Quantitative Electron-Excited X-ray Microanalysis with Low Energy L-shell X-ray Peaks Measured with Energy Dispersive Spectrometry
Dale E. Newbury, Nicholas Ritchie
Quantification of electron-exited X-ray spectra following the standards-based "k-ratio" (unknown/standard intensity) protocol with corrections for "matrix effects" (electron energy loss and backscattering, X-ray absorption, and secondary X-ray fluorescence) is a well-established method with a record of rigorous testing and extensive experience. Two recent studies by Gopon et al and Llovet et al have renewed interest in studying the accuracy of measurements made using L-shell X-ray lines. Gopon worked in the Fe – Si system and Llovet worked in the Ni – Si system. Both have reported unexpectedly large deviations in analytical accuracy when analyzing intermetallic compounds systems using the low photon energy Fe or Ni L-shell X-ray peaks with pure element standards and wavelength dispersive X-ray spectrometry. This study confirms those observations on the Ni intermetallic compounds using energy dispersive X-ray spectrometry, and extends the study of analysis with low photon energy L-shell peaks to a wide range of elements, Ti to Se. Within this range of elements, anomalies in analytical accuracy have been found for Fe, Co, and Ge in addition to Ni. For these elements, the use of compound standards instead of pure elements usually resulted in improved analytical accuracy. However, compound standards are not always better than elemental as is demonstrated with FeS using FeS2 as a standard.
and Ritchie, N.
Quantitative Electron-Excited X-ray Microanalysis with Low Energy L-shell X-ray Peaks Measured with Energy Dispersive Spectrometry, Microscopy and Microanalysis, [online], https://tsapps.nist.gov/publication/get_pdf.cfm?pub_id=932514
(Accessed June 1, 2023)