Safety evaluation of a radioactive waste repository requires credible activity estimates confirmed by actual measurements. A long-lived radionuclide, Pd, which can be found in radioactive wastes, is one of the difficult-to-measure nuclides and results in a deficit in experimentally determined contents. In this study, a precipitation-based separation method has been developed for the determination of Pd with inductively coupled plasma mass spectrometry. The photoreduction induced by pulsed laser irradiation at 355 nm provides short-time and one-step recovery of Pd. The proposed method was verified by applying it to a spent nuclear fuel sample. To recover Pd efficiently, a natural Pd standard was employed as the Pd carrier. Taking advantage of the absence of Pd in spent nuclear fuel, Pd in the Pd carrier was utilized as the internal standard. The chemical yield of Pd was about 90% with virtually no impurities, allowing accurate quantification of Pd. The amount of Pd in the Pd precipitate was 17.3 ± 0.7 ng, equivalent to 239 ± 9 ng per mg of U in the sample.

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http://dx.doi.org/10.1021/acs.analchem.6b03286DOI Listing

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