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Determination of Calcium in Wolframite Concentrates by Fluorescent X-Ray Spectrography

Published online by Cambridge University Press:  06 March 2019

William J. Campbell  and
John W. Thatcher
William J. Campbell
Affiliation:
U. S. Department of the Interior, Bureau of Mines, Eastern Experiment Station, College Park, Maryland
John W. Thatcher
Affiliation:
U. S. Department of the Interior, Bureau of Mines, Eastern Experiment Station, College Park, Maryland
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Abstract

The purpose of this investigation was to develop a rapid, accurate method of analysis for small amounts of calcium in wolframite concentrates. This analysis is necessary to determine if wolframite concentrates meet the U. S. National Stockpile Specification P-57R2, which limits the calcium content to 0.2 per cent.

Because of the small depth of sample analyzed in fluorescent x-ray spectrography the calcium Kα line intensity was found to be a function of the chemical composition of the calcium-bearing particle as well as the matrix composition. This particle-conn position effect was particularly important in this analysis because the calcium may be present as a carbonate, tungstate, phosphate, etc. Three methods of sample preparation were found to eliminate the variation of calcium Kα intensity with mineralogical occurrences: (1) Reduction in particle size by extensive grinding, (2) chemical fusion wtli sodium carbonate, and (3) solution of the calcium by an add.

Determinations by all three procedures are believed to be accurate to within ± 5 per cent for more than 0.30 per cent calcium and ± 10 per cent at the 0.1-per cent level. The lower limit of detectability is in the order of 0.005-0.01 per cent.

The operating characteristics of a gas-flow proportional counter used in conjunction with a pulse-height analyzer were studied in detail. This detector was found to have a high counting efficiency for calcium Ka radiation, to have a low counting efficiency for overlapping higher order radiation and to have counting stability equivalent to Geiger tubes.

Type
Research Article
Information
Advances in X-Ray Analysis , Volume 2: Seventh Annual Conference on Industrial Applications of X-ray Analysis, August 13-15, 1958 , 1958 , pp. 313 - 332
Copyright
Copyright © International Centre for Diffraction Data 1958

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References

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