHDN
3HUIRUPLQJWKH$FWXDO&DOLEUDWLRQRIWKH+LJK$OOR\6WHHO0HWKRG

8 Click on Calibration Method.
8 Select Database and SSD files, then select high-alloy-steel under Material, and Solid under
Preparation.
3-16 M84-E00030 -0899
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8 Press Next.
$ Check that all standards are listed. If not, see Troubleshooting.
8 Press Next to go to Compute Coefficient (the actual calibration screen).

8 Select from the Toolbox the element Mo.
M84-E00030 -0899 3-17

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8 Place and resize the windows for the Graphical Display and the Tabular Display as shown in the
screenshot below.
8 Select the high-alloy-steel line, and press Compute and Refresh.

8 Disable all Standards with Trace (concentration).
8 Make this Line 1.
8 Check if the Std.Dev and the concentrations are the same as shown in the screenshot below.
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8 Click on the Overlay button in the Toolbox. Then press the ?? button for each listed overlay and select
None to remove all overlays from the Overlay window.
$ Compare the Std. Dev. From the toolbox with the screenshot.
3KRVSKRUXV
8 Select element P.
M84-E00030 -0899 3-19

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8 Select the high-alloy-steel line and make it line 1.

8 Select Overlay.
8 Remove all listed overlays, except the one for Mo.
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8 Deselect the fixed option for the Mo overlay.
8 Activate the Offset.

8 Check that you have the same results as shown in the next screen shot.
You might note that the graph looks a little different from the one for Mo. The Standards are
certified to 3 digits. Allowed deviations of the standards are listed in the certificate and match the
obtained results.
1RWH When in one of your calibrations the standards do not fit within their allowed deviation
range, check first on the counting statistic and then on sample preparation (e.g. sample not
polished, fingerprint, dust, cracks etc.)
M84-E00030 -0899 3-21

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6XOIXU
8 Select element S.
8 Select the S KA1-HR-Min/high-alloy line.
8 Make this Line 1.
8 Select the Line Overlay tab (bottom of screen).
8 Remove all overlays, except Mo, and deselect the fix option for Mo.
$ Compare Std Dev to the screenshot below.
3-22 M84-E00030 -0899

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6LOLFLXP
8 Select Si KA1-HS-Min/high-alloy-steel.
8 Make this Line 1.
8 Remove all overlays (since there are none for this material).
8 Disable standards SS_462 and SS_61 in the Tabular Display.
$ Compare results with the screen below.
M84-E00030 -0899 3-23

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&KURPLXP
8 Select element Cr. Then select Cr KA1-HS-Min/high-alloy-steel line, and make this Line 1.
8 Press Compute and Refresh. Then disable all overlays.
0DQJDQHVH
8 Select element Mn. Then select the KA1-HR-Min/high-alloy-steel line, and make this Line 1.
8 Press Compute and Refresh. Then select the Overlay tab and remove all overlays.
8 Query by pressing the ?? button and select Cr KB1. Then set the Overlay type to Calculated.
3-24 M84-E00030 -0899

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,URQ
8 Select the KA1-Maj/high-alloy-steel line.
8 Select Line 1.
M84-E00030 -0899 3-25

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The reason why the calibration for Iron is not as good as for the other elements is that the Fe
concentrations are NOT certified but regarded as balance to 100%.
Some of these standards also contain other elements which were not analyzed (e.g. Niobium or
Cobalt), so the balance is not even absolutely correct.
But, for our case, we can clearly see by the results of the other elements that the Matrix correction
with Iron as balance works perfectly.
1LFNHO
8 Select element Ni. Then select the HS-Min/high-alloy-line,and make it Line 1.
8 Select Computed (Offset).
Now you have calibrated all elements for this material!

In the next section you will see how to document your work!
3-26 M84-E00030 -0899

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'RFXPHQWLQJWKH&DOLEUDWLRQ
%DVLF2SWLRQVLQ3ULQW3UHYLHZ
8 Select any element and press Print Preview.
In print preview mode, you get a view of your page(s) and see the position frames of the activated toolbox
item. In the case below, there are three position frames:
the graphical view.
the tabular display of the standards
the summary of the calibration.
M84-E00030 -0899 3-27

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Whenever the actual contents of a tabular or summary frame do not fit fully inside that page, the
frame will be split automatically to the next page. The graphical display view will not split,
however. It will print altogether on the next page.
8 To move the summary to the second page, click on the summary frame, then click the right mouse
button (as for defining the properties of a selected object), and select Move Summary To Page 2.
8 Press on the Page Selector to go to the next page. Notice that the summary is now on the second
page, but there are also the frames from the graphical display and the standards, which you must now
adjust.
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8 Click on any frame.

8 Click the right mouse button and select Remove All Splits.
$ Now it looks much better:
8 Press on the Page Selector to go to page 1 again.

