Quantitative SEM/EDS analysis of high-level waste glasses
- and others
Silicate glass will be used to stabilize high-level radioactive wastes (HLW) for disposal in a geological repository. The chemical durability of waste glass in the repository will be determined by the nature and progress of the glass-water (underground water) reaction. Aqueous corrosion of HLW glasses is known to result in the chemical alteration of the glass surface and the formation of secondary phases. Accurate quantitative analysis the altered glass surface and the reaction products that form is important for understanding the reaction kinetics and mechanism of glass corrosion. SEM/EDS is a powerful tool to study the alteration of waste-disposal glasses through quantitatively characterizing the reaction products. It is able to detect trace elements at concentrations less than 1 wt.%: for example, Fig. 1 shows the uranium peaks detected by SEM/EDS of a typical simulated waste glass, which contains 0.25 wt.% uranium in the matrix glass according to ICP/MS analysis. Nickel (0.44 wt.%) and chromium (0.47 wt.%) peaks are also clearly distinguishable in the spectrum. However, quantitative analyses of glass compositions are complicated by the lack of well-characterized reference samples having known and homogeneous compositions for candidate waste glasses, which may contain a combination of more than 20 different elements in one matrix. It has been proposed that unreacted glass with known compositions could satisfactorily serve as standards for quantitative analysis of waste-disposal glasses and the secondary phases. The main advantage of using such standards is that they contain all the elements to be analyzed in the homogeneous vitreous matrices. In this paper, we evaluate several reference waste glasses with respect to their suitability as standard samples for quantitative SEM/EDS analysis. The precision and accuracy using such standards for quantitative analysis are also discussed. All the experiments were carried out on a Topeon ABT 60 SEM operating at 20 kV.
- Research Organization:
- Argonne National Lab. (ANL), Argonne, IL (United States)
- Sponsoring Organization:
- USDOE, Washington, DC (United States)
- DOE Contract Number:
- W-31109-ENG-38
- OSTI ID:
- 83799
- Report Number(s):
- ANL/CMT/CP-86025; CONF-950865-4; ON: DE95014080; TRN: 95:017271
- Resource Relation:
- Conference: 29. annual meeting of the Microbeam Analysis Society, Breckenridge, CO (United States), 6-11 Aug 1995; Other Information: PBD: Mar 1995
- Country of Publication:
- United States
- Language:
- English
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