nist dtsa-ii guide - university of oregonepmalab.uoregon.edu/workshop3/nist dtsa-ii_guide.pdfnist...
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NIST DTSA-II (“Son of DTSA”):Step-by-Step
Dale E. Newbury (grateful user)National Institute of Standards and Technology
Gaithersburg, MD 20899-8370
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NIST-NIH Desktop Spectrum Analyzer (DTSA)
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Photon Energy (keV)
Log
Inte
nsity
FeKα
FeKβ
CaKα
CaKβ
SiKα,β
AlKα,β
FeL
OK
CaL
NIST Glass K411E0 = 20keVInside specimenAfter specimen absorptionAfter EDS window absorptionAfter EDS broadening (145 eV)
Spectral Simulation with DTSA
For 16 years, I have heard: “When will you have DTSA for the pc?”
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NIST DTSA-II• Created by Nicholas Ritchie of NIST ([email protected]),
inspired by NIST-NIH Desktop Spectrum Analyzer (DTSA) invented1990-92 by Chuck Fiori (NIH and NIST) and Carol Swyt-Thomas (NIH),and then further developed by Carol and Bob Myklebust (NIST).
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NIST DTSA-II• Created by Nicholas Ritchie of NIST ([email protected]),
inspired by NIST-NIH Desktop Spectrum Analyzer (DTSA) invented1990-92 by Chuck Fiori (NIH and NIST) and Carol Swyt-Thomas (NIH),and then further developed by Carol and Bob Myklebust (NIST).
• DTSA ran only on Macintosh, and then only up to system 10. (NewMacs won’t run DTSA) A painful question heard many, many times:When will you have DTSA for the pc? DTSA-II is the long awaitedanswer!!
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NIST DTSA-II• Created by Nicholas Ritchie of NIST ([email protected]),
inspired by NIST-NIH Desktop Spectrum Analyzer (DTSA) invented1990-92 by Chuck Fiori (NIH and NIST) and Carol Swyt-Thomas (NIH),and then further developed by Carol and Bob Myklebust (NIST).
• DTSA ran only on Macintosh, and then only up to system 9. (NewMacs won’t run DTSA) A painful question heard many, many times:When will you have DTSA for the pc? DTSA-II is the long awaitedanswer!!
• DTSA-II is written in Java and operates on Mac, pc, UNIX, Linux.
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NIST DTSA-II• Created by Nicholas Ritchie of NIST ([email protected]),
inspired by NIST-NIH Desktop Spectrum Analyzer (DTSA) invented1990-92 by Chuck Fiori (NIH and NIST) and Carol Swyt-Thomas (NIH),and then further developed by Carol and Bob Myklebust (NIST).
• DTSA ran only on Macintosh, and then only up to system 10. (NewMacs won’t run DTSA) A painful question heard many, many times:When will you have DTSA for the pc? DTSA-II is the long awaitedanswer!!
• DTSA-II is written in Java and operates on Mac, pc, UNIX, Linux.• DTSA-II is NOT DTSA! Nicholas started from scratch and used DTSA
as a guide to develop DTSA-II.
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NIST DTSA-II• Created by Nicholas Ritchie of NIST ([email protected]),
inspired by NIST-NIH Desktop Spectrum Analyzer (DTSA) invented1990-92 by Chuck Fiori (NIH and NIST) and Carol Swyt-Thomas (NIH),and then further developed by Carol and Bob Myklebust (NIST).
• DTSA ran only on Macintosh, and then only up to system 10. (NewMacs won’t run DTSA) A painful question heard many, many times:When will you have DTSA for the pc? DTSA-II is the long awaitedanswer!!
• DTSA-II is written in Java and operates on Mac, pc, UNIX, Linux.• DTSA-II is NOT DTSA! Nicholas started from scratch and used DTSA
as a guide to develop DTSA-II.• DTSA-II is being continually improved and the latest version can be
downloaded for free athttp://www.cstl.nist.gov/div837/837.02/epq/dtsa2/index.html
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NIST DTSA-II• Created by Nicholas Ritchie of NIST ([email protected]),
inspired by NIST-NIH Desktop Spectrum Analyzer (DTSA) invented1990-92 by Chuck Fiori (NIH and NIST) and Carol Swyt-Thomas (NIH),and then further developed by Carol and Bob Myklebust (NIST).
