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Light Element Analysis

Published online by Cambridge University Press:  06 March 2019

A. K. Baird
A. K. Baird*
Affiliation:
Geology Department, Pomona College Claremont, California
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Abstract

Qualitative and quantitative analyses of elements below atomic number 20, and extending to atomic number 4, have been made practical and reasonably routine only in the past five to ten years by advances in: 1) excitation sources; 2) dispersive spectrometers; 3) detection devices; and 4) reductions of optic path absorption. At present agreement is lacking on the best combination of parameters for light element analysis. The principal contrasts in opinion concern excitation.

Direct electron excitation, particularly as employed in microprobe analysis (but not limited to such instruments), provides relatively high emission intensities of all soft X-rays, but also generates a high continuum, requires the sample to be at essentially electron gun vacuum, and introduces practical calibration problems (“matrix effects“). X-ray excitation of soft X-rays overcomes some of the latter three disadvantages, and has its own limitations. Sealed X-ray sources of conventional or semi-conventional design can provide useful (if not optimum) light element emission intensities down to atomic number 9, hut with serious loss of efficiency in many applications below atomic number 15 largely because of window-thinness limitations under electron bombardment.

Type
Research Article
Information
Advances in X-Ray Analysis , Volume 13: Eighteenth Annual Conference on Applications of X-ray Analysis, August 6-8, 1969 , 1969 , pp. 26 - 48
Copyright
Copyright © International Centre for Diffraction Data 1969

