Hostname: page-component-78c5997874-4rdpn Total loading time: 0 Render date: 2024-11-06T08:03:51.626Z Has data issue: false hasContentIssue false

Surface Preparation of Solid Metallic Samples for X-Ray Spectrochemical Analysis

Published online by Cambridge University Press:  06 March 2019

R.E. Michaelis
Affiliation:
National Bureau of Standards Washington, D.C
Betty Ann Kilday
Affiliation:
National Bureau of Standards Washington, D.C
Get access

Abstract

In X-ray spectrochemical determinations, the surface preparation of metal samples is important since the emitted secondary radiation is absorbed except for that emerging from the immediate surface. Surface preparation also has been found to be a critical factor in eliminating or at least in minimizing the effects of certain metallurgical changes among or within samples on the X-ray determinations. For example, a change of particle size of an undissolved constituent, or a change in grain size, may markedly influence the X-ray analysis, depending on the surface preparation. A metallographic polishing technique, whereby the sample surfaces were finished with ¼μ diamond dust, was reported for the determination of lead in leaded steel (Kilday and Michaelis, in press). This investigation has been extended to other materials such as hypereutectic silicon-aluminum alloy and white-cast iron. A comparison is made of the effects of different surface preparations on X-ray determinations.

Type
Research Article
Copyright
Copyright © International Centre for Diffraction Data 1961

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

1. Adler, I. and Axelrod, J. M., “Application at X-Ray Fluorescence Spectroscopy to Analytical Problems.” Norelco Reporter, Vol. 3, 1956, p. 65.Google Scholar
2. Claisse, P., “Accurate X-Ray Fluorescence Analyses Without Internal Standard,” Quebec Dept. Mines Prelim. Repr., No. 327, 1956.Google Scholar
3. Gunn, E. L., “Fluorescent X-Ray Spectral Analysis of Powdered Solids by Matrix Dilution,” Anal. Chem., Vol. 29, 1957, p. 184.Google Scholar
4. Liebhafsky, H. A. et al., X-Ray Absorption and Emission in Analytical Chemistry, John Wiley & Sons, New York, 1960, p. 173.Google Scholar
5. Scott, R. K., “Analysis of Clays, Bauxites and Other Silicates by the X-Ray Spectrograph,” Pittsburgh Conference on Analytical Chemistry and Applied Spectroscopy, Pittsburgh, Pa., March 1957.Google Scholar
6.The Standards are described in Natl. Bur, Standards (U.S.) Circ. 552, “Standard Materials Issued by the National Bureau of Standards,” This circular may be obtained from the Superintendent of Documents, U.S. Government Printing Office, Washington 25, D. C. for $.35. Supplementary Insert Sheets are issued periodically to revise the Circular, and these may be obtained free upon request from the Standard Sample Clerk, National Bureau of Standards, Washington 25, D.C.Google Scholar
7. Kilday, Betty A. and Michaelis, R. E., “Determination of Lead in Leaded Steels by X-Ray Spectroscopy” Appl. Spec., Vol. 16. Presented in part at the 8th Detroit Anachem Conference, October, 1960.Google Scholar
8. Michaelis, R. E. and Wyman, L. L., “Preparation and Evaluation of Eight NBS White-Cast Iron Spectroscopic Standards” (in press). Presented in part at the Pittsburgh Conference on Analytical Chemistry and Applied Spectroscopy, March 1961.Google Scholar