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At least 343 records · Page 19
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

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.

McSwiggen, Peter [JEOL USA, 11 Dearborn Road, Peab↗
NASA NTRS1976

Determination of particle size using measurement of scatter

Scatter from glass beads placed on a mirror was measured using a quartz lamp and laser. Data were obtained in the plane containing the normal to the surface and the incident beam. For the quartz lamp the best correlation can be obtained for data measured at a zenith of 55 deg and 180 deg from the incident beam. The best correlation when the laser is used is obtained at about the same position. However, the correlation variables are angular spacing of the minimums of the data versus the size. Whereas, with the quartz lamp the correlation variables are the amount of scattered energy versus size.

Scott, R. L., Jr.↗
NASA NTRS1977

Determination of particle size using measurement of scatter

Scatter measurements were taken from glass spheres of size 5 to 50 microns placed on a mirror to see whether such scatter data could be correlated with size. The spheres were illuminated with a laser whose wavelength was 0.62 microns. A Gonioreflectometer was used to vary the detector between the normal to the mirror and 85 deg from the normal and in the plane containing the normal to the mirror and the incident laser light. The azimuth of the detector with respect to the source was 180 deg. The light detector was driven by a step motor. The scatter was dark and bright lines. They appeared as minima and maxima on the output recorder. As the size of the beads increased the number of maxima increased.

Scott, R. L., Jr.↗