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Thin-Film Analysis of Clay Particles Using Energy Dispersive X-Ray Analysis

Published online by Cambridge University Press:  02 April 2024

G. N. White ,
V. E. Berkheiser ,
F. N. Blanchard  and
C. T. Hallmark
G. N. White
Affiliation:
Soil Science Department, University of Florida, Gainesville, Florida 32611
V. E. Berkheiser
Affiliation:
Soil Science Department, University of Florida, Gainesville, Florida 32611
F. N. Blanchard
Affiliation:
Department of Geology, University of Florida, Gainesville, Florida 32611
C. T. Hallmark
Affiliation:
Department of Soil and Crops Science, Texas A&M University, College Station, Texas 77843
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Abstract

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A standardless method of energy dispersive X-ray fluorescence in conjunction with scanning electron microscopy was used to analyze selected areas of clay-size particles of talc, pyrophyllite, and kaolinite supported by a carbon planchet. Peak intensity ratios of fluorescing elements relative to silicon were converted directly to weight or mole ratios using conversion factors determined theoretically. The conversion factors depend upon particle thickness and mass adsorption coefficients of the sample for the elements analyzed. The effects of particle thickness become significant above ~0.1 μm. Without using particle thickness corrections, the mean molar ratios of metal to Si agreed to within 6.1,0.5, and 9.7% of the theoretical ratios for kaolinite, pyrophyllite, and talc, respectively.

Резюме

Резюме

Резюме—Использовался бесстандартный метод энергетическо-дисперсионной рентгеновской флуо-ресценции вместе сосканирующей электронной микроскопией для химического анализа выбран-ных мест частиц талька, пирофиллита, и каолинита о размере частиц глины, поддерживаемых угольной основой. Соотношения максимальной интенсивности флуоризуюших элементов по отно-шению к кремнию были превращены непосредственно в весовые или молярные соотношения, используя теоретически определенные факторы. Эти факторы зависят от толщины частиц и коеф-фициентов массовой адсорбции образца для анализированных элементов. Эффекты толщины частиц становятся значительными выше ~0,1 μим. Средние молярные соотношения металла к Si, без использования поправок на толщину частиц, согласовались с теоретическими соотношениями в пределах 6,1, 0,5, и 9,7% для каолинита, пирофиллита и талька, соответственно. [E.C.]

Resümee

Resümee

Eine standardfreie Methode der energiedispersiven Röntgenfluoreszenz in Verbindung mit Rasterelektronenmikroskopie wurde verwendet, um ausgewählte Bereiche von Talk, Pyrophyllit, und Kaolinit in der Größe der Tonfraktion chemisch zu untersuchen, die auf Kohlenstoffträgern aufgebracht waren. Die Peakintensitätsverhältnisse der fluoreszierenden Elemente im Vergleich zu Silizium wurden direkt in Gewichts- oder Molverhältnisse umgerechnet, wozu theoretisch bestimmte Umrechnungsfaktoren verwendet wurden. Die Umrechnungsfaktoren hängen von der Teilchengröße und von den Masseadsorptionskoeffizienten der Probe für die analysierten Elemente ab. Die Auswirkungen der Teilchendicke wurde über etwa 0,1 μm von Bedeutung. Ohne Korrektur der Teilchendicke weicht das durchschnittliche Molverhältnis Metall/Si für Kaolinit, Pyrophyllit bzw. Talk um etwa 6,1%, 0,5% bzw. 9,7% von den theoretischen Verhältnissen ab. [U.W.]

Résumé

Résumé

Une méthode sans standard de fluorescence de rayons-X dispersant l’énergie en conjonction avec la microscopie balayante à électrons a été utilisée pour analyser chimiquement des régions choisies de particules de talc, de pyrophyllite, et de kaolinite de taille de l'argile. Les plus hautes proportions d'intensité d’éléments fluorescents relativement à la silice ont été convertis directement en proportions de poids, ou molaires en utilisant des facteurs de conversions déterminés théoriquement. Les facteurs de conversion dépendent de l’épaisseur et des coefficients d'adsorption de masse de l’échantillon pour les éléments analysés. Les effets de l’épaisseur de la particule devenaient significatifs au dessus d’ ~0,l μm. Sans utiliser les corrections pour l’épaisseur de particule, les proportions molaires moyennes du métal à la silice s'accordaient à 6,1, 0,5, et 9,7% près avec les proportions théoriques pour la kaolinite, la pyrophyllite, et le talc, respectivement. [D.J.]

