Extraction of plutonium-containing microcrystals from Hanford soil using a focused ion beam for single-crystal X-ray diffraction analysis

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

doi:10.1107/S1600576719012299

Extraction of plutonium-containing microcrystals from Hanford soil using a focused ion beam for single-crystal X-ray diffraction analysis

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

Research output: Contribution to journal › Article › peer-review

6 Scopus citations

Abstract

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 μm³ 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 PuO2. As a systematic proof of concept, the technique was first tested using UO2 crystals milled into cubic shapes with approximate volumes of 4620, 1331, 125, 8 and 1 μm³, 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.

Original language	English
Pages (from-to)	1244-1252
Number of pages	9
Journal	Journal of Applied Crystallography
Volume	52
DOIs	https://doi.org/10.1107/S1600576719012299
State	Published - Dec 1 2019
Externally published	Yes

Funding

This research was conducted under the Laboratory Research and Development Program at the US Department of Energy (DOE)’s Pacific Northwest National Laboratory (PNNL), which is operated for the DOE by Battelle Memorial Institute under contract DE-AC05-76RL1830.

Funders	Funder number
US Department of Energy
U.S. Department of Energy
Battelle	DE-AC05-76RL1830
Research and Development
Pacific Northwest National Laboratory	PNNL

Keywords

FIB/SEM
Hanford
SCXRD
focused ion beam/scanning electron microscope
microcrystals
plutonium
single-crystal X-ray diffraction

Access to Document

10.1107/S1600576719012299

Cite this

@article{246761acbaf44a85b7714b0b6de97d18,

title = "Extraction of plutonium-containing microcrystals from Hanford soil using a focused ion beam for single-crystal X-ray diffraction analysis",

abstract = "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 μm3 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 PuO2. As a systematic proof of concept, the technique was first tested using UO2 crystals milled into cubic shapes with approximate volumes of 4620, 1331, 125, 8 and 1 μm3, 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.",

keywords = "FIB/SEM, Hanford, SCXRD, focused ion beam/scanning electron microscope, microcrystals, plutonium, single-crystal X-ray diffraction",

author = "Corbey, {Jordan F.} and Reilly, {Dallas D.} and Sweet, {Lucas E.} and Lach, {Timothy G.}",

note = "Publisher Copyright: {\textcopyright} 2019 International Union of Crystallography.",

year = "2019",

month = dec,

day = "1",

doi = "10.1107/S1600576719012299",

language = "English",

volume = "52",

pages = "1244--1252",

journal = "Journal of Applied Crystallography",

issn = "0021-8898",

publisher = "International Union of Crystallography",

}

TY - JOUR

T1 - Extraction of plutonium-containing microcrystals from Hanford soil using a focused ion beam for single-crystal X-ray diffraction analysis

AU - Corbey, Jordan F.

AU - Reilly, Dallas D.

AU - Sweet, Lucas E.

AU - Lach, Timothy G.

PY - 2019/12/1

Y1 - 2019/12/1

N2 - 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 μm3 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 PuO2. As a systematic proof of concept, the technique was first tested using UO2 crystals milled into cubic shapes with approximate volumes of 4620, 1331, 125, 8 and 1 μm3, 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.

AB - 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 μm3 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 PuO2. As a systematic proof of concept, the technique was first tested using UO2 crystals milled into cubic shapes with approximate volumes of 4620, 1331, 125, 8 and 1 μm3, 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.

KW - FIB/SEM

KW - Hanford

KW - SCXRD

KW - focused ion beam/scanning electron microscope

KW - microcrystals

KW - plutonium

KW - single-crystal X-ray diffraction

UR - http://www.scopus.com/inward/record.url?scp=85075776326&partnerID=8YFLogxK

U2 - 10.1107/S1600576719012299

DO - 10.1107/S1600576719012299

M3 - Article

AN - SCOPUS:85075776326

SN - 0021-8898

VL - 52

SP - 1244

EP - 1252

JO - Journal of Applied Crystallography

JF - Journal of Applied Crystallography

ER -

Extraction of plutonium-containing microcrystals from Hanford soil using a focused ion beam for single-crystal X-ray diffraction analysis

Abstract

Funding

Keywords

Access to Document

Other files and links

Fingerprint

Cite this