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.
[1]
David B. Williams,et al.
X-Ray Spectrometry in Electron Beam Instruments
,
2012,
Springer US.
[2]
C R Swyt,et al.
"Standardless" quantitative electron probe microanalysis with energy-dispersive X-ray spectrometry: is it worth the risk?
,
1995,
Analytical chemistry.
[3]
K. Heinrich,et al.
Absorption of primary x-rays in electron probe microanalysis
,
1975
.
[4]
R. Packwood.
A Comprehensive Theory of Electron Probe Microanalysis
,
1991
.
[5]
J.-L. Pouchou,et al.
Quantitative Analysis of Homogeneous or Stratified Microvolumes Applying the Model “PAP”
,
1991
.
[6]
Cedric J. Powell,et al.
Cross sections for ionization of inner-shell electrons by electrons
,
1976
.