Blunders in Automatic Qualitative Analysis (Peak Identification) for Energy Dispersive X-Ray Spectrometry: The Low Voltage Microanalysis Situation
Dale E. Newbury
Automatic qualitative analysis for peak identification is a standard feature of virtually all modern computer-aided analysis software for energy dispersive x-ray spectrometry with electron excitation. Testing of recently installed systems from four different manufacturers has revealed the occasional occurrence of misidentifications of peaks of major constituents whose concentrations exceeded 0.1 mass fraction. Test materials where peak identification failures were observed included ZnS, KBr, FeS2, tantalum-niobium alloy, NIST Standard Reference Material 482 (copper-gold alloy), Bi2Te3, uranium-rhodium alloy, platinum-chromium alloy, GaAs and GaP. These misidentifications of major constituents were exacerbated when the incident beam energy was 10 keV or lower, which restricted or excluded the excitation of the high photon energy K- and L- shell x-rays where multiple peaks, e.g. Ka-Kb or La-Lb-Lg, are well resolved and amenable to identification with high confidence. These misidentifications present a serious challenge to the credibility of this critical analytical technique. The analyst must assume responsibility to manually check peak identifications suggested by automatic qualitative analysis procedures even for major constituents.
Microscopy and Microanalysis
analytical electron microscopy, automated analysis, energy dispersive x-ray spectrometry, peak identification, qualitative analysis, scanning electron microscopy, transmission electron microscopy, x-ray microanalysis
Blunders in Automatic Qualitative Analysis (Peak Identification) for Energy Dispersive X-Ray Spectrometry: The Low Voltage Microanalysis Situation, Microscopy and Microanalysis
(Accessed May 30, 2023)