• DTSA ran only on Macintosh, and then only up to system 10. (NewMacs won’t run DTSA) A painful question heard many, many times:When will you have DTSA for the pc? DTSA-II is the long awaitedanswer.
• DTSA-II is written in Java and operates on Mac, pc, UNIX, Linux.• DTSA-II is NOT DTSA! Nicholas started from scratch and used DTSA
as a guide to develop DTSA-II.• DTSA-II is being continually improved and the latest version can be
downloaded for free athttp://www.cstl.nist.gov/div837/837.02/epq/dtsa2/index.html
• Tools currently embedded in DTSA-II:
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Basic operations
• Opening and manipulating spectral files
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Display and overlay spectra with various scaling options on linear/log/sqrt axes
Basic DTSA-II display window
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Spectrum file selection window
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A single spectrum is selected.
Spectrum preview opens in this window.
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Display and overlay spectra with various scaling options on linear/log/sqrt axes
“OK” or double click loads spectrumBasic display of single spectrum
Intensity (x-ray counts)
Energy scale in eV
Openedspectra are listed here
Spectrum informationfrom header
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But wait!
• A brilliant feature, the “Report” is going torecord your actions. A daily diary of actions(file named by date) is automatically saved.
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But wait!• A brilliant feature, the “Report” is going to record your actions. A
daily diary of actions (file named by date) is automatically saved.
The Report is a great feature for those of us approaching geezerhood.
Now, what was I saying?
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Open several spectra at a time:Holding down “SHIFT” key gives a continuous run
Preview of spectra in this window
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To open several spectra at a time:Holding down “CTRL” key allows multiple separate selections
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3 spectrum files have openedNote data from header
List of loaded spectra.Highlightedare displayed
When spectra have differences in the header data, only the terms in common will be displayed when more than one spectrum is selected
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Basic operations• Opening and manipulating spectral files• Display of spectra
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Changing the vertical axis scale:Method 1: Use arrows: x2 or x5 /2 or /5This arrow button restores full spectrum display Method 2: Mouse in y-axis number field; click and drag up or down
Basic display of single spectrum
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Basic display of single spectrum
Changing the vertical axis scale: Method 3Right click in spectrum display brings up thisWindow; choose zoom in or zoom out; this operation can be repeated.Note: “Zoom to all” restores full spectrum
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Basic display of single spectrum
Changing the vertical axis scale from linear to log1. Right click in spectrum window.2. Select “Ordinate scale”3. Select “Log”
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Basic display of single spectrum
Changing the vertical axisscale from linear to log1. Right click in spectrum window.2. Select “Ordinate scale”3. Select “Log”
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Basic display of single spectrum
Changing the vertical axisscale from linear to square root1. Right click in spectrum window.2. Select “Ordinate scale”3. Select “Square root”
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Basic display of single spectrum
Changing the horizontal axis scale: Method 11. Click a preset to show 0-5, 0–10, 0-15, or 0-20 keV
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Basic display of single spectrum
Changing the horizontal axis scale: Method 1• Click a preset to show 0-5, 0–10, 0-15, or 0-20 keV• 0 – 5 keV is shown
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Basic display of single spectrum
Changing the horizontal axis scale: method 2• Right click in spectrum field• Choose “create an ROI”
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Basic display of single spectrum
Changing the horizontal axis scale: Method 21. Right click in spectrum field2. Choose “create an ROI”3. Define start and end energies
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Basic display of single spectrum
Changing the horizontal axis scale: Method 21. Right click in spectrum field2. Choose “create an ROI”3. Define start and end energies 4. “OK” This action creates yellow ROI5. Click this icon to fully expand this ROIor6. Click within ROI and select ”Zoom to region”
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Basic display of single spectrum
Changing the horizontal axis scale: Method 26. Final display of 3.0 – 5.0 keV range
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Basic display of single spectrum
Changing the horizontal axis scale: Method 31. Double click and sweep an ROI(low to high energy) creating yellow ROI2. Immediate display of ROI parameters
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Basic display of single spectrum
Changing the horizontal axis scale: Method 31. Double click and sweep an ROI(low to high energy) creating yellow ROI2. Immediate display of ROI parameters3. Click icon to expandOR4. Right click within yellow ROI5. Select “zoom to region”
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Basic display of single spectrum
Changing the horizontal axis scale: Method 31. Double click and sweep an ROI(low to high energy) creating yellow ROI2. Immediate display of ROI parameters3. Click icon to expandOR4. Right click within yellow ROI5. Select “zoom to region”6. Final display of expanded ROI
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Basic operations• Opening and manipulating spectral files• Display of spectra• Peak labeling (manual only)
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KLM selection
One spectrumselected from list.
