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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

Abstract

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.

Authors:
ORCiD logo [1];  [1];  [1]; ORCiD logo [1]
  1. BATTELLE (PACIFIC NW LAB)
Publication Date:
Research Org.:
Pacific Northwest National Lab. (PNNL), Richland, WA (United States)
Sponsoring Org.:
USDOE
OSTI Identifier:
1577981
Report Number(s):
PNNL-SA-143576
DOE Contract Number:  
AC05-76RL01830
Resource Type:
Journal Article
Journal Name:
Journal of Applied Crystallography
Additional Journal Information:
Journal Volume: 52; Journal Issue: Part 6
Country of Publication:
United States
Language:
English
Subject:
microcrystals, Plutomium, focused ion beam/scanning electron microscope, FIB/SEM, Hanford, SCXRD, single-crystal x-ray diffraction

Citation Formats

Corbey, Jordan F., Reilly, Dallas D., Sweet, Lucas E., and Lach, Timothy G. Extraction of Plutonium-Containing Microcrystals from Hanford Soil using a Focused Ion Beam for Single-Crystal X-ray Diffraction Analysis. United States: N. p., 2019. Web. doi:10.1107/S1600576719012299.
Corbey, Jordan F., Reilly, Dallas D., Sweet, Lucas E., & Lach, Timothy G. Extraction of Plutonium-Containing Microcrystals from Hanford Soil using a Focused Ion Beam for Single-Crystal X-ray Diffraction Analysis. United States. doi:10.1107/S1600576719012299.
Corbey, Jordan F., Reilly, Dallas D., Sweet, Lucas E., and Lach, Timothy G. Sun . "Extraction of Plutonium-Containing Microcrystals from Hanford Soil using a Focused Ion Beam for Single-Crystal X-ray Diffraction Analysis". United States. doi:10.1107/S1600576719012299.
@article{osti_1577981,
title = {Extraction of Plutonium-Containing Microcrystals from Hanford Soil using a Focused Ion Beam for Single-Crystal X-ray Diffraction Analysis},
author = {Corbey, Jordan F. and Reilly, Dallas D. and Sweet, Lucas E. and Lach, Timothy G.},
abstractNote = {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.},
doi = {10.1107/S1600576719012299},
journal = {Journal of Applied Crystallography},
number = Part 6,
volume = 52,
place = {United States},
year = {2019},
month = {12}
}

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