Hostname: page-component-78c5997874-4rdpn Total loading time: 0 Render date: 2024-11-05T05:44:41.622Z Has data issue: false hasContentIssue false

A Versatile X-Ray Fluorescence Method for the Analysis of Sulfur in Geologic Materials

Published online by Cambridge University Press:  06 March 2019

H. N. Elsheimer
Affiliation:
U. S. Geological Survey, Menlo Park, California 94025
B. F. Fabbi
Affiliation:
U. S. Geological Survey, Menlo Park, California 94025
Get access

Abstract

Nonproportionality of X-ray fluorescence intensity vs. concentration of sulfur occurs in geologic materials prepared as ground samples. Samples containing sulfur as sulfate yield higher intensities than an equivalent amount of sulfur as the Sulfide. Although the intensity of free sulfur decreases markedly during a short exposure to X-rays in a vacuum, and sulfide intensities decrease over a much longer time period, sulfate intensities show no deterioration with time.

A fusion procedure utilizing a LiBO2-Ce(NH4)2(NO3)5 flux has been developed for geologic materials to oxidize all sulfur in a multiplicity of oxidation states to a single oxidation state, namely, the sulfate. The procedure is applicable over a wide range of concentrations (0.5 - 28 wt. % total sulfur) with a detection limit of 0.01%. A suite of chemically analyzed rocks containing both sulfides and Sulfates is used for standardization.

Type
Research Article
Copyright
Copyright © International Centre for Diffraction Data 1973

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. Parratt, L. G., “Effect of Chemical Binding on the X-ray Kα1,2 Doublet Lines of Sulfur Studied with a Two Crystal Spectrometer,Phys. Rev., 49, 1416 (1936).Google Scholar
2. White, E. W., McKinstry, H. A. and Bates, T. F., “Crystal Studies by X-ray Fluorescence,” Advances in X-Ray Analysis, Vol. 2, Plenum Press, 239–45 (1960).Google Scholar
3. Faessler, A and Goehring, M., “X-Ray Spectrum and Bond Characteristics; Kα Fluorescence Radiation of Sulfur.Naturwiss., 39, 169177 (1952).Google Scholar
4. Faessler, A and Mecke, P., “Bonding in Sulfides and Polysulfides,Z. Electrochem., 64, 587591 (1960).Google Scholar
5. Gianturco, F. A. and Coulson, C. A., “Influence of Chemical Combination on K Fluorescence Lines of Compounds of Aluminum, Silica, ancl Sulfur,” Inorg. Chim. Acta, 3(4), 607611 (1969).Google Scholar
6. Conti, D and Estour, H., “Chemical Effect on Wavelength of Characteristic X-Rays. Application Test,” J. Microsc. (Paris), 15(3), 297303 (1972).Google Scholar
7. Fabbi, B. P., “A Refined Fusion X-Ray Fluorescence Technique and Determination of Major and Minor Elements in Silicate Standards,Amer. Mineral., 57, 237245 (1972).Google Scholar
8. Fabbi, B. P., “A Die for Pelletizing Samples for X-Ray Fluorescence Analysis,” U.S. Geol. Surv. Prof. Paper 700B, B187-B189 (1970).Google Scholar
9. Fabbi, B. P. and Moore, W. J., “Rapid X-Ray Fluorescence Determination of Sulfur in Mineralized Rocks from the Bingham Mining District, Utah,Appl. Spectrosc, 24, 426428 (1970).Google Scholar