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Anal Chem. 2016 Jul 19;88(14):7145-53. doi: 10.1021/acs.analchem.6b01209. Epub 2016 Jun 29.

Measurement of Uranium Isotopes in Particles of U3O8 by Secondary Ion Mass Spectrometry-Single-Stage Accelerator Mass Spectrometry (SIMS-SSAMS).

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Materials Science and Technology Division, Code 6367, U.S. Naval Research Laboratory, 4555 Overlook Avenue SW, Washington, DC 20375, United States.
National Research Council Fellow at the Naval Research Laboratory, Washington, DC 20375, United States.


A commercial secondary ion mass spectrometer (SIMS) was coupled to a ± 300 kV single-stage accelerator mass spectrometer (SSAMS). Positive secondary ions generated with the SIMS were injected into the SSAMS for analysis. This combined instrument was used to measure the uranium isotopic ratios in particles of three certified reference materials (CRM) of uranium, CRM U030a, CRM U500, and CRM U850. The ability to inject positive ions into the SSAMS is unique for AMS systems and allows for simple analysis of nearly the entire periodic table because most elements will readily produce positive ions. Isotopic ratios were measured on samples of a few picograms to nanograms of total U. Destruction of UH(+) ions in the stripper tube of the SSAMS reduced hydride levels by a factor of ∼3 × 10(4) giving the UH(+)/U(+) ratio at the SSAMS detector of ∼1.4 × 10(-8). These hydride ion levels would allow the measurement of (239)Pu at the 10 ppb level in the presence of U and the equivalent of ∼10(-10 236)U concentration in natural uranium. SIMS-SSAMS analysis of solid nuclear materials, such as these, with signals nearly free of molecular interferences, could have a significant future impact on the way some measurements are made for nuclear nonproliferation.

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