NIST DTSA-II ( Son of DTSA ): Step-by-Step
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1 NIST DTSA-II ( Son of DTSA ): Step-by-Step Dale E. Newbury (grateful user) National Institute of Standards and Technology Gaithersburg, MD
2 NIST-NIH Desktop Spectrum Analyzer (DTSA)
3 Spectral Simulation with DTSA OK SiKα,β AlKα,β CaKα FeKα Log Intensity CaL FeL CaKβ FeKβ NIST Glass K411 E 0 = 20keV Inside specimen After specimen absorption After EDS window absorption After EDS broadening (145 ev) Photon Energy (kev) For 16 years, I have heard: When will you have DTSA for the pc?
4 NIST DTSA-II Created by Nicholas Ritchie of NIST inspired by NIST-NIH Desktop Spectrum Analyzer (DTSA) invented by Chuck Fiori (NIH and NIST) and Carol Swyt-Thomas (NIH), and then further developed by Carol and Bob Myklebust (NIST).
5 NIST DTSA-II Created by Nicholas Ritchie of NIST inspired by NIST-NIH Desktop Spectrum Analyzer (DTSA) invented 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. (New Macs won t run DTSA) A painful question heard many, many times: When will you have DTSA for the pc? DTSA-II is the long awaited answer!!
6 NIST DTSA-II Created by Nicholas Ritchie of NIST inspired by NIST-NIH Desktop Spectrum Analyzer (DTSA) invented 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. (New Macs won t run DTSA) A painful question heard many, many times: When will you have DTSA for the pc? DTSA-II is the long awaited answer!! DTSA-II is written in Java and operates on Mac, pc, UNIX, Linux.
7 NIST DTSA-II Created by Nicholas Ritchie of NIST inspired by NIST-NIH Desktop Spectrum Analyzer (DTSA) invented 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. (New Macs won t run DTSA) A painful question heard many, many times: When will you have DTSA for the pc? DTSA-II is the long awaited answer!! 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.
8 NIST DTSA-II Created by Nicholas Ritchie of NIST inspired by NIST-NIH Desktop Spectrum Analyzer (DTSA) invented 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. (New Macs won t run DTSA) A painful question heard many, many times: When will you have DTSA for the pc? DTSA-II is the long awaited answer!! 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 at
9
10 NIST DTSA-II Created by Nicholas Ritchie of NIST inspired by NIST-NIH Desktop Spectrum Analyzer (DTSA) invented 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. (New Macs won t run DTSA) A painful question heard many, many times: When will you have DTSA for the pc? DTSA-II is the long awaited answer. 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 at Tools currently embedded in DTSA-II:
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12 Basic operations Opening and manipulating spectral files
13 Display and overlay spectra with various scaling options on linear/log/sqrt axes Basic DTSA-II display window
14 Spectrum file selection window
15 A single spectrum is selected. Spectrum preview opens in this window.
16 Display and overlay spectra with various scaling options on linear/log/sqrt axes OK or double click loads spectrum Basic display of single spectrum Intensity (x-ray counts) Energy scale in ev Opened spectra are listed here Spectrum information from header
17 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.
18 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?
