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An Iterative Qualitative-Quantitative Sequential Analysis Strategy for Electron-Excited X-ray Microanalysis with
Dale E Newbury1, Nicholas W M Ritchie1
1National Institute of Standards and Technology,Gaithersburg,MD 20899,USA.
Discovering minor elements in unknown samples using electron-excited energy dispersive X-ray spectrometry is challenging. This study presents an iterative method combining peak identification and quantitative analysis to overcome interfering peaks from major constituents.
Area of Science:
- Materials Science
- Analytical Chemistry
- Spectroscopy
Background:
- Electron-excited energy dispersive X-ray spectrometry (EDX) is crucial for elemental analysis.
- Identifying minor and trace elements can be difficult due to intense peaks from major constituents.
Purpose of the Study:
- To present an iterative analytical approach for improved detection of minor and trace elements in EDX analysis.
- To demonstrate a method for overcoming peak overlaps in complex samples.
Main Methods:
- An iterative approach alternating qualitative (peak identification) and quantitative analysis.
- Utilizing raw analytical total monitoring and peak fitting residual spectrum inspection.
- Incorporating newly identified elements in subsequent quantitative analysis rounds using DTSA-II software.
Main Results:
- The iterative method successfully identifies and quantifies elements even when their peaks are obscured by major constituents.
- The approach allows for the detection of elements down to the limits of detection defined by total spectrum counts.
- Demonstrated effectiveness in analyzing complex unknown samples.
Conclusions:
- The proposed iterative analytical strategy enhances the capability of EDX for detecting low-concentration elements in the presence of high-concentration matrix elements.
- This method provides a robust framework for accurate elemental analysis of complex materials.
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