<p>Capabilities to extract and analyse nanogram-scale uranium dioxide (UO<sub>2</sub>) samples to allow spatial isotopic analysis were established by the development of techniques from wider literature. A Helios 5CX Focussed Ion Beam Scanning Electron Microscope (FIB-SEM) adapted for alpha-emitting radioactive material was used to extract samples of 2–80&#xa0;ng from a depleted UO<sub>2</sub> pellet. These were analysed by Thermal Ionisation Mass Spectrometry (TIMS) and Triple Quadrupole Inductively Coupled Mass Spectrometry (ICP-QQQ-MS). TIMS produced measurements for <sup>234</sup>U, <sup>235</sup>U, <sup>236</sup>U, and <sup>238</sup>U weight-percent (wt%) with relative standard uncertainties (RSU) of between 0.26 and 11%. ICP-QQQ-MS measured the <sup>235</sup>U/<sup>238</sup>U ratio with an RSU of 37.4%.</p>

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Sample preparation for actinide isotopic analysis using FIB-SEM

  • A. D. Wood,
  • S. A. Dunn,
  • P. Kaye,
  • M. Higginson,
  • J. Robb,
  • R. W. Harrison

摘要

Capabilities to extract and analyse nanogram-scale uranium dioxide (UO2) samples to allow spatial isotopic analysis were established by the development of techniques from wider literature. A Helios 5CX Focussed Ion Beam Scanning Electron Microscope (FIB-SEM) adapted for alpha-emitting radioactive material was used to extract samples of 2–80 ng from a depleted UO2 pellet. These were analysed by Thermal Ionisation Mass Spectrometry (TIMS) and Triple Quadrupole Inductively Coupled Mass Spectrometry (ICP-QQQ-MS). TIMS produced measurements for 234U, 235U, 236U, and 238U weight-percent (wt%) with relative standard uncertainties (RSU) of between 0.26 and 11%. ICP-QQQ-MS measured the 235U/238U ratio with an RSU of 37.4%.