8 Adjust the graphical frame and the tabular frame with standards such that both of them fit the page.
$ Note that you can change the setting for how many columns to display in the tabular frame. Look more
closely at the standard display (a few screens back) and notice that 11 columns are displayed. Now
look ahead 3 screens and notice that only 8 columns are displayed.
M84-E00030 -0899 3-29

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8 Click on the Standards tab at the bottom of the screen and you are back in the usual display for the
standards.
8 Press the Glasses button on the right. The Column Selection pop-up window appears. In this window,
you see on the left the headings of all available columns that are not displayed. On the right, you can
see headings of all columns that are displayed.
8 Select columns Gross Intensity, Net Intensity, and Background, and press Remove. They will transfer
from the right window to the left window.
8 Click on any column heading on the right and change the sequence by clicking the Move Up or Move
Down button.
8 Click on Standard name. Then in the Width field, enter a number that corresponds to the width of the
column you would like in the printout. Try to change it to 120. Then press OK.
8 Click on the Print Preview tab at the bottom of your screen and notice the change to 8 columns (with
greater width) in the tabular display.
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This formatting applies to the entire calibration. The format will be automatically stored with the calibration
once you save it.
8 Press the Print button (circled above) to print the active element.
$ When finished printing, the program returns you to the main FQuant display window.
8 Select the next element from the toolbox and press Print to print the calibration for that element.
5HSHDW the procedure for all elements.
8 Save your work with the filename: high-alloy-steel.
M84-E00030 -0899 3-31

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$GYDQFHG2SWLRQVLQWKH3ULQW3UHYLHZ
Windows NT allows you to freely exchange information between any Windows-based software by
transferring an object via the clipboard. All objects displayed in the Print Preview can be transferred (for
example to Winword) by selecting the desired object and clicking on the WMF Clipboard Copy button.
(WMF stands for Windows Meta File and is a standard interchange format for Microsoft certified products.)
8 Select the Graphical Display in the Print Preview.
8 Press the WMF Clipboard Copy button.
8 Open Winword (or your word processor).

8 Select Paste in that program. And there it is for you to resize.
25
24
900
23
22
21
XRF Concentration (%)
800
Intensity (KCps)
20
19
700 18
17
16
600
15
14
500 13
12
450
12 20
Concentration (%)
Int. net Int. corrected
3-32 M84-E00030 -0899

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8 You can do the same with the frame containing the standards, this time from the tabular display.
Num Standard namChemical C XRF concen Absolute de Relative dev Count. stat. re Count. stat
1 SS_261 17.400 17.130 -0.270 -1.5490 0.1678 1.2292
2 SS_461 15.200 15.182 -0.018 -0.1193 0.1741 1.1909
3 SS_462 12.350 12.560 0.210 1.7011 0.1903 1.0918
4 SS_463 18.300 18.339 0.039 0.2124 0.1618 1.2727
5 SS_465 18.000 17.911 -0.089 -0.4962 0.1634 1.2608
6 SS_466 17.600 17.618 0.018 0.1050 0.1683 1.2242
7 SS_61 15.200 15.204 0.004 0.0261 0.1737 1.1885
8 SS_63 18.700 18.779 0.079 0.4230 0.1604 1.2867
9 SS_64 25.600 25.649 0.049 0.1933 0.1435 1.4298
8 Or for the Summary. This can also be achieved by going to the Summary window, selecting the text
you want to copy, and then pressing copy.
Abridged calibration data for line Cr KA1-HS-Min/high-alloy-steel

Instrument# 273, Mask: 34 mm, Mode: Vacuum, 50 kV , 81 mA, Filter: None
Crystal (nominal): 2d = 4.026 Ao, Collimator aperture (nominal) = 0.15 degrees
Detector: flow counter LLD = 21, ULD = 129 % of nominal peak.
Adjusted peak at 69.363 degrees 2-theta, Wavelength = 2.2897 Ao
Background 1 at 68.727 degrees 2-theta, weight 1
Absorption correction: Variable alphas
Intensity model: net intensity
Minimization target: absolute error, 9 standards from 12.35 % to 25.60 %, standard deviation:
0.13 %
Slope: 0.03258 %/KCps / Sensitivity: 30.7 KCps/% (Adjustable by regression)
Quadratic correction: +2.397e-005
M84-E00030 -0899 3-33

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7HVWLQJWKH&DOLEUDWLRQ
After you have finished the calibration, it is always a good idea to test the calibration with known samples
of the same material, especially if you used empirical calibration corrections or fixed alphas, because
testing might show you potential or actual problems.
To test, we will evaluate one of our standards with the XRF Interactive Evaluation Program and print the
results to compare them with the certified results. As a good exercise, you can do that for the rest of the
standards as well:
8 Close the Quantification Editor and save your work.
8 Start the XRF Interactive Evaluation Program and select File > Next SSD. The following screen
appears.
8 Press the Search () button and open your SPECTRA directory. From there, open the
SOXV
directory..\Libraries\Materials\High-Alloy-Steel\Solid\, and from there open the file SS_462. The

following window displays.
8 Check that settings are as shown. Press OK. The interactive evaluation screen appears. Since we
defined iron in our program as Balance, the result under Total will be 100.0%.
3-34 M84-E00030 -0899
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8 Double-click on Iron. The Compound Property window will appear.