Keywords

Chemical analysisEnergy dispersive X-ray analysisKaoliniteParticle thicknessPyrophylliteScanning electron microscopyTalc
Type
Research Article
Information
Clays and Clay Minerals , Volume 30 , Issue 5 , October 1982 , pp. 375 - 382
Copyright
Copyright © 1982, The Clay Minerals Society

Footnotes

1

Contribution from the Agricultural Experiment Station, University of Florida, Journal Series No. 3342.

References

Berkheiser, V. E. and Monsees, M. B. (1982) Dispersion of clays on graphite supports for X-ray microprobe analysis: Soil Sci. Soc. Amer. J. 46 (in press).CrossRefGoogle Scholar
Brindley, G. W. and Wardle, R., 1970 Monoclinic and triclinic forms of pyrophyllite and pyrophyllite anhydride Amer. Minerai. 55 1259–1272.Google Scholar
Cliff, G. and Lorimer, G. W., 1975 The quantitative analysis of thin specimens J. Microsc. 103 203–207.CrossRefGoogle Scholar
Colby, J. W., 1968 Quantitative microprobe analysis of thin insulating films Adv. X-Ray Anal. 11 287–305.Google Scholar
Duncomb, P., 1962 Enhanced X-ray emission from extinction contours in a single-crystal gold film Phil. Mag. 7 2101–2105.CrossRefGoogle Scholar
Goldstein, J. I., Colby, J. W., Goldstein, J. I. and Yakowitz, H., 1975 Special techniques in the X-ray analysis of samples Practical Scanning Electron Microscopy New York Plenum Press 435–490.CrossRefGoogle Scholar
Goldstein, J. I., Costley, J. L., Lorimer, G. W. and Reed, S. J. B., 1977 Quantitative X-ray analysis in the electron microscope SEM 197. 1 315–325.Google Scholar
Hirsch, P. B., Howie, A. and Whelan, M. J., 1962 On the production of X-rays in thin metal films Phil. Mag. 7 1095–2100.CrossRefGoogle Scholar
König, R. and Wenk, H. R., 1976 Quantitative X-ray microanalysis of thin foils Electron Microscopy in Mineralogy New York Springer-Verlag 526–536.CrossRefGoogle Scholar
McCrary, H. J., Singman, L. V., Ziegler, L. H., Looney, L. D., Edmonds, C. M. and Harris, E., 1971 K-fluorescent X-ray relative intensity measurements Phys. Rev. A4 1745–1750.CrossRefGoogle Scholar
Namae, T., 1975 A method for quantitative analysis for thin specimens by energy dispersive spectrometer fitted to transmission electron microscope J. Electron Microsc. 24 1–6.Google Scholar
Philibert, J., Tixier, R., Siegel, B. and Beaman, D. R., 1975 Electron probe microanalysis of transmission electron microscope specimens Physical Aspects of Electron Microscopy and Microbeam Analysis,. New York Wiley 333–354.Google Scholar
Reed, S. J. B., 1975 Electron Microprobe Analysis. New York Cambridge University Press 308–310.Google Scholar
Slivinsky, V. W. and Ebert, P. J., 1972 Kß/K. X-ray transition-probability ratios for elements 18 « Z ss 39 Phys. Rev. A5 1581–1586.CrossRefGoogle Scholar
Stemple, I. S. and Brindley, G. W., 1960 Structural study of talc and talc-tremolite relations J. Amer. Ceram. Soc. 43 34–42.CrossRefGoogle Scholar
Zaluzec, N. J., 1978 An analytical electron microscope study of the omega phase transformation in a zirconium-niobium alloy Oak Ridge National Laboratory Report ORNL/TM6705 Virginia National Technical Information Service, Spring-field.Google Scholar
Zaluzec, N. J., Hren, J. J., Goldstein, J. I. and Joy, D. C., 1979 Quantitative X-ray microanalysis: Instrumental considerations and applications to materials science Introduction to Analytical Electron Microscopy New York Plenum Publishing Corp. 121–167.CrossRefGoogle Scholar