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Verifying the presence of low levels of neptunium in a uranium matrix with electron energy-loss spectroscopy
Authors:Edgar C Buck  Matt Douglas  Rick S Wittman
Institution:1. Materials Science & Engineering Department, Idaho National Laboratory, Idaho Falls, ID 83415-2211, USA;2. Fuel Performance and Design Department, Idaho National Laboratory, Idaho Falls, ID 83415-6188, USA;3. Micron School of Materials Science and Engineering, Boise State University, Boise, ID 83725-2090, USA;4. Center for Advanced Energy Studies, Idaho Falls, ID 83401, USA;1. Department of Physics, Pondicherry University, R. V Nagar, Kalapet, Pondicherry 605014, India;2. Condensed Matter Physics Division, Saha Institute of Nuclear Physics, 1/AF Bidhannagar, Kolkata 700064, India;3. Indus Synchrotrons Utilization Division, Raja Ramanna Centre for Advanced Technology, Indore 452013, India;1. Electron Microscopy for Materials Science (EMAT), University of Antwerp, Groenenborgerlaan 171, 2020 Antwerp, Belgium;2. Department of Materials, University of Oxford, Parks Road, OX1 3PH Oxford, UK;1. European Commission, Joint Research Centre, Institute for Transuranium Elements, P.O. Box 2340, 76125 Karlsruhe, Germany;2. Institut für Nukleare Entsorgung, Hermann-von-Helmholtz-Platz, 76344 Eggenstein-Leopoldshafen, Germany
Abstract:This paper examines the problems associated with analysis of low levels of neptunium in a uranium matrix with electron energy-loss spectroscopy (EELS) on the transmission electron microscope (TEM). The detection of neptunium in a matrix of uranium can be impeded by the occurrence of a plural scattering event from uranium (U-M5 + U-O4,5) that results in severe overlap on the Np-M5 edge at 3665 eV. Low levels of Np (1600–6300 ppm) can be detected in a uranium solid, uranophane Ca(UO2)2(SiO3OH)2(H2O)5], by confirming that the energy gap between the Np-M5 and Np-M4 edges is at 184 eV and showing that the M4/M5 ratio for the neptunium is smaller than that for uranium. The Richardson–Lucy deconvolution method was applied to energy-loss spectral images and was shown to increase the signal to noise ratio.
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