$ In the Compound Property window, you can switch to Matrix, a Fixed (value), or to the calibrated Line.
(In other cases, you could switch to other measured and calibrated lines for the same element, e.g.
Standardless Analysis.)
8 Tick the Fe-KA1-Maj/high-alloy-steel option (the calibrated iron concentration), press OK, and notice
what happens. By default, Fe in our case is defined as to 100 (matrix) but we can see what
happens if we use the actual measured intensity for the calibration.
M84-E00030 -0899 3-35

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8 Click on the Mn line. Then press the View button (circled) and select Line 1. A View Line (graphical
display) appears for the individual line, where you can get information of the actual lower limit of
detection based on the actual sample and actual scan conditions.
Active Line in the

same color as the
header
Info for the

displayed line
Updates the
window
3-36 M84-E00030 -0899

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Here you can also select and copy the contents of the Graphical window to the clipboard (by
pressing Clipboard) and paste them into another program.
8 Press the Select button, select S, and press Update in the View Line 1 window. The graphical display
changes to show details for element S.
Display of lines
near the cursor
8 Print the results by pressing the Print Result button in the interactive evaluation window.
5HSHDW this procedure for some more standards, and also try to change the sequence of the elements in
the prinout.
M84-E00030 -0899 3-37

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6HWWLQJXSD5HFDOLEUDWLRQ
This section covers the following:
Removing existing recalibration settings for the high-alloy-steel lines
Setting up the new recalibration samples and lines
Evaluating the recalibration samples
Checking the recalibration
Making a loader definition file for an easy recalibration
Measuring the recalibration samples
The best system for recalibration would be to link all custom-made lines to the glass samples and the
recalibration measurement method associated with these glass samples. So it would be possible to
recalibrate all your used methods with one set of glass samples. Using one set increases the flexibility and
leads to better productivity. All your programs will then be up to date after a recalibration.
8 Close all open SPECTRA
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programs, except the Measurement Server.
8 Select the Measurement Parameters program.
8 Select the measurement method High-Alloy-Steel.
8 Select the Cr /high-alloy-steel line.
8 Select the Global Recalibration tab.
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$ Note the following from the screenshot above:

The custom line retained the global settings and thus the recalibration.
The line is recalibrated using the RECAL-SQ1 sample and the Mn KA1-HS-Min line.
Reference is made to the master spectrometer (273) used and measurements made on your
system or in this case of the system 309.
Entries should appear for all of your masks and modes (helium, vacuum) with the intensities and
the date when your system measured the reference samples.
8 Select the Fe-KA1-Maj/high-alloy-steel line.

8 Press the Delete button to remove the actual reference sample.
8 Press OK to confirm.
8 Enter High-Alloy-RECAL1 in the Reference Sample field, and press New.
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8 Select the Fe KA1-Maj/high-alloy-steelline from the drop down window at the reference line.
Though we have selected this line for simplicity, you could select from the many other lines.
All lines shown correspond to the same crystal and use the same settings for the counters as the
Fe KA1-Maj line (except for Peak and BKG positions).
8 Select Mn as next element, and write the changes to the library when prompted to do so.
8 Click on the Global Recalibration tab.
8 Press Delete to remove the original reference sample.
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8 Enter High-Alloy-Recal2 as reference sample, and choose Mn KA1-HR-Min/high-alloy-steel as

reference line.
8 Select Si and delete the original reference sample.

8 Select High-Alloy-Recal1 as reference sample, and the Si high-alloy-steel line as reference line.
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8 Select element P.
8 Press Delete to remove the original reference sample.
8 Enter High-Alloy-RECAL1 as reference and, again, the Si high-alloy-steel line as reference line.
5HSHDW the procedure for all other elements of the High-Alloy-Steel Method, according to the table below,
and check that they are set accordingly. Note that we will be recalibrating the P line with the same line as
we recalibrate Si since they have the same setting.
Line Reference Sample Reference Line

Fe High-Alloy-Recal1 Fe KA1-Maj/high-alloy-steel
Si High-Alloy-Recal1 Si KA1-HS.Min/high-alloy-steel
P High-Alloy-Recal1 Si KA1-HS.Min/high-alloy-steel
S High-Alloy-Recal1 S KA1-HS-Min/high-alloy-steel
Cr High-Alloy-Recal2 Cr KA1-HS-Min/high-alloy-steel
Mn High-Alloy-Recal2 Mn KA1-HS-Min/high-alloy-steel
Mo High-Alloy-Recal3 Mo KA1-HS-Min/high-alloy-steel
Ni High-Alloy-Recal3 Mo KA1-HS-Min/high-alloy-steel
Make sure to use only one reference sample and to select the correct line. Write the changes to the library
when prompted.
8 Once you have set all elements, close the Measurement Parametersprogram.
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8 Open the Measurement Method program.
8 Select File > New.
8 Click the Elements tab and select elements Fe, S, and Si.
8 Click the Lines tab and select the high alloy steel lines for each of the elements.
8 Click the Modes/Time tab, and set Measure at Fixed Positions (for peak and background
measurements), Fixed (for measuring time), 100 sec (for time of peak), and Same as Peak (for
background).
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8 Tick Local parameters for line, select the Fe line, and set Time per Range to 100 seconds.
$ Compare your settings with the screenshot.

