Abstract
Chapter 9 presented the procedures for performing quantitative electron probe x-ray microanalysis for the casef an ideal specimen. The ideal specimen surface is flat and highly polished to reduce surface roughness to a negligible level so that electron and x-ray interactions are unaffected by geometric effects. Such a highly polished surface has a short-range surface topography (sampled at distances less than 1 μm) that is reduced to an amplitude of a few nanometers and the long-range topography (sampled at distances greater than 100 μm) that is reduced to 100 nm or less. These ideal specimens satisfy three “zeroth” assumptions that underlie the conventional EPMA technique:
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1.
The only reason that the x-ray intensities measured on the unknown differ from those measured on the standards is that the compositions of specimen and standard are different. Specifically, no other factors such as surface roughness, size, shape, and thickness, which can be generally grouped together as “geometric” factors, act to affect the intensities measured on the unknown.
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2.
The specimen is homogeneous over the full extent of the interaction volume excited by the primary electron beam and sampled by the primary and secondary x-rays. Because x-rays of different excitation energies are generated with different distributions within the interaction volume, it is critical that the specimen has a uniform composition over the full region. If a thin surface layer of different composition than the underlying bulk material is present, this discontinuity is not properly considered in the conventional matrix correction analysis procedure.
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3.
The specimen is stable under the electron beam. That is, the interaction volume is not modified through loss of one or more atomic or molecular species by the electron beam over the time period necessary to collect the x-ray spectrum (EDS) or peak intensities (WDS). Biological and polymer specimens are likely to alter composition under electron bombardment.
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Goldstein, J.I. et al. (2003). Special Topics in Electron Beam X-Ray Microanalysis. In: Scanning Electron Microscopy and X-ray Microanalysis. Springer, Boston, MA. https://doi.org/10.1007/978-1-4615-0215-9_10
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