Uncertainty estimates for electron probe X-ray microanalysis measurements.

Anal Chem

Materials Measurement Science Division, National Institute of Standards and Technology, 100 Bureau Drive, MS 8372, Gaithersburg, Maryland 20899-8372, United States.

Published: November 2012

It has been over 60 years since Castaing (Castaing, R. Application of Electron Probes to Local Chemical and Crystallographic Analysis. Ph.D. Thesis, University of Paris, Paris, France, 1951; translated by P. Duwez and D. Wittry, California Institute of Technology, 1955) introduced the technique of electron probe X-ray microanalysis (EPMA), yet the community remains unable to quantify some of the largest terms in the technique's uncertainty budget. Historically, the EPMA community has assigned uncertainties to its measurements which reflect the measurement precision portion of the uncertainty budget and omitted terms related to the measurement accuracy. Yet, in many cases, the precision represents only a small fraction of the total budget. This paper addresses this shortcoming by considering two significant sources of uncertainty in the quantitative matrix correction models--the mass absorption coefficient, [μ/ρ], and the backscatter coefficient, η. Understanding the influence of these sources provides insight into the utility of EPMA measurements, and equally important, it allows practitioners to develop strategies to optimize measurement accuracy by minimizing the influence of poorly known model parameters.

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http://dx.doi.org/10.1021/ac301843hDOI Listing

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