Trace Element Analyses of Micron-Size Particles and Statistical Determination of Minimum Detection Limits

Savannah River National Laboratory (SRNL) has developed expertise in producing homogeneous, ca. 1 m-diameter spherical particles of mixed-element components, wherein dopants can be varied from a trace constituent (ppm) to wt.% concentrations. The samples used for this work are nickel-doped cerium oxide microspheres produced by SRNL. They were initially selected as analogs for plutonium-doped uranium oxide particles and analyzed as part of a larger study to evaluate whether electron probe microanalyzers (EPMA) can be used to characterize nuclear materials as an alternative or complementary method to mass spectrometers. The five samples used in this study contained nominal compositions of 0, 0.004, 0.04, 0.4 and 4 wt.% Ni. They were analyzed by both an Agilent 7900 Q-ICP-MS at SRNL and the JEOL JXA8530F Plus EPMA at the University of Minnesota. In addition to EPMA results (calibrated with high-precision Q-ICP-MS analyses) suggesting that the EPMA could address outstanding nuclear material characterization needs, these samples 1) showcase the ability of the EPMA to quantify not just trace concentrations, but trace concentrations in microparticles (1 m diameter, Fig. 1), and 2) offer a unique opportunity to evaluate the methodology for assessing the minimum detection limits of EPMA analyses.. Authors: McSwiggen, Peter [JEOL USA, 11 Dearborn Road, Peabody, MA 01960, USA]; Riche, Alexis T. [Savannah River National Laboratory (SRNL), Aiken, SC (United States)]; Harvey, Kayleigh [JEOL USA, 11 Dearborn Road, Peabody, MA 01960, USA]; Bowden, Shelby [Savannah River National Laboratory (SRNL), Aiken, SC (United States)]; Bergin, Rachel A. [Savannah River National Laboratory (SRNL), Aiken, SC (United States)]. DOE Contract: 89303321CEM000080