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Extraction of plutonium‐containing microcrystals from Hanford soil using a focused ion beam for single‐crystal X‐ray diffraction analysis
Author(s) -
Corbey Jordan F.,
Reilly Dallas D.,
Sweet Lucas E.,
Lach Timothy G.
Publication year - 2019
Publication title -
journal of applied crystallography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.429
H-Index - 162
ISSN - 1600-5767
DOI - 10.1107/s1600576719012299
Subject(s) - materials science , diffractometer , diffraction , single crystal , powder diffraction , ion beam , crystal (programming language) , x ray crystallography , x ray , characterization (materials science) , ion beam analysis , crystal structure , ion , analytical chemistry (journal) , crystallography , scanning electron microscope , chemistry , optics , nanotechnology , physics , chromatography , programming language , organic chemistry , computer science , composite material
Herein, the successful use of a focused ion beam/scanning electron microscope to prepare microsamples of radioactive single crystals for X‐ray diffraction analysis is reported. This technique was used to extract and analyze crystalline Pu‐containing particles as small as 28 µm 3 from Hanford soil taken from the 216‐Z‐9 waste crib, which were then crystallographically characterized using single‐crystal X‐ray diffraction to confirm the cubic structure of PuO 2 . As a systematic proof of concept, the technique was first tested using UO 2 crystals milled into cubic shapes with approximate volumes of 4620, 1331, 125, 8 and 1 µm 3 , in order to empirically determine the crystal size limits for characterization by a laboratory‐based diffractometer with a sealed tube Mo or Ag anode X‐ray source and a charge‐coupled device detector.