Hostname: page-component-78c5997874-dh8gc Total loading time: 0 Render date: 2024-11-02T21:10:48.459Z Has data issue: false hasContentIssue false
  • English
  • Français

Measurement of Mass Absorption Coefficients Using Compton-Scattered Cu Radiation in X-ray Diffraction Analysis

Published online by Cambridge University Press:  06 March 2019

Steve J. Chipera  and
David L. Bish
Steve J. Chipera
Affiliation:
Earth & Environmental Sciences Division Los Alamos National Laboratory Mail Stop D469, Los Alamos, NM 87545
David L. Bish
Affiliation:
Earth & Environmental Sciences Division Los Alamos National Laboratory Mail Stop D469, Los Alamos, NM 87545
Get access

Abstract

The mass absorption coefficient is a useful parameter for quantitative characterization of materials. If the chemical composition of a sample is known, the mass absorption coefficient can be calculated directly. However, the mass absorption coefficient must be determined empirically if the chemical composition is unknown. Traditional methods for determining the mass absorption coefficient involve measuring the transmission of monochromatic X-rays through a sample of known thickness and density. Reynolds (1963,1967), however, proposed a method for determining the mass absorption coefficient by measuring the Compton or inelastic X-ray scattering from a sample using Mo radiation on an X-ray fluorescence spectrometer (XRF). With the recent advances in solid-state detectors/electronics for use with conventional powder diffractometers, it is now possible to readily determine mass absorption coefficients during routine X-ray diffraction (XRD) analyses.

Using Cu Kα radiation and Reynolds’ method on a Siemens D-500 diffractometer fitted with a Kevex Si(Li) solid-state detector, we have measured the mass absorption coefficients of a suite of minerals and pure chemical compounds ranging in μ/ρ from graphite to Fe-metal (μ/ρ = 4.6-308 using Cu Kα radiation) to ±4.0% (lσ). The relationship between the known mass absorption coefficient and the inverse count rate is linear with a correlation coefficient of 0.997. Using mass absorption coefficients, phase abundances can be determined during quantitative XRD analysis without requiring the use of an internal standard, even when an amorphous component is present.

Type
VII. Solid State and Position-Sensitive Detectors for XRD
Information
Advances in X-Ray Analysis , Volume 34: Thirty-Ninth Annual Conference on Applications of X-ray Analysis, July 30 - August 3, 1990 , 1990 , pp. 325 - 335
Copyright
Copyright © International Centre for Diffraction Data 1990

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

Baron, P., Zevin, L., and Lack, S., 1981, Calculation of sample absorption by means of Compton scattering in X-ray diffraction analysis, X-Ray Spectrom., 10: 57.Google Scholar
Battaglia, S., and Leoni, L., 1977, Experimentally measured mass absorption coefficients in quantitative X-ray diffraction analysis, Anal. Chem., 49: 1168.Google Scholar
Beavers, A. H., and Olson, K. R., 1986, Use of Rayleigh scatter for determining X-ray mass absorption coefficients, Soil Sci. Soc. Am. J., 50: 1088.Google Scholar
Chung, F. H., 1974a, Quantitative interpretation of X-ray diffraction patterns of mixtures. I. Matrix-flushing method for quantitative multicomponent analysis, J. Appl. Cryst., 7: 519.Google Scholar
Chung, F. H., 1974b, Quantitative interpretation of X-ray diffraction patterns of mixtures, II, Adiabatic principle of X-ray diffraction analysis of mixtures, J. Appl. Cryst. 7: 526.Google Scholar
Compton, A. H., and Allison, S. K., 1935, “X-Rays in Theory and Experiment,” D. van Nostrand, Princeton, NJ.Google Scholar
Cullity, B. D., 1978, “Elements of X-Ray Diffraction,” Addison-Wesley, Reading, MA.Google Scholar
DeLong, S. E., and McCullough, D., 1973, Compton-scattered tungsten X-rays as a measure of mass absorption coefficients in rocks, Amer. Mia, 58: 1073.Google Scholar
Feather, C. E., and Willis, J. P., 1976, A simple method for background and matrix correction of spectral peaks in trace element determination by X-ray fluorescence spectrometry, X-Ray. Spectrom., 5;41.Google Scholar
Franzini, M., Leoni, L., and Santa, M., 1976, Determination of the X-ray mass absorption coefficient by measurement of the intensity of Ag Ka Compton scattered radiation, X-Ray Spectrom., 5: 84.Google Scholar
Giauque, R. D., Garrett, R. B., and Goda, L. Y., 1977, Energy dispersive X-ray fluorescence spectrometry for detennination of twenty-six trace and two major elements in geochemical specimens, Anal. Chem., 49: 62.Google Scholar
Goldstein, J. I., Newbury, D. E., Echlin, P., Joy, D. C. Fiori, C., and Lifshin, E. 1981, “Scanning Electron Microscopy and X-Ray Microanalysis,” Plenum Press, New York.Google Scholar
Harvey, P. K., and Atkin, B. P., 1982, The estimation of mass absorption coefficients by Compton scattering: Extension to the use of Rh Kα Compton radiation and intensity ratios, Amer. Mm., 67: 534.Google Scholar
International Tables for X-ray Crystallography, 1968, Physical and Chemical Tables, Vol. 111: 162. Jenkins, R., 1989, Instrumentation, in: “Reviews in Mineralogy: Modern Powder Diffraction,” D. L. Bish and J. E. Post, eds., Mineralogical Society of America, Washington, D. C., 20: 19.Google Scholar
Klug, H. P., and Alexander, L.E., 1974, “X-Ray Diffraction Procedures for Polycrystalline and Amorphous Materials,” Wiley, New York.Google Scholar
Reynolds, R. C. Jr., 1963, Matrix correction in trace element analysis by X-ray fluorescence: Estimation of the mass absorption coefficient by Compton scattering, Amer. Min., 48: 1133.Google Scholar
Reynolds, R. C. Jr., 1967, Estimation of mass absorption coefficients by Compton-scattering: Improvements and extensions of the method, Amer. Min., 52: 1493.Google Scholar
Sahores, J. J., 1973, New improvements in routine quantitative phase analysis by X-ray diffractometry, “Advances in X-ray Analysis,” Plenum Press, NY, 16: 186.Google Scholar
Sumartojo, J. and Paris, M. W., 1980, A method for measuring X-ray mass-absorption coefficients of geological materials, Chem. Geol., 28: 341.Google Scholar