Journal
ANALYTICAL CHEMISTRY
Volume 91, Issue 15, Pages 10081-10087Publisher
AMER CHEMICAL SOC
DOI: 10.1021/acs.analchem.9b02013
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Funding
- U.S. Department of Homeland Security, Domestic Nuclear Detection Office [2016-DN-077-RI102]
- Defense Threat Reduction Agency [HDTRA1-16-10026]
- College of Engineering
- Health Sciences Center
- Office of the Vice President for Research
- Utah Science Technology and Research (USTAR) Initiative of the State of Utah
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The morphological effect of impurities on alpha-U3O8 has been investigated. This study provides the first evidence that the presence of impurities can alter nuclear material morphology, and these changes can be quantified to aid in revealing processing history. Four elements: Ca, Mg, V, and Zr were implemented in the uranyl peroxide synthesis route and studied individually within the alpha-U3O8. Six total replicates were synthesized, and replicates 1-3 were filtered and washed with Millipore water (18.2 M Omega) to remove any residual nitrates. Replicates 4-6 were filtered but not washed to determine the amount of impurities removed during washing. Inductively coupled plasma mass spectrometry (ICP-MS) was employed at key points during the synthesis to quantify incorporation of the impurity. Each sample was characterized using powder X-ray diffraction (p-XRD), high-resolution scanning electron microscopy (HRSEM), and SEM with energy dispersive X-ray spectroscopy (SEM-EDS). p-XRD was utilized to evaluate any crystallographic changes due to the impurities; HRSEM imagery was analyzed with Morphological Analysis for MAterials (MAMA) software and machine learning classification for quantification of the morphology; and SEM-EDS was utilized to locate the impurity within the alpha-U3O8. All samples were found to be quantifiably distinguishable, further demonstrating the utility of quantitative morphology as a signature for the processing history of nuclear material.
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