8 Select the Parameters tab.
8 Set Vacuum and 34mm. Then Save As the Method as High-Alloy-Recal1 into the
Measurementmethods\Recalibration directory.
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7 Create the measurement methods high-alloy-recal2 with Cr, Mn as scan measurements and high-
alloy-recal3 with Mo and Ni.
$ At this point, you should have the three measurement methods stored in the directory
MeasMethods\Recalibration.
$ Locate the SSD files High-alloy-recal1 through 4 using the Explorer to ensure that you have saved
them.
8 Start the Autoevaluation program from the SPECTRA

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folder.
8 Select the high-alloy-recal1.ssd file as sample data file, the high-alloy-recal1.mm as calibration
(measurement method), and Solid as preparation. Then press OK.
5HSHDW the procedure for the other two samples respectively.

M84-E00030 -0899 3-45
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8 Close the Autoevaluation program.

8 Open Measurement Parameters.
8 Under File, open the high-alloy-steel method. Select the P KA1 line and click the Global Recalibration
tab.For all lines, you should now see an entry like that circled.
You have just performed a recalibration using previously measured samples.

With a real spectrometer, you just need to measure the sample with the name given (high-alloy-
recal1) in the reference sample section and the method that uses the right lines.
Automatically, the recalibration will be entered in your line library.
1RWH: For a routine program, it is good practice to set up a customized window for the loader (as you will
do in the next section), so that no typing mismatches endanger the recalibration.
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8 Find and start the Sample-def program (see also Chapter 10 of the Reference Manual for details) The
following window appears.
8 Press the Load button and select file RECAL34.def to load the file into the program. Columns List data
appears.
8 Select Sample (in the Columns List). Then click on Fill with wildcards (under Automatic value) and
enter the following string: %Measurement Methods Path%\Recalibration\high-Alloy-recal*.mm
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7 Repeat the procedure for Method, Sample-ID, and SSD-File, entering the appropriate string that
follows.
METHOD %Measurement Methods Path%\Recalibration\#Sample
Sample-ID #sample
SSD-file %Measurement Methods Path%\Recalibration\#Sample
8 Save the new definition as High-Alloy-Recal34.def, and exit the program.
8 Start the Loader.

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8 Select Samples > Sample Definition and select the .def file that you just created a moment ago. Then
try to enter the three recalibration samples by pressing the Insert Sample button (circled).
When the measurement is finished, the recalibration is automatically written into your line library!
M84-E00030 -0899 3-49

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8VLQJWKH'XPS66'
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Use DumpSSD to get an ASCII file, which shows what SPECTRA actually measured.
8 Start the DumpSSD program. The DumpSSD window appears.
8 Under Input (SSD) file, select an SSD file that you want to dump.
8 Under Text out, select a location where you want to place the ASCII file.
8 Press Dump button.
8 Open the ASCII text file with Notepad or Wordpad and look for the following:
Example output:
Dump of file D:\AS\Training\xrf\SPECplus\Libraries\Materials\High-Alloy-Steel\Solid\SS_465.ssd
Measured under Vacuum
Instrument serial number: 273
Sample Id: SS_465
Range # 1
Channel: 3 Crystal: LiF200
Collimator: 0.15 degr. Mask: 34 mm
Tube : 60 kV 67 mA Filter: none
FC: 58.3% - 120.8% SC: 54.2% - 145.8%
Steps: 195 Size: 0.016 Time: 0.530 s
From: 18.700 to 21.804 2Theta
Range # 2
FC: 33.3% - 129.2% SC: 50.0% - 150.0%
Steps: 195 Size: 0.016 Time: 0.530 s
From: 47.100 to 50.204 2Theta
Range # 3
FC: 25.0% - 300.0% SC: 25.0% - 300.0%
Steps: 195 Size: 0.016 Time: 0.530 s
From: 84.100 to 87.204 2Theta
Range # 4
FC: 20.8% - 129.2%
Steps: 195 Size: 0.016 Time: 0.530 s
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From: 93.600 to 96.704 2Theta

Range # 5
FC: 20.8% - 129.2%
Steps: 195 Size: 0.016 Time: 0.530 s
From: 67.800 to 70.904 2Theta
Range # 6
Channel: 1 Crystal: PET
FC: 54.2% - 145.8%
Steps: 195 Size: 0.016 Time: 0.530 s
From: 74.200 to 77.304 2Theta
Range # 7
FC: 54.2% - 145.8%
No scan in range
Peak: P KA1
Time: 10.00 s 2Theta: 89.500 Rate: 1.5382 KCps
Bkg # 1 2Theta 86.576 Coeff 1.000 Rate 0.3204 KCps
Range # 8
FC: 54.2% - 145.8%
No scan in range
Peak: Si KA1
Time: 10.00 s 2Theta: 109.124 Rate: 8.7817 KCps
Bkg # 1 2Theta 105.957 Coeff 1.000 Rate 0.3854 KCps
M84-E00030 -0899 3-51

