Microscopy and Microanalysis


Standardless Quantitative Electron-Excited X-ray Microanalysis by Energy-Dispersive Spectrometry: What Is Its Proper Role?

Dale E.  Newbury  a1
a1 Surface and Microanalysis Science Division, National Institute of Standards and Technology, Building 222, Room A113, Gaithersburg, MD 20899


Electron beam X-ray microanalysis with semiconductor energy-dispersive spectrometry (EDS) performed with standards and calculated matrix corrections can yield quantitative results with a distribution such that 95% of analyses fall within ±5% relative for major and minor constituents. Standardless methods substitute calculations for the standard intensities, based either on physical models of X-ray generation and propagation (first principles) or on mathematical fits to remotely measured standards (fitted standards). Error distributions have been measured for three different standardless analysis procedures with a suite of microanalysis standards including metal alloys, glasses, minerals, ceramics, and stoichiometric compounds. For the first-principles standardless procedure, the error distribution placed 95% of analyses within ±50% relative, whereas for two commercial fitted standards procedures, the error distributions placed 95% of analyses within ±25% relative. The implication of these error distributions for the accuracy of analytical results is considered, and recommendations for the use of standardless analysis are given.

(Received September 15 1998)
(Accepted November 16 1998)

Key Words: electron beam X-ray microanalysis; electron probe microanalyzer; energy-dispersive spectrometry (EDS); quantitative X-ray microanalysis; scanning electron microscope; X-ray microanalysis.