Hostname: page-component-586b7cd67f-l7hp2 Total loading time: 0 Render date: 2024-11-23T11:37:08.986Z Has data issue: false hasContentIssue false
  • English
  • Français

Micro Fluorescent X-Ray Analyzer

Published online by Cambridge University Press:  06 March 2019

Toshio Shiraiwa  and
Nobukatsu Fujino
Toshio Shiraiwa
Affiliation:
Central Research Laboratories, Sumitomo Metal Industries Amagasaki, Japan
Nobukatsu Fujino
Affiliation:
Central Research Laboratories, Sumitomo Metal Industries Amagasaki, Japan
Get access

Abstract

A micro fluorescent X-ray analyzer with a focusing type of spectrometer has been developed to analyze samples of small amounts such as extracted inclusions or precipitates from metals or small areas in samples from 0.1 to 2.0 mm in diameter. This instrument is expected especially to analyze powder samples of small quantity because average values from such samples can be obtained and because surface conditions of the samples scarcely affect the results compared with their effect in electron probs microanalysis. A commercial X-ray tube is combined with a device of slits limiting incident X-rays, a focusing spectrometer with a Rowland circle of 4-in. radius, and a microscope of low magnification for observing the analyzing point on the samples. The wavelength range of the spectrometer with LiF and ADP analyzing crystals is from 1.20 to 9.94 Å, and, therefore, higher elements than aluminum in atomic number can be analyzed. The authors exerted their efforts to obtain the higher X-ray intensities in order to analyze smaller areas. The X-ray intensities obtained are satisfactory, except for light elements. For example, the detected X-ray intensity of pure nickel is 1650 cps with the use of a 0.1-mm diameter specimen, and that of pure sulfur is 52 cps with the use of a 0.1-ramdiameter specimen; however, with a 1-mm-diameter specimen, the intensity of pure nickel is over 5000 cps and that of pure sulfur is 1650 cps. These correspond to the intensities from 20-mm-diameter specimens of those elements when a flat-crystal spectrometer is used. The calibration curve for quantitative analysis generally varies with the sample area under analysis, but the same curves are obtained if the sample area is larger than 1 mm in diameter. Then, powder samples are analyzed quantitatively by using a plastic sample holder of 1-mm diameter and 0.3-mm depth. This instrument has good ability for microanalyzing trace elements by, for example, the ion-exchenge membrane method. The sensitivity represented is nearly 5000 cps/μg for Ni Kα from NiSO4 that is soaked and dried in thin rice paper. Some applications of the micro fluorescent X-ray analyzer to precipitates in steels and corrosion products are reported.

Type
Research Article
Information
Advances in X-Ray Analysis , Volume 11: Sixteenth Annual Conference on Applications of X-ray Analysis, August 9-11, 1967 , 1967 , pp. 95 - 104
Copyright
Copyright © International Centre for Diffraction Data 1967

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. Thatcher, J. W. and Campbell, W. J., Fluorescent X-Ray Spectrographs Probe-Design and Applications, U.S. Bur. Mines Rept. Invest. 5500, 1959.Google Scholar
2. Adler, I. A., Axelrod, J., and Branco, J. J. E., “Further Application of the Intermediate X-Ray Probe,” in; W. M. Mueller (ed.), Advances in X-Ray Analysis, Vol. 2, Plenum Press, New York, 1960, p. 167.Google Scholar
3. Despujols, J., Roulet, H., and Seneraaud, G., “X-Ray Fluorescence Analysis with a Focused Primary Beam,” in: H. H. Pattee, V. E. Cosslett, and A. Engstrom (eds.), X-Ray Optics and X-Ray Microanalysis, Academic Press, New York, 1963, p. 445.Google Scholar
4. Long, J. V. P. and Rockert, H. O. E., “X-Ray Fluorescence Microanalysis and the Determination of Potassium in Nerve Cells,” in: H. H. Pattee, J. E. Cosslett, and A. Engstrom (eds.), X-Ray Optics and X-Ray Microanalysis, Academic Press, New York, 1963, p. 513.Google Scholar
5. Miller, D. C., “Norelco Pinhole Attachment,” in: W. M. Mueller (cd.), Advances in X-Ray Analysis, Vol. 5, Plenum Press, New York, 1961, p. 513.Google Scholar
6. Campbell, W. J., “Fluorescent X-Ray Spectrographic Analysis of Trace Elements, Including Thin Films,” ASTM STP No. 349, p. 48, 1964.Google Scholar
7. Lund, P. K., “X-Ray Fluorescence.Spectroscopy in Biology and Medicine,” in: H. H. Pattee, V. E. Cosslett, and A. Engstrom (eds.), X-Ray Optics and X-Ray Microanalysis, Academic Press, New York, 1963, p. 523.Google Scholar
8. Shiraiwa, T. and Matsuno, F., “Identification of Scales of Heavy Oil-Fired Boilers by X-Ray Diffraction Method,” Tetsu To Hagane 52: 1592–1594, 1966.Google Scholar
9. Pfeiffer, H. G. and Zemany, P. D., “Trace Analysis by X-Ray Emission Sp echography,” Nature 174: 397, 1954.Google Scholar
10. Liebhafsky, H. A., Pfeiffer, H. G., Winslow, E. H., and Zemany, P. D., X-Ray Absorption and Emission in Analytical Chemistry, John Wiley & Sons, New York, 1960.Google Scholar
11. Birks, L. S., “Comparison of X-Ray Fluorescence and Electron Probe Methods: Future Trends,” ASTM STP No. 349, p. 151, 1964.Google Scholar