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An Iterative Qualitative – Quantitative Sequential Analysis Strategy for Electron-Excited X-ray Microanalysis with Energy Dispersive Spectrometry: Finding the Unexpected Needles in the Peak Overlap Haystack

Published

Author(s)

Dale E. Newbury, Nicholas Ritchie

Abstract

When analyzing an unknown by electron-excited energy dispersive X-ray spectrometry with the entire periodic table possibly in play, how does the analyst discover minor and trace constituents when their peaks are overwhelmed by the intensity of an interfering peak(s) from a major constituent? In this paper we advocate for and demonstrate an iterative analytical approach, alternating qualitative analysis (peak identification) and standards-based quantitative analysis and employing two "tools": (1) monitoring of the "raw analytical total" and (2) careful inspection of the "peak fitting residual spectrum" that is constructed as part of the quantitative analysis procedure in the software engine NIST DTSA-II. Elements newly recognized after each round are incorporated into the next round of quantitative analysis until the limits of detection are reached, as defined by the total spectrum counts.
Citation
Microscopy and Microanalysis
Volume
24

Keywords

energy dispersive x-ray spectrometry, quantitative x-ray microanalysis, peak fitting, scanning electron microscopy, standards-based analysis

Citation

Newbury, D. and Ritchie, N. (2018), An Iterative Qualitative – Quantitative Sequential Analysis Strategy for Electron-Excited X-ray Microanalysis with Energy Dispersive Spectrometry: Finding the Unexpected Needles in the Peak Overlap Haystack, Microscopy and Microanalysis, [online], https://doi.org/10.1017/S1431927618012394 (Accessed April 21, 2024)
Created June 20, 2018, Updated March 8, 2023