Abstract
An intercomparison was organized, with six laboratories tasked to quantify sixty-nine impurities in two uranium materials. The main technique employed for analysis was inductively coupled plasma mass spectrometry in combination with matrix-matched external calibration. The results presented highlight the current state-of-the-practice; lessons learned include previously unaccounted polyatomic interferences, issues related to sample dissolution, blank correction and calibration, and the challenge of estimating measurement uncertainties. The exercise yielded consensus values for the two analysed materials, suitable for use as laboratory standards to partially fill a gap in the availability of uranium reference materials characterized for impurities.
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Notes
The preparation of the U3O8 material was arranged by the Laboratoire Central d’Analyse et de Controle in Grenoble. A large uranium metal billet of industrial origin was molten together with a small uranium ingot carrying the trace elements. It was then converted to U3O8 by ignition under a stream of oxygen. The resulting U3O8 itself was milled, ground, and sieved in order to obtain a 100 mesh grain size powder. The whole batch was then homogenized, and the homogeneity was verified by six laboratories. In 1982 the French Government donated a batch of the resulting material to the IAEA.
Concentrations of Br and Cl impurities, not measured by any of the participating laboratories, remain undetermined.
Technical Meeting on Analysis of Elemental Impurities in Uranium Samples. IAEA, Vienna, 30 May–1 June 2012.
The certified atom (molar) ratios with respective expanded uncertainties (k = 2) are: 234U/238U = 0.00005472(76), 235U/238U = 0.0072568(36). Certified atom ratio 236U/238U is < 2 × 10−8.
Recent measurements at SAL using MTE MC-TIMS yielded the following atom (molar) ratios, traceable to CRM IRMM-184, with respective expanded uncertainties (k = 2): 234U/238U = 0.00005471(21), 235U/238U = 0.0072544(29), and 236U/238U < 5 × 10–9.
Recent measurements at SAL using MTE MC-TIMS yielded atom (molar) ratios traceable to CRM IRMM-184, with respective expanded uncertainties (k = 2): 234U/238U = 0.00005449(23), 235U/238U = 0.0072561(30), and 236U/238U < 1 × 10–8.
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Acknowledgments
Authors are grateful to Mikhail Ryzhinskiy for the in-depth discussions of the quality of analysis results on impurities in uranium samples, which led to the initiation of this interlaboratory comparison, and for his advice regarding the selection of test materials. Also acknowledged is the contribution of Zsolt Varga (ITU) who thoroughly reviewed the manuscript and provided valuable comments.
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S. Bürger: deceased.
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Bürger, S., Boulyga, S.F., Peńkin, M.V. et al. Quantifying multiple trace elements in uranium ore concentrates: an interlaboratory comparison. J Radioanal Nucl Chem 301, 711–729 (2014). https://doi.org/10.1007/s10967-014-3224-9
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DOI: https://doi.org/10.1007/s10967-014-3224-9