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(UUDWD
$ Check on the sample concentrations for SS_261 and ensure that they are correct. If wrong, change if
in the Standard Material section.
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SPECTRA Tutorial Manual Tutorial in XRF Standardless Measurements
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8VLQJ63(&75$SOXV
Tutorial in XRF Standardless Measurements Using SPECTRAplus .......................................................... 4-1
What is Standardless Analysis all about ?.................................................................................................. 4-2
How to make a measure a sample using the predefined methods............................................................. 4-4
Evaluating samples using the XRF Evaluation program ............................................................................ 4-7
Evaluating solid samples (Metals) .......................................................................................................... 4-7

Evaluating the STG Glass sample ........................................................................................................ 4-13
Evaluating samples prepared as pressed pelltes with binder............................................................... 4-16
Pressed Pellet with Boric Acid (Preparation already in database) ................................................... 4-16
Scaling / Normalizing Concentrations ............................................................................................... 4-17
Defining the sequence of the printout ............................................................................................... 4-18
Entering non measured Elements..................................................................................................... 4-19
Evaluation of samples prepared as fused bead.................................................................................... 4-21
Entering a new preapration in the database ..................................................................................... 4-21
Customizing the output via the Clipboard ......................................................................................... 4-27
Create your own Standardless Measurement Method ............................................................................. 4-29
Compton and Rayleigh Ratios in Standardless Analysis.......................................................................... 4-32
Measurement of Rhodium Compton Line ............................................................................................. 4-33

Calibration of Rhodium Compton Line .................................................................................................. 4-34
Examples .................................................................................................................................................. 4-35
Effects of different matrices on the calculated Compton Intensities ..................................................... 4-35

Influence of Thickness and Density of the sample ............................................................................... 4-35
4-1
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Tutorial in XRF Standardless Measurements SPECTRA Tutorial Manual
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Imagine you would get a totally unknwon sample (e.g. a brown powder).
Someone wants to know from you very quickly the approx compostion of that sample.
Befor you can measure that sample you would have to:
Get an idea of the composition
Find appropriate standards
Choose a method for the preparation of standrdss and unknown
Set up measuring conditions
Measure standards
Calibrate (i.e. determine sensitivity, line overlaps, and matrix correction).
Measure the sample
Evaluate the sample
That adds up to at least one or two days of work !Most of the times you will not even get the idea of the
composition since you might not have other complementary methods (XRD, IR, Raman, AAS) at hand. Or
you would have to make wet chemical assays for qualitative analysis first.
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LQOHVVWKDQPLQXWHV
X-ray fluorescence Analysis is never standardless since the system compares mesured intensities with a
curve based on previously measured standards.
Bruker-axs measured 300 different standards (Metals, Glasses, Ceramics, Rocks, Minerals, Oils,
Polymers etc.) on the Master spectrometer in the application laboratory with universal measurement
conditions.
A calibration was made and stored in the line library. The calibration is then transferred to the customers
XRF system with the help of three glass samples. Included in the Line Library are Calibrations from F to U,
valid from ppm to 100% ranges.
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With this calibration you can analyse totally unknown samples for all elements from O to U with you
standard SRS3400 or S4Explorer.
Just prepare the sample and measure it with a predefined measurement method our build your own:
4-2
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Since the calibrations are covering the entire concentration range and have to be usable for all types of
material the typical results are accurate in the range of max. +/- 10% relative.
For trace elements there might be a slightly larger deviation depending on the actual counting time used.
You can easily improove the standardless calibration by adding your materials or make a specialized
program for a specific matrix:
Bruker-axs offers you specialized Standardless Calibrations for:
Oils = OilQuant
Igneous Rocks and Sediments = GeoQuant fused
Copper based alloys=CopperQuant
Steels=SteelQuant based on NIST and BCS Standards
Or ask your Bruker-axs application scientists to solve your analytical question
The User-groups also exchange calibrations via WWWeb or Email.
4-3
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In this section you will be shown which standardless methods are part of the Spectraplus distribiution and
how to use them:
All measurement methods which you can use in Spectraplus are to be found in the directory
Measmethods which is a subdirectory of Libraries in the Spectraplus folder.
In order to use the predfined methods you just need to perform the following steps
Check if the Measurement server is active on your system (or if your system is configured
for network operation, that the measurement server is running on the system attached to the
SRS or S4)
Activate the Loader from the Spectraplus folder
The next step is to choose make sure we have the right setup for the sample input screen
which you can also custom tailor to your needs. Please refer to the section SAMPLEDEF in
your reference manual for details.
Click on Sample
Click on Sample Definition
Select the Routine.def file (this is a allround setup for your sample input)
Click on an empty loader position where you want to place the sample
Press the Insert Sample button or select Sample/EDIT