19 Open several spectra at a time: Holding down SHIFT key gives a continuous run Preview of spectra in this window
20 To open several spectra at a time: Holding down CTRL key allows multiple separate selections
21 3 spectrum files have opened Note data from header List of loaded spectra. Highlighted are displayed When spectra have differences in the header data, only the terms in common will be displayed when more than one spectrum is selected
22 Basic operations Opening and manipulating spectral files Display of spectra
23 Basic display of single spectrum Changing the vertical axis scale: Method 1: Use arrows: x2 or x5 /2 or /5 This arrow button restores full spectrum display Method 2: Mouse in y-axis number field; click and drag up or down
24 Basic display of single spectrum Changing the vertical axis scale: Method 3 Right click in spectrum display brings up this Window; choose zoom in or zoom out; this operation can be repeated. Note: Zoom to all restores full spectrum
25 Basic display of single spectrum Changing the vertical axis scale from linear to log 1. Right click in spectrum window. 2. Select Ordinate scale 3. Select Log
26 Basic display of single spectrum Changing the vertical axis scale from linear to log 1. Right click in spectrum window. 2. Select Ordinate scale 3. Select Log
27 Basic display of single spectrum Changing the vertical axis scale from linear to square root 1. Right click in spectrum window. 2. Select Ordinate scale 3. Select Square root
28 Basic display of single spectrum Changing the horizontal axis scale: Method 1 1. Click a preset to show 0-5, 0 10, 0-15, or 0-20 kev
29 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
30 Basic display of single spectrum Changing the horizontal axis scale: method 2 Right click in spectrum field Choose create an ROI
31 Basic display of single spectrum Changing the horizontal axis scale: Method 2 1. Right click in spectrum field 2. Choose create an ROI 3. Define start and end energies
32 Basic display of single spectrum Changing the horizontal axis scale: Method 2 1. Right click in spectrum field 2. Choose create an ROI 3. Define start and end energies 4. OK This action creates yellow ROI 5. Click this icon to fully expand this ROI or 6. Click within ROI and select Zoom to region
33 Basic display of single spectrum Changing the horizontal axis scale: Method 2 6. Final display of kev range
34 Basic display of single spectrum Changing the horizontal axis scale: Method 3 1. Double click and sweep an ROI (low to high energy) creating yellow ROI 2. Immediate display of ROI parameters
35 Basic display of single spectrum Changing the horizontal axis scale: Method 3 1. Double click and sweep an ROI (low to high energy) creating yellow ROI 2. Immediate display of ROI parameters 3. Click icon to expand OR 4. Right click within yellow ROI 5. Select zoom to region
36 Basic display of single spectrum Changing the horizontal axis scale: Method 3 1. Double click and sweep an ROI (low to high energy) creating yellow ROI 2. Immediate display of ROI parameters 3. Click icon to expand OR 4. Right click within yellow ROI 5. Select zoom to region 6. Final display of expanded ROI
37 Basic operations Opening and manipulating spectral files Display of spectra Peak labeling (manual only)
38 Peak Labeling KLM selection One spectrum selected from list.
39 Peak Labeling To make labels stick click these check boxes
40 Peak Labeling Labeled Spectrum
41 Peak Labeling Choosing the peak label style
42 Peak Labeling Choosing the peak label style IUPAC Long labels
43 Peak Labeling Choosing the peak label style Siegbahn labels
44 Basic operations Opening and manipulating spectral files Peak labeling (manual only) Exporting spectra for publication (Gnuplot)
45 Exporting spectrum for publication as gnuplot
46 Publication-quality graphics from Gnuplot
47 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 or may not be embedded in the.msa header). When a spectrum is read into DTSA-II, the calibration information is checked against the current calibration. If there is a mismatch, a message prompts the analyst.
48 Spectrum Calibration When attempting to open a spectrum file with a different calibration, this message appears:
49 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 or may not be embedded in the.msa header). When a spectrum is read into DTSA-II, the calibration information is checked against the current calibration. If there is a mismatch, a message 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 its calibration data so that when it is the only spectrum being displayed, its own calibration will be applied.)
50 Comparing multiple spectra Matching to a particular ROI
51 Comparing multiple spectra We wish to match the spectra for the integral of SiKα,β Step 1: Click and swipe across SiKα,β peak to define ROI for matching.
52 Comparing multiple spectra We wish to match the spectra for the integral of SiKα,β Step 2: Right click and select Spectrum Comparison, then Region integral
53 Comparing multiple spectra Result shows Si peaks matched
54 Spectrum sub-sampling tool Take an experimentally measured spectrum and create one or more sub-samples, that is, equivalent spectra that would have been collected at lower dose. Sub-sampled spectra are useful for statistical studies. e.g., how does detection limit vary with dose.
55 Spectrum sub-sampling : creating equivalent spectra for other doses Starting measured spectrum
56 Spectrum sub-sampling : creating equivalent spectra for other doses Random Number seed Equivalent dose factor; set to 5% for this calculation Number of synthesized spectra, each with different statistics
57 Spectrum sub-sampling : creating equivalent spectra for other doses Note: for this example, 5% dose lowered the intensity scale by a factor of 20, as expected 3 sub-sampled spectra added to list
58 Spectrum sub-sampling : creating equivalent spectra for other doses Each sub-sampled spectrum is prepared with different random statistics.
