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Direct Assay for Molybdenum and Ruthenium in Uranium Alloys by X-Ray Emission Spectrometry

Published online by Cambridge University Press:  06 March 2019

D. S. Flikkema
Affiliation:
Argonne National Laboratory, Lemont, Illinois
R. V. Schablaske
Affiliation:
Argonne National Laboratory, Lemont, Illinois
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Abstract

It has been found possible to determine quickly the concentrations of molybdenum and ruthenium in non-radioactive alloys representative of high burn-up reactor fuels by the method of X-ray emission spectrometry. Preliminary steps of chemical dissolution and separation are not required. The alloys, essentially ternaries of molybdenum and ruthenium with uranium, are being studied because they are considered to typify the alloys which will result from cycling uranium fuel elements through the sequence of fabrication, use and pyro.metallurgical processing.

The analytical procedure involves sampling of the ingot by slicing with a silicon carbide wheel at the plane of interest and reducing the surface to the flatness and finish obtained by a five-minute grinding and polishing operation. In the X-ray spectrograph the flat surface is examined for the intensities of its molybdenum and ruthenium K emission lines, with counting times of one to eight minutes. Calibration plots of intensity versus chemically determined weight per cent are established and used for subsequent sets of analyses.

Type
Research Article
Copyright
Copyright © International Centre for Diffraction Data 1957

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References

page 387 note * The selective oxidation of zirconium in a uranium matrix depends on a precise set of conditions; its removal in pilot plant-scale processing remains to be demonstrated.

page 388 note * Recently additional alloys, up to 14 weight per cent molybdenum and 10 weight per cent ruthenium, have been made to permit more careful definition, of so.me factors in the method as well as to extend its applicability.

page 389 note * Specimens designated with the same Arabic number were taken from the same ingot, A from one end, B from the other. Designations such as 2E, 2EAA, and 2EAB indicate that a given ingot was initially sliced to give specimen 2E and that subsequently specimens 2EAA and 2EAB were taken from the ends of the remaining piece.

page 397 note * When heterogeneity in a specimen surface is suspected, a more representative and reproducible analysis can be obtained by the usual technique of rotating the specimen in its own plane to integrate out the nonuniforrmty of the exciting beam.