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Enter the sample name
Click on Measmethod and select a method
The predefined standardless methods all begin with st-less and use the standard 34mm
sample masks and will run as scan measurements.
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St-less-HR-He Standardless using High Resolution Lines HELIUM
St-less-HR-Vac Standardless using High Resolution Lines Vacuum
St-Less-HS-He Standardless using High Sensitivity Lines HELIUM
St-Less-HS-Vac Standardless using High-Sensitivity Lines Vacuum
Select St-less-HS-Vac for your first try
Select Bulk for sample preparation
Select Solid as Preparation
Now place the STG Glass sample at that loader position and make sure you use a 34mm
sample cup and that the sample is not wobbeling around (You might use the practical
BrukerAXS distance rings (Order no.: 7KP--------).
Press Create samples

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Press the Send Selected Samples button
The Measurement will start, the sample will be moved into the system.
In the window just below the Loader display you will be prompted with the list of all active
samples and their estimated times as well as the estimated end time.
In approx 20 minutes the sample will be ready for your interactive evaluation
4-6
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In this section the XRF interactive evaluation program is introduced.
The following options will be covered:
Opening an exsisting (done) measurement
Evaluating previously measured samples with the standardless calibration using different
preparations techniques.
Evaluating of the sample measurement started in the second section (Hwo to test if the
standardless calibration is working)
Printing and documenting of measurements
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In this sub section you are going to evaluate a steel sample, which was measured previously on the
MasterSRS.
Open XRF Evaluation form the Spectraplus folder
Select File/NEXT SSD
Navigate to the tutorial directory by pressing the button
Select the sample:JSS610-7
Press Open
Select the Method ST-LESS-HS-VAC
Select Solid as preparation
Select Elements
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Press OK
Tick AutoUpdate
Click on a line to inspect it
Select View Line1
Press Update in the View Line Window
4-8
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In the view line window you see three panes:
A graphical pane showing a Zoom Area around the lines
A pane listing all the spectral lines which are to be found at bthe cursor position, when moving
the mouse pointer in the graphical pane.
A line list of up to three measured lines of that element in the actual scan.
Three tick boxes let you modify the graphical pane:
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Peak only will display just the marker for the current element
Zoom Peak will only display a zoom around the current peak
Five buttons underneath the list:
Clipboard moves the actual list pane into the Windows Clipboard:
View Line (1): JSS610-7 [024] (Jss610-7.ssd )
Name Position Peak Backgrnd. L.L.D. Overlaid

V KA1-HS-Min 76.928 81.755 0.477 92 ppm 0.003
Metafile copys the graphical view to the clipboard

V KA1-HS-Min
50
40
30
20
10
5.256 5.26 5.27 5.28 5.29
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Select will select the highlighted line for viewing
Update will display the activated line form the main window in the view line window
View brings you to the qualtiative view of the scan ranges
Select Lu as active element in the main window
Press Update on the view Line window
In this case we see a typical overlay:
Lu LA1 HS line is at the same 2theta as the Co KB1 line:
Click on the Lu LB1-HS Line
Again this is overlaid by W
Check on Co and W
You are now sure that both Co and W are present in a notable quantity and the Lu signal is
due to an overlay.
Click back on Lu and press the button to set the element to 0
Check on the main window: Lu is not longer displayed and a new matrix correction was
made
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Repeat the procedure for Au and Hg (Au overlayed with Rh Compton, Hg overlayed with W)
Click on Fe
Since the sample is a steel sample we define Fe as matrix:
In other words we will not be using the measured value, but a calculated concentration:
Applying this we make sure that:
We are not introducing more analytical errors than necessary
Use the usual procedure for steels (since the Fe values are rarely certified)
Sum will be 100%
Check Matrix
Press OK
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Press Print Results Button to get the results printed on the printer.
See Troubleshooting Section if you do not get a printout.
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Select File / Next SSD
Select the Browse Button
Navigate to Specplus\Libraries\Measmethods\Recalibration
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Select the RECAL-STG-VAC file
Press Open
Press Open again
Check if Method is ST-LESS-HS-VAC
Check if preparation is SOLID
Click on OXIDES
Click on OK
Click on SiO2 and select Matrix

4-14
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Compare with the next table:

