Hostname: page-component-586b7cd67f-2brh9 Total loading time: 0 Render date: 2024-11-27T04:51:58.896Z Has data issue: false hasContentIssue false

Application of a Computer-Coupled Radioisotope X-Ray Spectrometer to Analysis of Steels

Published online by Cambridge University Press:  06 March 2019

J. R. Rhodes
Affiliation:
Columbia Scientific Research Institute, 3625 Bluestein Blvd., Austin, Texas
C. B. Hunter
Affiliation:
Columbia Scientific Research Institute, 3625 Bluestein Blvd., Austin, Texas
D. L. Kellogg
Affiliation:
Columbia Scientific Research Institute, 3625 Bluestein Blvd., Austin, Texas
R. D. Sieberg
Affiliation:
Columbia Scientific Research Institute, 3625 Bluestein Blvd., Austin, Texas
T. Furuta
Affiliation:
Columbia Scientific Research Institute, 3625 Bluestein Blvd., Austin, Texas
Get access

Abstract

A compact X-ray energy spectrometer has been developed consisting essentially of a radioisotope X-ray source, a lithium-drifted silicon (or germanium) detector and a small computer. Interchangeable sources enable efficient excitation of K X-rays from Na to U and L X-rays from about Ag to U. Energy resolution of K X-rays from adjacent elements down to Na is possible. Depending on the source and the part of the spectrum examined, the characteristic X-rays from up to about 15 elements can be simultaneously excited and measured, for either qualitative or quantitative multi-element analysis. The computer stores detected spectra and performs simple data processing such as peak recognition, background subtraction, peak integration, ratioing and solution of linear equations.

The analysis reported in this paper is the determination of V, Cr, Fe, Co, W and Mo in tool steels and is intended to illustrate the capabilities of the radioisotope X-ray fluorescence analysis technique, and the instrument, for multi-element analysis of a system having fairly complex interelement effects.

A 100 mCi Pu-238 source was used to excite the K X-rays of V, Cr, Fe, Co and Mb and the L X-rays of W. The count time used was five minutes per sample. Data reduction consisted essentially of peak integration, background subtraction and solution of sixth order linear matrices of a modified Criss-Birks type. The 36 matrix coefficients were determined using six standards, and were then used to analyze seven other analyzed specimens which were treated as unknowns. The measured values of concentration were in very good agreement with the quoted values. An iteration technique was employed to reduce errors in the matrix inversioiis.

Type
Research Article
Copyright
Copyright © International Centre for Diffraction Data 1970

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

“Energy Dispersion X-Ray Analysis , “ ASTM Special Technical Publication 485 (1971).Google Scholar
Rhodes, J. R., “Radioisotope X-Ray Spectrometry - A Review”, The Analyst, Vol. 91, pp. 683699 (1966).Google Scholar
Rhodes, J. R. and Furuta, T., “Appication of a Portable Radioisotope X-Ray Fluorescence Spectrometer to Analysis of Minerals and Alloys,” in Advances in X-Ray Analysis, Newkirk, J. B., Mallett, G. R. and Pfeiffer, H. G., Editors, Vol. 11, pp. 249274, Plenum Press (1968).Google Scholar
Lucas-Tooth, H. J. and Price, B. J., “A Mathematical Method for the Invsetigation of Interelement Effects in X-Ray Fluorescent Analyses,” Metallurgia, Vol. 54, No. 363, pp. 149152 (1961).Google Scholar
Lucas-Tooth, H. J. and Pyne, C., “The Accurate Determination of Major Constituents by X-Ray Fluorescent Analysis in the Presence of Large Interelement Effects,” Mueller, W. M., Mallett, G. R. and Fay, M. J., Editors, Advances in X-Ray Analysis, Vol 7, pp. 523541 (1964).Google Scholar
Gillieson, A. H., Reed, D. J., Milliken, K. S. and Young, M. J., “X-Ray Spectrochemical Analysis of High Temperature Alloys,” In ASTM Special Technical Publication Mo. 376, ASTM (1964).Google Scholar
Alley, B. J. and Myers, R. H., “Corrections for Matrix Effects in X-Ray Fluorescence Analysis Using Multiple Regression Methods,” Anal. Chem., Vol 37, No. 13, pp. 16851690 (1965).Google Scholar
Criss, J. W. and Birks, L. S., “Calculational Methods for Fluorescent X- ray Spectrometry,” Anal. Chem. Vol 40, No. 7, pp. 10801086 (1968).Google Scholar