Extraction of Plutonium-Containing Microcrystals from Hanford Soil using a Focused Ion Beam for Single-Crystal X-ray Diffraction Analysis

Corbey, Jordan F.; Reilly, Dallas D.; Sweet, Lucas E.; Lach, Timothy G.

doi:10.1107/S1600576719012299

Title: Extraction of Plutonium-Containing Microcrystals from Hanford Soil using a Focused Ion Beam for Single-Crystal X-ray Diffraction Analysis

Journal Article · Sun Dec 01 00:00:00 EST 2019 · Journal of Applied Crystallography

DOI:https://doi.org/10.1107/S1600576719012299· OSTI ID:1577981

^[1]; Reilly, Dallas D. ^[1]; Sweet, Lucas E. ^[1];

^[1]

BATTELLE (PACIFIC NW LAB)

Herein we report the successful use of a focused ion beam/scanning electron microscope (FIB/SEM) to prepare microsamples of radioactive single-crystals for X-ray diffraction analysis. This technique was used to extract and analyze crystalline Pu-containing particles as small as 28 µm3 from Hanford soil taken from the 216-Z-9 waste crib which were then crystallographically characterized using single-crystal X-ray diffraction (SCXRD) to confirm the cubic structure of PuO2. As a systematic proof of concept, the technique was first tested using UO2 crystals milled into cubic shapes with approximate volumes 4620, 1331, 125, 8 and 1 µm3, respectively, 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 (CCD) detector.

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Research Organization:: Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

Sponsoring Organization:: USDOE

DOE Contract Number:: AC05-76RL01830

OSTI ID:: 1577981

Report Number(s):: PNNL-SA-143576

Journal Information:: Journal of Applied Crystallography, Vol. 52, Issue Part 6

Country of Publication:: United States

Language:: English

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Title: Extraction of Plutonium-Containing Microcrystals from Hanford Soil using a Focused Ion Beam for Single-Crystal X-ray Diffraction Analysis

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