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References

1. Campbell, W. J. and Brown, J. D., “X-ray Absorption and Emission,” Anal. Chem. 40:346R–375R, (1968).Google Scholar
2. Chodos, A. A. and Engel, C. G., “Fluorescent X-ray Spectrographic Analyses of Amphibolite Rocks and Constituent Hornblendes,” Advances in X-ray Analysis 4:401–413, (1961).Google Scholar
3. Sterk, A. A., “X-ray Techniques in the 1 to 400Å Range,” Advances in X-ray Analysis 9:410–419, (1965).Google Scholar
4. Sterk, A. A., Marks, C. L., and Saylor, W. P., “Production Efficiencies of X-ray Emission Spectra by Proton Bombardment,” Advances in X-ray Analysis 10:399–409, (1966).Google Scholar
5. Thatcher, J. W. and Campbell, W. J., “Instrumentation for Primary and Secondary Excitation of Low-Energy X-ray Spectral Lines,” U. S. Bureau of Mines, Report of Investigations 6689:1–29, (1965).Google Scholar
6. Mattson, R. A., “Some Measurements of Carbon K Excitation in a New Ultrasoft X-ray Spectrometer,” Advances in X-ray Analysis 8:333–340, (1964).Google Scholar
7. Bernstein, F. and Mattson, R. A., “Quantitative X-ray Emission Analysis of Magnesium through Fluorine with X-ray and Electron Excitation,” Advances in X-ray Analysis 10:494–505, (1966).Google Scholar
8. Wyckoff, R. W. G. and Davidson, F. D., “Windowless Tubes for X-ray Spectroscopy,” Rev. Sci. Instr. 34:572, (1963).Google Scholar
9. Fischer, D. W. and Baun, W. L., “Experimental Dispersing Systems for soft X-rays,” Advances in X-ray Analysis 7:489–496, (1963).Google Scholar
10. Henke, B. L., “Sodium and Magnesium Fluorescence Analysis— Part I: Method,” Advances in X-ray Analysis 6:361–376, (1962).Google Scholar
11. Henke, B. L., “Some Notes on Ultrasoft X-ray Fluorescence Analysis—10 to 100Å Region,” Advances in X-ray Analysis 8:269–234, (1964).Google Scholar
12. Canon, M., “A Polycrystalline X-ray Analyzing Crystal,” Advances in X-ray Analysis 8:285–300, (1964).Google Scholar
13. Gould, R. W., Bates, S. R. and Sparks, C. J., “Application of the Graphite Monochromator to Light Element X-ray Spectroscopy,” Applied Spectroscopy 22:549–551, (1968).Google Scholar
14. Ehlert, R. C., “The Diffraction of X-rays by Multilayer Stearate Soap Films,” Advances in X-ray Analysis 8:325–332, (1964).Google Scholar
15. Henke, B. L., “Application of Multilayer Analyzers to 15-150Å Fluorescence Spectroscopy for Chemical and Valence Band Analysis,” Advances in X-ray Analysis 9:430–440, (1965).Google Scholar
16. Davidson, F. D. and Wyckoff, R. W. G., “L and M X-ray Spectra in the Region 2-85Å,” Advances in X-ray Analysis 9:344–353, (1965).Google Scholar
17. Nicholson, J. B. and Wittry, D. B., “A Comparison of Gratings and Crystals in the 20-115Å Region,” Advances in X-ray Analysis 7:497–511, (1963).Google Scholar
18. Holliday, J. E., “Determination of Electron Distribution and Bonding from Soft X-ray Emission Spectroscopy,” Advances in X-ray Analysis 9:365–375, (1965).Google Scholar
19. Spielberg, H., “Characteristics of Flow Proportional Counters for X-rays,” Advances in X-ray Analysis 10:534–545, (1966).Google Scholar
20. Personal communication from Nuclear Diodes, Inc. (1969).Google Scholar
21. Jenkins, R. and van Gelder, S., “Determination of Low Concentrations of Fluorine in Cement by X-ray Fluorescence Spectroscopy,” Scientific and Analytical Equipment Bulletin 79.177/ FS19, H. V. Philips, Eindhoven, The Netherlands (1969).Google Scholar
22. Baird, A. K. and Henke, B. L., “Oxygen Determinations in Silicates and Total Major Elemental Analysis of Rocks by Soft X-ray Spectrometry,” Anal. Chem. 37:727–729, (1965).Google Scholar
23. Henke, B. L., “X-ray Fluorescence Analysis for Sodium, Fluorine, Oxygen, Nitrogen, Carbon, and Boron,” Advances in X-ray Analysis 7, 460:488–1963.Google Scholar
24. Bernstein, F., “Application of X-ray Fluorescence Analysis to Process Control,” Advances in X-ray Analysis 5:486–499, (1962)Google Scholar
25. Claisse, F. and Samson, C., “Heterogeneity Effects in X-ray Analysis,” Advances in X-ray Analysis 5:335–354, (1961).Google Scholar
26. Gunn, E. L., “The Effect of Particles on Surface Irregularities on the X-ray Fluorescent Intensity of Selected Substances,” Advances in X-ray Analysis 4:382–400, (1960).Google Scholar
27. Madlem, K. W., “Matrix and Particle Size Effects in Analyses of Light Elements, Zinc through Oxygen by Soft X-ray Spectrometry,” Advances in X-ray Analysis 9:441–455, (1965).Google Scholar
28. Claisse, F., “Accurate X-ray Fluorescence Analysis Without Internal Standard,” Quebec Dept, of Mines P.R. 327, (1956).Google Scholar
29. Welday, E. E., Baird, A. K., and Madlem, K. W., “Silicate Sample Preparation for Light-Element Analyses by X-ray Spectrography, Am. Mineral. 49:889–903, (1964).Google Scholar
30. Rose, H. J., Adler, I., Flanagan, F. J., “Use of La20 as a Heavy Absorber in the X-ray Fluorescence Analysis of Silica Rocks,” U. S. Geol. Surv. Prof. Paper 450-B:80-82, (1962).Google Scholar
31. Volborth, A., “X-ray Spectrographic Determination of All Major Oxides in Igneous Rocks and Precision and Accuracy of a Direct Pelletizing Method,” Nevada Bureau of Mines Rept. 6: 1–72, (1963).Google Scholar
32. Stanley, R. C., “Counting Statistics in X-ray Spectroscopy,” British Jour. Appl. Physics 12:503, (1961).Google Scholar
33. Baird, A. K. and Welday, E. E., “Precision and Accuracy of Silicate Analyses by X-ray Fluorescence,” Advances in X-ray Analysis 11:114–128, (1967).Google Scholar
34. Baun, W. L. and Fischer, D. W., “The Effect of Valence and Coordination on K series Diagram and Nondiagram Lines of Magnesium, Aluminum, and Silicon,” Advances in X-ray Analysis 8:371–383, (1964).Google Scholar
35. Mallett, G. R., Fay, M. J., and Mueller, W. M. (editors), “The Effect of Chemical Combination on X-ray Spectra: Open Discussion,” Advances in X-ray Analysis 9:393–397, (1965). See also papers preceding this discussion, pages 323-392.Google Scholar
36. Henke, B. L., Elgin, R. L., Lent, R. E., and Ledingham, R. B., “X-ray Absorption in the 2-to-200Å Region,” Norelco Reporter XIV:112–134, (1967).Google Scholar
37. Gunn, B. M., “Matrix Corrections for X-ray Fluorescence Spectrometry by Digital Computer,” Canadian Spectroscopy 12:1–7, (1967).Google Scholar
38. Traill, R. J. and Lachance, G. R., “A New Approach to X-ray Spectrochemical Analysis,” Canadian Dept. Hines Technical Survey Paper, p. 57–64, (1965).Google Scholar