The Use of Energy Dispersive X-Ray Microanalysis in the Geological Sciences: 30 Years of Heavy and Creative Application

1998 ◽  
Vol 4 (S2) ◽  
pp. 180-181
Author(s):  
John T. Armstrong

Considering the heavy use by the geological community that followed, it is not surprising that first two authors of the introductory paper in Science on the energy dispersive x-ray spectrometer applied their x-ray microanalysis skills predominantly in the geological sciences. The energy dispersive spectrometer became first commercially available at an ideal time for the geological community. During the 1960’s, mineralogists and petrographers like K. Keil, J.V.P. Long, J.C. Rucklidge, J.V. Smith, A. Albee, and A. Chodos demonstrated that electron microprobe analysis with wavelength dispersive spectrometers could provide accurate in-situ analysis of portions of individual mineral grains on a scale not readily obtainable by other techniques (e.g., 2-3 and cited refs.). The electron microprobe enabled analysis of features observed by reflected- and transmitted-light polarized optical microscopy (prime tools of the mineralogist and petrographer) and was beginning to be used routinely for the study of meteorites and terrestrial rocks and even more exotic types of specimens, like individual microparticles from sediment and airborne particulate samples.

2000 ◽  
Vol 6 (2) ◽  
pp. 145-149 ◽  
Author(s):  
S. B. J. Reed

In truly standardless electron microprobe analysis, generated X-ray intensities calculated from first principles are combined with a detector efficiency model. Though already used for energy dispersive (ED) analysis, the application of this concept to wavelength dispersive (WD) analysis is problematic, mainly because the reflectivity of spectrometer crystals is not well known. However, the need to carry out standard measurements with every batch of WD analyses can be avoided by using stored intensity data, and interpolation may be used when no standard is available. An empirical adjustment factor allowing for changes in spectrometer efficiency with time can be applied as necessitated by the variability of the spectrometer characteristics and the accuracy required. A similar approach to background corrections, based on measured continuum intensities, can be used. While the convenience of standardless WD analysis is attainable only at the expense of reduced accuracy, it can have a useful role where high accuracy is not needed or as a preliminary to applying a more rigorous routine using standards.


1984 ◽  
Vol 28 ◽  
pp. 367-375 ◽  
Author(s):  
R. G. Johnston ◽  
M. B. Strope ◽  
R. P. Anantatmula

AbstractX-ray diffraction and electron microprobe analysis were used in combination to identify reaction phases that formed on the surfaces of low-carbon steel specimens reacted with a 75% basalt-25% bentonite mixture and anion-doped water in sealed pressure vessels at 100°C and 250°C. Reaction phases on specimen surfaces and in adhering geologic material were identified by conventional X-ray diffraction scans of entire specimens with intact reaction layers. Comparison of results from adhering geologic material and scans of selectively removed layers allowed establishment of approximate reaction gradients in the adhering packing material. Electron microprobe analysis of specimens in cross-section provided quantitative chemical analyses of adhering reaction phases, and identification of reaction layer composition gradients and thicknesses. Magnetite formed on the surface of specimens reacted at 250°C for 4 weeks. Iron-enriched clay was also observed on specimen surfaces and in the adjacent basalt-bentonite mixture. The 100°C experiments yielded surface films of a siderite-structure phase, (Fe,Ca,Mn)CO3, that were not observed in previous experiments with synthetic ground-water. Less extensive iron enrichment of the adjacent clays compared to that seen in the 250°C experiments was observed. The siderite-structure phase generally formed when no carbonate ion was present in the initial solution, implying dissolution of impurity calcite in the bentonite as the controlling factor in the reaction. The results demonstrate the utility of combining X-ray diffraction and electron microprobe analysis for characterization of reaction phases on alloys reacted with complex geologic materials.


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