Inca EDS Quantitative Analysis Simplified Instructions

For Met 313 Lab

  1. Set Up Microscope according to instructions
  2. Find the copper tape
  3. Fill the image window with just the copper tape, avoid surface artifacts. Focus, Link Z, move to 5mm WD and lock Z.
  4. Open Inca Software on the third computer screen
  5. At the bottom of the left, select Analyzer tab.
  6. A flow chart will show up on the left. Select Project , a different window will open on the right, Project 1 is the default, you can add a new project by clicking “New Project”, this will increase the Project # only.
  7. Sample: Sample ID and give the sample a name or identifying number. At the bottom check the boxes by “Sample has been polished” and Sample has been Coated, Carbon, 15nm and use the density default.
  8. Microscope Setup: To fix the process time and set the dead time, which should be <64%. Acquire a spectrum, clicking the round green button to the upper right above the spectrum window. Change the Process Time and notice the difference in the Dead Time. A dead time between 1-45% is good. The red square button by the green button stops the acquisition of the spectrum. (There should be three peaks present in this spectrum)
  9. Quant Optimization: Select copper as the element for quant optimization. Acquire a new spectrum, allow the acquisition to finish. Click “Measure”. There might be an error message about the processor.
  10. Move the sample to an area for analysis, the glass. Fill the image window with the sample to be analyzed, avoid surface artifacts, magnification should be as low as possible.
  11. Acquire Spectra: Termination of acquisition set to Live time to 50 sec. Check the spectra conditions, Process time was set in Quant Opt., Spectrum range is 0-10 keV, and the Number of Channels is 1K which corresponds to 10eV/channel. Start to acquire a spectrum with the green circle button. To enlarge the spectrum, left click and hold the cursor in the spectrum window and move it up, to decrease move the cursor down. Right and left only change the position of the spectrum. Right click and you and select “Reset Scale” to return he spectrum back to the original.
  12. Confirm Elements: Can do this while acquiring the spectrum. It is best to Clear All the elements and adding them by double clicking them on the periodic table. When the spectrum is complete make sure the correct elements are labeled on the spectrum.
  13. Quant Setup: Processing Option, select Element by Stoichiometry and put oxygen as the element, Check Normalize Quant Results, Use the current element list.
  14. Quant: Will automatically give the results. Have Full Results tab selected at the bottom of the window.
  15. Report: To put the results in a report format, for Template select Spectra/Summary of Results. Click the blue “W” to export the report to a word document. Each new quantification will be added to the report when exported. Save the word document. (This puts Word as the active window)
  16. Go back to the Inca Analyzer and select Standardize. Must have a spectrum in the spectrum window. Click “New Standard” and give it a unique name. At the lower left add the elements and the wt%. The total should be 100%. Highlight an element and click “Standardize”, the first element will pop up a box to save the Standardization, click yes. Repeat this for each element in the list. There will be a warning pop up when an element is less than 10%, click yes and proceed.
  17. Select a different area on the glass.
  18. Go back to Acquire Spectrum and repeat steps 11, 12, 14, 15.
  19. When finished with report go back to Standardize and click “Restore” to return the quantification back to default.
  20. Close Inca and save the project
  21. Shut down scope according to instructions.