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Anal Chem. 2017 Mar 7;89(5):3177-3183. doi: 10.1021/acs.analchem.6b05020. Epub 2017 Feb 10.

Quantifying Morphological Features of α-U3O8 with Image Analysis for Nuclear Forensics.

Author information

1
University of Utah Department of Civil and Environmental Engineering, Nuclear Engineering Program, 201 Presidents Circle, Salt Lake City, Utah 84112, United States.
2
University of Utah Energy & Geoscience Institute (EGI) , 423 Wakara Way #300, Salt Lake City, Utah 84108, United States.
3
Scientific Computing and Imaging (SCI) Institute , 72 South Central Campus Drive, Room 3750 Salt Lake City, Utah 84112, United States.
4
Los Alamos National Laboratory , Materials Chemistry, J514, Los Alamos, New Mexico 87545, United States.

Abstract

Morphological changes in U3O8 based on calcination temperature have been quantified enabling a morphological feature to serve as a signature of processing history in nuclear forensics. Five separate calcination temperatures were used to synthesize α-U3O8, and each sample was characterized using powder X-ray diffraction (p-XRD) and scanning electron microscopy (SEM). The p-XRD spectra were used to evaluate the purity of the synthesized U-oxide; the morphological analysis for materials (MAMA) software was utilized to quantitatively characterize the particle shape and size as indicated by the SEM images. Analysis comparing the particle attributes, such as particle area at each of the temperatures, was completed using the Kolmogorov-Smirnov two sample test (K-S test). These results illustrate a distinct statistical difference between each calcination temperature. To provide a framework for forensic analysis of an unknown sample, the sample distributions at each temperature were compared to randomly selected distributions (100, 250, 500, and 750 particles) from each synthesized temperature to determine if they were statistically different. It was found that 750 particles were required to differentiate between all of the synthesized temperatures with a confidence interval of 99.0%. Results from this study provide the first quantitative morphological study of U-oxides, and reveals the potential strength of morphological particle analysis in nuclear forensics by providing a framework for a more rapid characterization of interdicted uranium oxide samples.

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