Compound Collimatormasks 23-37mm Collimatormask 08mm (vacuum)
Na2O 14,1 - 15,7 13 - 16
MgO 0,04 - 0,12 0,04 - 0,14
Al2O3 0,83 - 1,23 0,80 - 1,35
SiO2 67,0 - 71,0 66 - 71
SO3 0,50 - 0,85 0,50 - 0,87
Cl 0,20 - 0,38 0,20 - 0,38
K2O 4,90 - 5,25 4,8 - 5,3
CaO 5,05 - 5,50 5,0 - 5,5
TiO2 0,025 - 0,038 0,025 - 0,065
Fe2O3 0,040 - 0,090 0,04 - 0,10
SrO 1,75 - 2,35 1,75 - 2,50
Sb2O3 0,45 - 0,85 0,45 - 0,85
Please take into consideration that the check sample is a Setup-sample whose
concentrations are known and reproduced roughly. So the concentration ranges are mainly
determined by the samples. A comparison between different modes and between result in
the Bruker-AXS test field and on-site shows lower deviations. Nevertheless the performance
of a standardless method can be checked that way.
If your values are way off refer to the section recalibration of the line library in the tutorial
manual.
4-15
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Press Print Results.
Press Database to transfer the results into your measurement database
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The difference between the previous evaluations and this are that yoy have to select an adequate
preparation first to prepare the sample and secondly this type of preparation should be entered also into
the database so you can use it in XRF Evaluation.
The sample to be evaluated was prepared using 5g of dried sample material and 1g of Boric Acid. The
binder was mixed thouroughly with the sample and it was pressed to 40mm disk.
The preparation of pressed pellets with Boric Acid is already included in the database of Spectraplus.
Select File/Next SSD
Navigate to the tutorial directory by pressing the button
Select the sample:CC209-H3BO3
Press Open twice
Select ST-LESS-HS-VAC as method
Select BoricAcid as preparation
Select Oxides
Enter the Original Material Weight :5g
Enter the Binder Weight: 1g
Check Diameter 4cm
Check Mass 6g
Press OK
4-16
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Look at the displayed results:
Since only one line was measured per element we can not compare the concentrations from
different lines of the same element.
But we should always check for some undetected Overlays:
Select View Line1 from the View Menu or press the View Line1 button
Click on the topmost element and press update on the view line 1 window
Check all elements
Mn is reported as MnO in this viewSuppose you want it reported as Mn2O3 ?
Changing the compounds:
Double-click on the element/compound ( here MnO)
Modify MnO to Mn2O3
Press OK
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To get the sum to a 100% press the scale button
4-17
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There are the several ways you can define the order of the compounds/elements in the printout:
$OSDEHWLFDOO\E\FRPSRXQGIRUPXOD
Click on the column header Compound Formula
A small arrow will appear facing up or down symbolizing the sort order
Clicking again on the column header will toggle the order from A-Z to Z-A
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Click on the compound header nZ
Toggle the order by clicking again on the column header

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Click on the compound header concentration
Toggle the order by clicking again on the column header

4-18
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A Userdefined order can be selected by double-clciking on each element and entering the
Line Order number:
You can also choose to make the element non printable, removing the tick in the box after
Element is printable !
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This sample contains some Carbonate (CO3) which is determined using the LOI.
The sample was reported to have an LoI of 0.21 weight %.
Press Insert Compund Button
Enter CO2 as a compound
Enter 0.21 as concentration
Select OK
Press the Scale/Normalize button
4-19
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Press Print Results
Compare the results to the table at the end of the section
4-20
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In this example we used a new preparation which is not yet in the database:The sample was
dried nd then fused using 1.5002 of original sample and 7.5 g of a flux calles A1000.
The flux consists purely of Lithiumtetraborate.
In order to enter the preparation into the database we need to:
Enter the flux A1000 into the database
Make a preparation containing this flux in the same database
Both actions have to be performed in the XRF Quantification Program
Select Fquant from the Spectraplus folder
Press File/New
Click on Preparation icon on the left hand side of the Quantification window
Enter Training-A1000 as preparation name in the preparation window
Press the New button
4-21
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Select fused bead as method
Enter Lithiumtetraborate as Additive
Select 1.5 g as Value for original Material, 7.5 g as value for the additive
Select Default values for sample specific input
4-22
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Press Next
Press Yes to save it
Click on diameter and select 4 cm
Click on weight and select 9g
Tick Default values for sample specific input
4-23
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Press Next
Press Yes to save it
With this procedure you entered this preparation into the database (fluo.mdb). All other
programs retrieve the preparations from there.
Close Fquant without saving.
Activate XRF Evaluation
Select File/Next SSD
Select the sample C209-a1000 from the tutorial directory
Press Open twice
4-24
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Select ST-LESS-HS-VAC as preparation
Select Preparation Training-A1000
Press OK
4-25
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Make sure that AUTO Update is ticked
Otherwise you would have to press an recalculate every time you change something.
Press Scale/Normalize
Enter an LOI of 0.21 with CO2 as lost compound
Press Scale/Normalize
4-26
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The button clipboard copy will move the entire view of the area where the results and lines are
displayed to the windows clipboard.
To define or customize this view you use the button
Press the Customize button
4-27
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Decide which columns you want to see and transfer to the clipboard:
Remove columns you do not want by clicking on them and press the remove button
To change the sequence click on the column you want to move and either press the MOVE UP
or the MOVE DOWN button.
Press OK when ready
Mark all lines (with the mouse)
Press ClipboardCopy
Open up EXCEL
Press Paste in EXCEL
4-28
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In the Methods used up to now, all elements were included which can be measured. The
average time of a 10 sec per range HS scan is 20 minutes.
To scale down the time and to increase accuracy at the same time you might want to
measure just the 10 or 11 most likely elements:
You get a plastic sample and the question if there is Cd, Pb, Cr, Sb and As present.
You do also not know if there are Flame retardants present (Br) and if it is possibly PVC (so
Cl has to be there)
The elements we would like to measure are Cl, Br, Cd, Pb,Cr,Sb, As and the Compton Peak
for matrix correction. Included could be Ti if you also want to know if the Polymer is filled
Select Measmethods from the Spectraplus folder
Press New
Select the Line Selection Tab
Tick two line Element
Select Compton
Press Reinitialize Button
Select the Elements Tab
Select Cd,Pb,Cr,Sb,As,Br,Cl and Ti
Select the Lines Tab
Check the selected lines:
Make sure to have always the HS and the HR line of the selected Element
For As (expecting Pb you should choose KB and for Pb LB1
4-29
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Press Modes and Time Tab
Make a mixed method, where the background is measured as scan and the peak as fixed
position:
4-30
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The Optimized Tab is for the Peak Measurement: select 1% and 30 sec
For the scan select 30s and 10 times the collimatore aperture.
Select the Parameters for that sampel using the Parameters TAB
Save the method and use it.
4-31
SOXV
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Intensity Graphite
[kcps] LiF 100
KA-Compton
Compton
KB-Compton
2 Theta
15,6 17,5
Rh KB1 Rh KA1
Rayleigh - scattering
The non measured elements impact in the quality of the matrix correction since Hydrogen , carbon and
oxygen greatly influence the matrix correction.
Analysis of these elements is difficult or impossible by means of XRF:H, Li cannot be measured.
The characteristic radiation of B,C,N and O is absorbed by any supporting foil material or the He in
Liquids, wet samples or loose powders.Meticulous lengthy sample preparation is required for solid
samples where these elements are of interest.
How to determine then these important non-measured elements ?
By compound definition a chemical fomula like SiO2 or CaCO3 allows the program to calculate
carbon or oxygen using the measured concentrations of Si and Ca.
By balance to 100%: - a chemical can be defined as a balance to 100, e.g. CH2 in oil or
polymers or H2O in water where C(matrix) = 100 % - C(measured elements)
The concentrations are calculated itteratively when using these options, recalculating the matrix correction
for each step.
How to check if our assumptions for the matrix are correct ?
4-32
SOXV
Measurement of the Compton Peaks:
i.e. the inelastically scattered characterstic tube lines Rh KA1,2 and Rh KB1 and comparsion with the
calculated theoretical intensities:
The ratio displayed will show a value around 1 (+/- 10% rel) when the matrix correction is resonable.
Why does this work ?
The intensity of the compton peaks is very sensitive to the concentrations of the elements from H to O.
These peaks can be measured on all samples.Theoretical Intensities can be predicted for the Compton
Peaks based on the concentrations of the light elements.
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4-37

