Recommended Values of ²³⁹Pu, ²⁴⁰Pu and ^239+240Pu Concentrations in Reference Material IAEA‐315 (Marine Sediment) Estimated by Thermal Ionisation Mass Spectrometry, Inductively Coupled Plasma‐Mass Spectrometry and Alpha Spectrometry

Abstract

The recommended concentrations of 239Pu, 240Pu and 239+240Pu in reference material IAEA‐315 (marine sediment) were estimated by three analytical methods: isotope dilution thermal ionisation mass spectrometry (TIMS), isotope dilution inductively coupled plasma‐mass spectrometry (ICP‐MS) and alpha spectrometry. The determination of 239Pu and 240Pu (239+240Pu by alpha spectrometry) was carried out with samples from randomly selected bottles using each method. Plutonium‐238 was also measured by alpha spectrometry. A plutonium‐242 reference material was used as a spike for the quantitative analysis. The influence of 242Pu in the samples was therefore calculated; however, this contribution was less than the range of uncertainty and did not influence the final results. The obtained data were statistically analysed using variance component analysis and paired comparison. The combined standard uncertainties from “method/measurement”, “bottle” and “sub‐sample” were in the order of 3 to 6%. The main contributions to the uncertainty were from the material heterogeneity and from systematic differences between methods. Based on this study with twenty‐seven analyses using 10–14 g sample mass, concentrations of (38 ± 3) Bq kg−1, (28 ± 3) Bq kg−1 and (66 ± 4) Bq kg−1 are proposed as recommended values for 239Pu, 240Pu and 239+240Pu, respectively, and (9.5 ± 0.4) Bq kg−1 for 238Pu as an information value in reference material IAEA‐315. In mass concentration units, these amount to (16.4 ± 1.2) ng kg−1, (3.3 ± 0.4) ng kg−1 and (0.015 ± 0.003) ng kg−1 for 239Pu, 240Pu and 238Pu, respectively. The certified reference materials NIST 4350B and NIST 4354 were also analysed by TIMS for quality assurance of the method used in this study.

Airborne Plutonium and Non-Natural Uranium from the Fukushima DNPP Found at 120 km Distance a Few Days after Reactor Hydrogen Explosions

“…Plutonium and U were then separated from the matrix using commercially available ion exchange and ion chromatographic resins. The analytical procedures are described in detail elsewhere. , After chemical separation of U and Pu, each nuclide in the fraction was coprecipitated with Fe(OH) 3 using ammonium hydroxide. The precipitate was washed with high purity water and prepared as Pu and U oxides by heating at to 550 °C for 10 h. The Pu and U oxide was then mixed with about 3 mg of Fe powder and pressed into an aluminum sample holder.…”

Production and Characterization of Plutonium Dioxide Particles as a Quality Control Material for Safeguards Purposes

“…The Am fraction was eluted with 0.1 M HCl from the TRU resin. The chemical procedure for Pu is described in detail elsewhere. ,− The sample sources for the α-spectrometry were prepared as NdF 3 (PuF 4 ) using the microcoprecipitation method …”

GGR Biennial Review: Reference Materials in Geoanalytical and Environmental Research – Review for 2008 and 2009

“…Plutonium isotopes: Despite the fact that the isotope ratios of Pu are important for the origin of Pu in the environment, certified values for 239 Pu and 240 Pu of natural samples are still rare. NIST SRM 4350B, SRM 4353, SRM 4354 and SRM 4357 as well as IAEA-385 and IAEA-384 were used as QCMs (Cizdziel et al 2008, Greis et al 2008, Shinonaga et al 2008. Shinonaga et al (2008) recommend Pu isotope data for the marine sediment RM IAEA-315 derived from TIMS, ICP-MS, and alpha spectrometry.…”

“…2008). Shinonaga et al. (2008) recommend Pu isotope data for the marine sediment RM IAEA‐315 derived from TIMS, ICP‐MS, and alpha spectrometry.…”