Peak Labeling
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To make labels “stick”click these check boxes
Peak Labeling
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Labeled Spectrum
Peak Labeling
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Choosing the peak label style
Peak Labeling
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Choosing the peak label styleIUPAC Long labels
Peak Labeling
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Choosing the peak label styleSiegbahn labels
Peak Labeling
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Basic operations• Opening and manipulating spectral files• Peak labeling (manual only)• Exporting spectra for publication (Gnuplot)
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Exporting spectrum for publication as gnuplot
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Publication-quality graphics from Gnuplot
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Comparing spectra from different EDS spectrometers,or from different dates from the same EDS:
The issue of EDS calibration• A spectrum is recorded with calibration data: eV/channel, zero offset,
number of channels (depending on manufacturer, this data may ormay not be embedded in the .msa header).
• When a spectrum is read into DTSA-II, the calibration information ischecked against the current calibration. If there is a mismatch, amessage prompts the analyst.
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When attempting to open a spectrum file with a different calibration, this message appears:
Spectrum Calibration
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The issue of EDS calibration• A spectrum is recorded with calibration data: eV/channel, zero offset,
number of channels (depending on manufacturer, this data may ormay not be embedded in the .msa header).
• When a spectrum is read into DTSA-II, the calibration information ischecked against the current calibration. If there is a mismatch, amessage prompts the analyst.
• The analyst then has two choices:– 1. Change the detector selection to match the incoming spectrum– 2. Accept the incoming spectrum but display it according to the current
calibration information. (Note: the incoming spectrum will retain itscalibration data so that when it is the only spectrum being displayed, itsown calibration will be applied.)
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Comparing multiple spectra
• Matching to a particular ROI
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Comparing multiple spectra
We wish to match the spectra for theintegral of SiKα,βStep 1: Click and swipe across SiKα,β peak to define ROI for matching.
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Comparing multiple spectra
We wish to match the spectra for the integral of SiKα,βStep 2: Right click and select“Spectrum Comparison”,then “Region integral”
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Comparing multiple spectra
Result shows Si peaks matched
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Spectrum sub-sampling tool
• Take an experimentally measured spectrum and createone or more “sub-samples”, that is, equivalent spectrathat would have been collected at lower dose.
• Sub-sampled spectra are useful for statistical studies.e.g., how does detection limit vary with dose.
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Spectrum “sub-sampling”: creating equivalent spectra for other doses
Startingmeasured spectrum
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Spectrum “sub-sampling”: creating equivalent spectra for other doses
Equivalent dose factor;set to 5% for this calculation
Number of synthesizedspectra, each with different statistics
RandomNumber “seed”
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Spectrum “sub-sampling”: creating equivalent spectra for other doses
3 sub-sampled spectra added to list
Note: for this example, 5% dose lowered the intensity scale by a factor of 20, as expected
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Spectrum “sub-sampling”: creating equivalent spectra for other doses
Each sub-sampledspectrum is preparedwith different randomstatistics.
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Background fitting tool
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Background Fitting
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Background Fitting
Enter materialcomposition
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Background Fitting
Enter materialcomposition
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Background Fitting
Fit with automaticplacement of background ROIs
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Background Fitting
Fit with maualplacement of background ROIs
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Background Fitting
Comparison ofmanual and automaticplacement of background ROIs
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DTSA-II Simulation Mode• EDS spectra calculated from
– 1. First principles, using best available cross sectionsand physical data (flat, bulk target only)
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Simulation Alien
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Simulation Alien: selecting Analytical Simulation
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Simulation Alien: specifying composition
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Simulation Alien: target composition
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Simulation Alien: instrument configuration
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Simulation Alien: Other options not invoked
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Simulation Alien
Hit “Finish” when “Progress”bar is filled
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Simulation Alien
Physics result
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Simulation Alien: Other options invoked
Counting statistics appropriate tothe dose and spectrometer efficiencyare applied for the specified number of replicates.