Spectra Plus Tutorial Manual M84-E00030 PDF

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Spectra Plus Tutorial Manual M84-E00030 PDF

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BRUKER ADVANCED X-RAY SOLUTIONS

8 Start the XRF Quantification (FQuant) program from the SPECTRA

M84-E00030 -0899 1-1

8 Press Next. The Orientation screen appears.

1-2 M84-E00030 -0899

M84-E00030 -0899 1-3

8 Press Next. The following message appears.

1-4 M84-E00030 -0899

8 Select 4 cm diameter, 100g, and Fixed values for all samples.

M84-E00030 -0899 1-5

8 Press Next three times. The Standard Samples screen appears.

8 Press the Wizard button (circled above).

8 Be sure to use short names, and select OK to all.

1-6 M84-E00030 -0899

8 Press on the Elements tab to display all elements.

1-8 M84-E00030 -0899

8 Press the Lines tab to check the choice SPECTRA

M84-E00030 -0899 1-9

1-10 M84-E00030 -0899

8 Click the Modes/Time Tab.

M84-E00030 -0899 1-11

1-12 M84-E00030 -0899

8 Press Yes to save the file (method).

M84-E00030 -0899 1-13

8 Click on an empty position in the Loader.

M84-E00030 -0899 1-15

8 Press Uncheck missing stds (standards).

1-16 M84-E00030 -0899

Youve arrived at the actual calibration screen!

M84-E00030 -0899 1-17

1-18 M84-E00030 -0899

M84-E00030 -0899 1-19

1-20 M84-E00030 -0899

The Overlaybutton displays the overlay menu.

The Alphasbutton displays the settings for the computation of alphas.

M84-E00030 -0899 1-21

8 Select the Tabular Display button.

1-22 M84-E00030 -0899

M84-E00030 -0899 1-23

8 Select 1 as a line sequence.

1-24 M84-E00030 -0899

8 Press the Active button (deactivate Offset).

8 Select 1 as a line sequence.

M84-E00030 -0899 1-25

This is the best that we can improve these standards.

1-26 M84-E00030 -0899

8 Select 1 as a line sequence.

M84-E00030 -0899 1-27

8 Select 1 as a line sequence.

1-28 M84-E00030 -0899

8 Click the Overlaysbutton.

M84-E00030 -0899 1-29

1-30 M84-E00030 -0899

M84-E00030 -0899 1-31

&RQJUDWXODWLRQV! You just corrected for a very nasty

1-32 M84-E00030 -0899

M84-E00030 -0899 1-33

you run the standardless recalibration procedure.

1-34 M84-E00030 -0899

8 Press the Create Samples button.

M84-E00030 -0899 1-35

In this subsection you will:

8 Double-click the Results Manager icon in the SPECTRA

8 Select ORZDOOR\VWHHO in the Measurement Methodline (first data field).