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X-Ray Absorption-Edge Determination of Cobalt in Complex Mixtures*

Published online by Cambridge University Press:  06 March 2019

E.A. Hakkila  and
G.R. Waterbury
E.A. Hakkila
Affiliation:
University of California, Los Alamos Scientific Laboratory, Los Alamos, New Mexico
G.R. Waterbury
Affiliation:
University of California, Los Alamos Scientific Laboratory, Los Alamos, New Mexico
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Abstract

The application of the X-ray absorption-edge technique was extended to the determination of cobalt in aqueous and alcoholic solutions containing a wide variety of impurity elements. In the procedure developed, secondary radiation from a 50% copper-nickel alloy is passed through an absorption cell filled alternately with the solvent and the sample solution. The transmitted Intensities of the Kα lines for copper and nickel are measured, and the concentration of cobalt is determined using accepted absorption principles. The K absorption edge for cobalt occurs at 1.604 A, restricting cell construction materials and solvents to those containing light elements with low X-ray absorption characteristics and also limiting the path length of the cell.

Cells of 0.16- and 0.34-cm path length were used in the analysis of aqueous and alcoholic solutions, respectively. With the 0.16-cm path-length cell, relative standard deviations of 4.6 to 0.5% were obtained for cobalt concentrations ranging from 1.00 to 10.00 mg/ml for known aqueous solutions that contain various known concentrations of nitric acid. With the longer path-length cell, relative standard deviations from 1.8 to 0.46% were obtained for cobalt concentrations in the same range in known alcoholic solutions containing various known concentrations of nitric acid. The standard deviation of determining the blank is 0.043 mg of cobalt per milliliter for the 0.16-cm cell and 0.016 mg of cobalt per milliliter for the longer cell.

A Norelco X-ray spectrograph with a three-position head was used in these analyses. Less than 5 min is required to convert this instrument from normal fluorescence operation to absorption-edge analysis. Approximately 15 to 20 analyses can be performed daily.

Type
Research Article
Information
Advances in X-Ray Analysis , Volume 5: Tenth Annual Conference on Applications of X-ray Analysis, August 7-9, 1961 , 1961 , pp. 379 - 388
Copyright
Copyright © International Centre for Diffraction Data 1961

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Footnotes

*

Work performed under the auspices of the U. S. Atomic Energy Commission.

References

1. Barieau, R. H., “X-Ray Absorption Edge Spectrometry as an Analytical Tool,” Anal. Chem., Vol. 19, No. 3, March 1957, p. 348.Google Scholar
2. Dietrich, W. C. and Barringer, R. E., “The Determination of Molybdenum in Uranium-Molybdenum Alloys by Monochromatic X-Ray Absorption,” U.S. Atomic Energy Comm, Rapt, Y-1153, February 21, 1957.Google Scholar
3. Dodd, C. G., “Applications of Optical and Electronic Dispersion to X-Ray Absorption Edge gpectromeiry,” Advances in X-Ray Analysis, Vol. 3, University of Denver, Plenum Press, 1960, p. 11.Google Scholar
4. Peed, W. F. and Dunn, H. W., “Preliminary Investigations of Monochromatic X-Ray Absorption as a Method of Analysis for Uranium,” U. S. Atomic Energy Comm. Rept. ORNL-1265, April 8, 1952.Google Scholar
5. Stewart, J. H. Jr., “Determination of Thorium by Monochromatic X-Ray Absorption,” Anal. Chem., Vol. 32, No. 9, August, 1960, p. 1090.Google Scholar
6. Wright, W. B. and Barringer, R. E., “Uranium Analysis by Monochromatic X-Ray Absorption,” U.S. Atomic Energy Comm. Rept. Y-1095, August 26, 1955.Google Scholar
7. Hughs, H. R. and Hochgesang, F. B., “X-Ray Absorption Sipectrometryfor Determination of Tetraethylead in Gasoline,” Anal. Chem., Vol. 22, No. 10. October. 1950, p. 1248.Google Scholar
8. Hakkila, E. A., “X-Ray Absorption Edge Determiation of Uranium in Complex Mixtures,” Anal. Chem, Vol. 33, No. 8, 1961, p. 1012.Google Scholar
9. Engstrom, A., “Quantitative Micro- and Histochemical Elementary Analysis by Roentgen Absorption Spectrograph,” Acta Radiol. Supp., Vol. 63, 1946.Google Scholar
10. Compton, A. H. and Allison, S. K., “X-Ray in Theory and Experiment,” 2nd ed., D. Van Nostrand Company, Inc., Princeton, N.J., 1935, pp. 800–806.Google Scholar