Plutonium assay by spectrophotometry and estimation of uncertainties on routine glove box samples
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Plutonium assay by spectrophotometry and estimation of uncertainties on routine glove box samples Alexandre Ruas1 · Shuuji Yamazaki2 · Kenichi Mise2 · Yoshiyasu Kato2 · Andreas Starzer3 · Dante R. Nakazawa1 · Konstantinos Raptis1 · Chang‑Kyu Kim1 · Georges E. Duhamel1 Received: 6 June 2020 © Akadémiai Kiadó, Budapest, Hungary 2020
Abstract Plutonium(VI) spectrophotometry is a precise analytical method for determining the concentration of plutonium solutions. It is simple and cost-effective to implement in nuclear environments such as glove boxes and hot-cells. Uncertainties were assessed at 0.64% (k = 1) for solutions of 0.150 mg g−1 initially prepared in a glove box. The critical limit of the method was estimated at 0.002 mg g−1 at 99% confidence. The good performances of the technique in the present work are due to a rigorous spectra processing as well as preparation steps conducted by weight control. Keywords Analysis · Spectrophotometry · Assay · Plutonium · Uncertainty
Introduction The development of high accuracy and reliable analytical techniques is essential for analytical laboratories in the nuclear field [1, 2]. This includes safeguards applications on solutions containing plutonium to ensure that protracted diversion of nuclear materials has not occurred and to verify the quality of the operator’s measurement system. To that end, the On-Site Laboratory (OSL) at the Rokkasho Reprocessing Plant (RRP) in Japan, jointly operated by the IAEA and the Japanese authority mandated technical agency, Nuclear Material Control Centre (NMCC), routinely uses Electronic supplementary material The online version of this article (https://doi.org/10.1007/s10967-020-07369-1) contains supplementary material, which is available to authorized users. * Alexandre Ruas [email protected] 1
Onsite Laboratory Team, Nuclear Material Laboratory, Office of Safeguards Analytical Services, Department of Safeguards, International Atomic Energy Agency, Tokyo Regional Office, Seibunkan Bldg, 9F, 1‑5‑9 Iidabashi, Chiyoda‑ku, Tokyo 102‑0072, Japan
2
Nuclear Material Control Centre (NMCC), 504‑36 Nozuki Obuchi, Rokkasho, Aomori 039‑3212, Japan
3
IAEA Laboratories, Office of Safeguards Analytical Services, Department of Safeguards, International Atomic Energy Agency, Friedensstrasse 1, 2444 Seibersdorf, Austria
and develops analytical techniques that are highly accurate and fit for plutonium routine analysis [3]. In the nuclear field, spectrophotometry is well-known for semi-quantitative speciation [4–7] or online analysis [8–10]. In the case dedicated reagents are added, spectrophotometry can be used for quantitative assays, with many advantages for routine safeguards analysis: simplicity, good accuracy, robustness, time-effectiveness, and cost-effectiveness [10–12]. Thanks to the use of optical fibers spectrophotometry can be easily installed in a nuclear environment, including in hot-cell [11]. The general principle relies on the quantitative oxidation of plutonium to the hexavalent state by the addition of cerium(IV) o
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