59 Background fitting tool
60 Background Fitting
61 Background Fitting Enter material composition
62 Background Fitting Enter material composition
63 Background Fitting Fit with automatic placement of background ROIs
64 Background Fitting Fit with maual placement of background ROIs
65 Background Fitting Comparison of manual and automatic placement of background ROIs
66 DTSA-II Simulation Mode EDS spectra calculated from 1. First principles, using best available cross sections and physical data (flat, bulk target only)
67 Simulation Alien
68 Simulation Alien: selecting Analytical Simulation
69 Simulation Alien: specifying composition
70 Simulation Alien: target composition
71 Simulation Alien: instrument configuration
72 Simulation Alien: Other options not invoked
73 Simulation Alien Hit Finish when Progress bar is filled
74 Simulation Alien Physics result
75 Simulation Alien: Other options invoked Counting statistics appropriate to the dose and spectrometer efficiency are applied for the specified number of replicates.
76 Simulation Alien Counting statistics appropriate to the dose and spectrometer efficiency are applied to the physics result for the specified number of replicates.
77 Simulation Alien Comparison of Physics Result Counting and statistics appropriate to after applying the dose and spectrometer efficiency counting statistics are applied to the physics result for the specified number of replicates.
78 DTSA-II Simulation Mode EDS spectra calculated from 1. First principles, using best available cross sections and physical data (flat, bulk target only) 2. Monte Carlo electron trajectory simulation for various 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
79 Simulation Alien: Monte Carlo simulation of a 1 μm K411 glass sphere on a C substrate
80 Simulation Alien: Monte Carlo simulation of a 1 μm K411 glass sphere on a C substrate
81 Simulation Alien: Monte Carlo simulation of a 1 μm K411 glass sphere on a C substrate
82 Simulation Alien: Monte Carlo simulation of a 1 μm K411 glass sphere on a C substrate Invoke x-ray generation images
83 Simulation Alien: Monte Carlo simulation of a 1 μm K411 glass sphere on a C substrate
84 Simulation Alien: Monte Carlo simulation of a 1 μm K411 glass sphere on a C substrate Report tab: Generated and emitted intensities
85 Simulation Alien: Monte Carlo simulation of a 1 μm K411 glass sphere on a C substrate X-ray production images under Report tab.
86 Simulation Alien: Monte Carlo simulation of a 1 μm K411 glass sphere on a C substrate X-ray production images under Trajectory Report View tab.
87 Simulation Alien: Monte Carlo simulation trajectories can be viewed with Cosmo Player
88 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)
89 Simulation Alien: Monte Carlo simulation of a 1 μm K411 glass sphere on a C substrate View along Y-axis
90 View along the beam 1 μm
91 View along the beam
92 View from bottom of particle
93 DTSA-II Simulation Mode EDS spectra calculated from 1. First principles, using best available cross sections and physical data (flat, bulk target only) 2. Monte Carlo electron trajectory simulation for various 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
94 Simulation Alien: Monte Carlo simulation of a 1 μm SiO 2 hemisphere in FeS 2 E 0 = 20 kev 1-μm inclusion of SiO 2 in FeS 2
95 Simulation Alien: Monte Carlo simulation of a 1 μm SiO 2 hemisphere in FeS 2 E 0 = 20 kev 1-μm inclusion of SiO 2 in FeS 2
96 Simulation Alien: Monte Carlo simulation of a 1 μm SiO 2 hemisphere in FeS 2
97 Simulation Alien: Monte Carlo simulation of a 1 μm SiO 2 hemisphere in FeS 2
98 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%, normalized weight%; 1σ statistics)
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100
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102 Select File
103 Choose a spectrum file
104
105 Continue specifying needed spectra
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107 Access Finder to select spectra
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110 Report contains ZAF details
111 Residuals after fitting peaks Note: symmetric structure of residuals at peak positions implies that the peak references used are appropriate for this unknown.
112 Comparison of Measured and Simulated FeS spectra Note good fit for FeK and S K, but poor fit for FeL
113 Comparison of Measured and Simulated FeS spectra
114 Comparison of Measured and Simulated FeS spectra after region integral scaling
115 Adding a new detector to the list under Preferences
116 Adding a new detector to the list under Preferences
117 Adding a new detector to the list under Preferences
118 Adding a new detector to the list under Preferences
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