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A Sampling Method for Semi-Quantitative and Quantitative Electron Microprobe Analysis of Glass Surfaces

Published online by Cambridge University Press:  19 May 2015

Jamie L. Weaver
Affiliation:
Washington State University, Chemistry Department, Pullman, WA 99164, USA
Joelle Reiser
Affiliation:
Washington State University, Chemistry Department, Pullman, WA 99164, USA
Owen K. Neill
Affiliation:
Washington State University, Chemistry Department, Pullman, WA 99164, USA
John S. McCloy
Affiliation:
Washington State University, Chemistry Department, Pullman, WA 99164, USA
Nathalie A. Wall
Affiliation:
Washington State University, Chemistry Department, Pullman, WA 99164, USA
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Abstract

The determination of the long-term stability and corrosion of vitrified nuclear waste is an important aspect of research for the U.S. Department of Energy (DOE). It is necessary to understand the rate and mechanisms of Nuclear Waste Glass (NWG) corrosion to determine whether or not the glassy matrix will be able to retain radionuclides for the required repository performance time period. Glass corrosion and the rate of glass corrosions is determined by both chemical and microscopy. Electron Microprobe Analysis (EPMA) is a common and powerful method utilized in the examination of the chemographic difference between corroded and uncorroded NGWs. In this work, two forms of quantitative and semi-quantitative EPMA methods are defined by optimizing the instruments counting statistics against a standard glass and NIST minerals that have compositions similar to the glasses under examination. Data collected on both the planar and cross-sectioned surfaces of an unaltered simulated NWG by Standard based Wavelength Dispersive Spectroscopy (WDS) was found to be comparable to the theoretical composition of the glass. Conventional standardless Energy Dispersive Spectroscopy (EDS) data collected on the same surfaces was not comparable. However, standard-based EDS analysis is shown to be able to discriminate between unaltered and corroded glass surfaces.

Type
Articles
Copyright
Copyright © Materials Research Society 2015 

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References

REFERENCES

Melcher, M., Wiesinger, R., and Schreiner, M., Acc. Chem. Res. 43, 916926 (2010).CrossRefGoogle Scholar
Bellendorf, P., Gerlach, G., Mottner, P., López, E., in Glass & Ceramic Conservation 2010, edited by Roemich, H., (Inter. Coun. Muse. Symp. Proc. Corning, New York, Jun 2010), 137143.Google Scholar
Bingham, P. and Jackson, C.M., J. Archaeol. Sci. 35, 302309 (2008).CrossRefGoogle Scholar
Gin, S., Abdelouas, A., Criscenti, L.J., Ebert, W.L., Ferrand, K., Geisler, T., Harrison, M.T., Inagaki, Y., Mitsui, S., Mueller, K.T., Marra, J.C., Pantano, C.G., Pierce, E.M., Ryan, J.V., Schofield, J.M., Steefel, C.I., Vienna, J.D., Mater. Today. 16, 243248 (2013).CrossRefGoogle Scholar
Boudreault, J.P., Dubé, J.S., Sona, M., , Hardy, E, E. Sci. Total Environ. 425, 199207, (2012).CrossRefGoogle Scholar
Geisler, T., Janssen, A., Scheiter, D., Stephan, T., Berndt, J., Putnis, A., J. Non. Cryst. Solids. 356, 14581465 (2010).CrossRefGoogle Scholar
Newbury, D. E., Microsc. Microanal. 11, 545561 (2005).CrossRefGoogle Scholar
ASTM C1285. Annual Book of ASTM Standards, Vol. 12.01: Standard Test Methods for Determining Chemical Durability of Nuclear, Hazardous, and Mixed Waste Glasses and Multiphase Glass Ceramics: The Product Consistency Test (PCT) Google Scholar
Bastin, G. F., Dijkstra, J. M., and Heijligers, H. J. M., X-Ray Spectrom. 27, 310, (1998).3.0.CO;2-L>CrossRefGoogle Scholar
Inagaki, Y., Kikunaga, T., Idemitsu, K., and Arima, T., Int. J. Appl. Glas. Sci. 4, 317327 (2013).CrossRefGoogle Scholar
Chaussidon, M., Robert, F., Mangin, D., Hanon, P., and Rose, E.F., Geostandards Newsletter 21, 717 (1997).CrossRefGoogle Scholar