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Simulation Alien
Counting statistics appropriate tothe dose and spectrometer efficiencyare applied to the physics result for the specified number of replicates.
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Simulation Alien
Counting statistics appropriate tothe dose and spectrometer efficiencyare applied to the physics result for the specified number of replicates.
Comparison ofPhysics Result andafter applyingcounting statistics
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DTSA-II Simulation Mode• EDS spectra calculated from
– 1. First principles, using best available cross sectionsand physical data (flat, bulk target only)
– 2. Monte Carlo electron trajectory simulation forvarious specimen configurations:
• 1. Flat, bulk• 2. Layer on bulk• 3. Inclusion (hemisphere) embedded in bulk• 4. Spherical particle on substrate• 5. Cubic particle on substrate
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Simulation Alien: Monte Carlo simulation of a 1 μm K411 glass sphere on a C substrate
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Simulation Alien: Monte Carlo simulation of a 1 μm K411 glass sphere on a C substrate
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Simulation Alien: Monte Carlo simulation of a 1 μm K411 glass sphere on a C substrate
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Simulation Alien: Monte Carlo simulation of a 1 μm K411 glass sphere on a C substrate
Invoke x-raygenerationimages
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Simulation Alien: Monte Carlo simulation of a 1 μm K411 glass sphere on a C substrate
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Simulation Alien: Monte Carlo simulation of a 1 μm K411 glass sphere on a C substrate
“Report” tab:Generated and emitted intensities
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Simulation Alien: Monte Carlo simulation of a 1 μm K411 glass sphere on a C substrate
X-rayproductionimagesunder“Report”tab.
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Simulation Alien: Monte Carlo simulation of a 1 μm K411 glass sphere on a C substrate
X-rayproductionimagesunder“Report”tab.
Trajectory View
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Simulation Alien: Monte Carlo simulation trajectories can be viewed with Cosmo Player
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Simulation Alien: Monte Carlo simulation of a 1 μm K411 glass sphere on a C substrate
View along X-axis (rotated view from Y-axis)
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Simulation Alien: Monte Carlo simulation of a 1 μm K411 glass sphere on a C substrate
View along Y-axis
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1 μm
View along the beam
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View along the beam
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View from bottom of particle
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DTSA-II Simulation Mode• EDS spectra calculated from
– 1. First principles, using best available cross sectionsand physical data (flat, bulk target only)
– 2. Monte Carlo electron trajectory simulation forvarious specimen configurations:
• 1. Flat, bulk• 2. Layer on bulk• 3. Inclusion (hemisphere) embedded in bulk• 4. Spherical particle on substrate• 5. Cubic particle on substrate
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E0 = 20 keV1-μm inclusion of SiO2 in FeS2
Simulation Alien: Monte Carlo simulation of a 1 μm SiO2 hemisphere in FeS2
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E0 = 20 keV1-μm inclusion of SiO2 in FeS2
Simulation Alien: Monte Carlo simulation of a 1 μm SiO2 hemisphere in FeS2
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Simulation Alien: Monte Carlo simulation of a 1 μm SiO2 hemisphere in FeS2
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Simulation Alien: Monte Carlo simulation of a 1 μm SiO2 hemisphere in FeS2
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DTSA-II: Quantitative Analysis
• ZAF analysis against standards• Standards are used to extract needed
peak references for MLLS fit.• Report contains pertinent data (ZAF
factors, weight%, atom%, normalizedweight%; 1σ statistics)
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Select “File”
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Choose a spectrum file
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Continue specifyingneededspectra
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AccessFinderto selectspectra
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Report containsZAF details
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Residuals after fitting peaksNote: symmetric structure of residualsat peak positions implies that the peak references used are appropriate for this unknown.
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Comparison of Measured andSimulated FeS spectraNote good fit for FeK and S K, but poorfit for FeL
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Comparison of Measured andSimulated FeS spectra
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Comparison of Measured andSimulated FeS spectraafter region integralscaling
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Adding a new detector to the list under “Preferences”
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Adding a new detector to the list under “Preferences”
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Adding a new detector to the list under “Preferences”
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Adding a new detector to the list under “Preferences”