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Quantitative Electron-Excited X-ray Microanalysis With Low-Energy L-shell X-ray Peaks Measured With Energy-Dispersive

Dale E Newbury1, Nicholas W M Ritchie1

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Microscopy and Microanalysis : the Official Journal of Microscopy Society of America, Microbeam Analysis Society, Microscopical Society of Canada
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Analyzing intermetallic compounds using low-energy X-ray peaks can lead to inaccuracies. Using compound standards improves accuracy for elements like Ni, Fe, Co, and Ge, but not always, as seen in the Fe-S system.

Keywords:
L-family X-ray analysiselectron-excited X-ray microanalysisenergy-dispersive X-ray spectrometryquantitative elemental microanalysis

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Area of Science:

  • Materials Science
  • Analytical Chemistry
  • Spectroscopy

Background:

  • Quantitative analysis of electron-excited X-ray spectra is a standard method.
  • Recent studies highlighted inaccuracies in analyzing intermetallic compounds using low-energy L-shell X-ray peaks.

Purpose of the Study:

  • To investigate the accuracy of quantitative analysis using low-energy L-shell X-ray peaks in intermetallic compounds.
  • To evaluate the effectiveness of pure element versus compound standards for improving analytical accuracy.

Main Methods:

  • Energy-dispersive X-ray spectrometry (EDS) was used to analyze Ni-based intermetallic compounds.
  • The study extended analysis to a range of elements (Ti to Se) using L-shell peaks.
  • Accuracy was assessed using both pure element and compound standards.

Main Results:

  • Confirmed previous findings of analytical inaccuracies with low-energy L-shell peaks for Ni.
  • Identified similar anomalies for Fe, Co, and Ge, indicating a broader issue.
  • Compound standards generally improved accuracy, but exceptions were found (e.g., Fe-S system).

Conclusions:

  • Low-energy L-shell X-ray peaks require careful consideration for accurate quantification in intermetallic compounds.
  • Compound standards can mitigate inaccuracies but are not a universal solution.
  • Further research is needed to understand and correct for matrix effects in these specific analytical scenarios.