Skip to main content
U.S. Department of Energy
Office of Scientific and Technical Information

Mixed Element Microparticle Characterization by Electron Probe Microanalysis

Journal Article · · Microscopy and Microanalysis
DOI:https://doi.org/10.1093/mam/ozaf022· OSTI ID:2544421
Abstract

Microparticle compositional characterization for nuclear forensics has traditionally been achieved by “gold-standard” destructive analytical techniques such as large geometry-secondary ion mass spectrometry and fission track-thermal ionization mass spectrometry, but long processing times and total sample consumption eliminate the option of subsequent analysis by other methods. Electron probe microanalysis has long been widely employed for rapid, nondestructive, micrometer-scale compositional measurements and imaging in fields such as material science and geology and may therefore need to be reevaluated as an alternative tool for microparticle analysis for the nuclear forensics community. This study presents the use of electron probe microanalysis for imaging and quantitative characterization of homogeneous microparticles utilizing a calibration curve based on high-precision quadrupole-inductively coupled plasma-mass spectrometry analyses. Samples of opportunity synthesized at Savannah River National Laboratory, nickel-doped cerium oxide microparticles, were selected as analogs for plutonium-doped uranium oxide microparticles. Positive detection and accurate quantification of variable amounts of nickel dopant down to trace levels (10s of parts per million) suggest applicability of this technique to other mixed element systems (e.g., actinides). Quantitative single-particle characterization via electron probe microanalyzer may thus provide a high fidelity, nondestructive complement to techniques currently in use.

Sponsoring Organization:
USDOE Office of Environmental Management (EM)
Grant/Contract Number:
89303321CEM000080
OSTI ID:
2544421
Journal Information:
Microscopy and Microanalysis, Journal Name: Microscopy and Microanalysis Journal Issue: 2 Vol. 31; ISSN 1431-9276
Publisher:
Oxford University PressCopyright Statement
Country of Publication:
United States
Language:
English

References (28)

Inter-laboratory comparison of a WDS-EDS quantitative X-ray microanalysis of a metallic glass journal December 2014
Quantitative Elemental Analysis of Individual Microparticles with Electron Beam Instruments book January 1991
SIMS Analysis of Uranium and Actinides in Microparticles of Different Origin journal April 2004
Comparing results of X-ray diffraction, µ-Raman spectroscopy and neutron diffraction when identifying chemical phases in seized nuclear material, during a comparative nuclear forensics exercise journal January 2018
Strengthening IAEA safeguards through environmental sampling and analysis journal June 1998
Characterization of uranium and plutonium containing particles originating from the nuclear weapons accident in Thule, Greenland, 1968 journal January 2005
Accurate determination of minor isotope ratios in individual plutonium–uranium mixed particles by thermal ionization mass spectrometry journal February 2018
Electron probe microanalysis: A review of recent developments and applications in materials science and engineering journal February 2021
Isotope ratio analysis of individual sub-micrometer plutonium particles with inductively coupled plasma mass spectrometry journal December 2010
240Pu/239Pu isotopic ratio measurements in micrometric Pu and MOX particles using Secondary Ion Mass Spectrometry journal January 2023
Correlative morphological, elemental and chemical phase analyses at the micrometric scale of powdered materials: Application to nuclear forensics journal September 2024
Electron Microprobe Analysis and Scanning Electron Microscopy in Geology book January 2009
The Use of SIMS and SEM for the Characterization of Individual Particles with a Matrix Originating from a Nuclear Weapon journal May 2007
Factors Affecting WDS Performance Superiority over EDS journal August 2015
The Promises when WDS Supports the EDS X-ray Analysis in SEM and the Evaluation Algorithms do Merge journal August 2022
Production and Characterization of Plutonium Dioxide Particles as a Quality Control Material for Safeguards Purposes journal February 2012
Quantitative chemical analysis of individual microparticles using the electron microprobe. Theoretical journal November 1975
Production and Characterization of Monodisperse Plutonium, Uranium, and Mixed Uranium−Plutonium Particles for Nuclear Safeguard Applications journal May 2010
The nature of Pu-bearing particles from the Maralinga nuclear testing site, Australia journal May 2021
Production of mixed element actinide reference particulates to support nuclear safeguards using THESEUS, an aerosol-based particulate synthetic methodology journal January 2023
Trace element analysis by EPMA in geosciences: detection limit, precision and accuracy journal January 2018
Exploring the limits of EDS microanalysis: rare earth element analyses journal January 2018
Detecting Pu in U-bearing Particles by SEM/EDS for Nuclear Safeguards Applications journal July 2023
Unified equations for the slope, intercept, and standard errors of the best straight line journal March 2004
Nuclear Forensic Science: Analysis of Nuclear Material Out of Regulatory Control journal June 2016
Evaluation of measurement data—Guide to the expression of uncertainty in measurement preprint January 2008
Evaluation of measurement data—Supplement 1 to the “Guide to the expression of uncertainty in measurement”—Propagation of distributions using a Monte Carlo method journal January 2008
International Vocabulary of Metrology – Basic and general concepts and associated terms (VIM) 3rd edition journal January 2008

Similar Records

Trace Element Analyses of Micron-Size Particles and Statistical Determination of Minimum Detection Limits
Conference · Wed Feb 12 23:00:00 EST 2025 · OSTI ID:2586423

Compositional mapping with the electron probe microanalyzer: Part I
Journal Article · Wed Nov 14 23:00:00 EST 1990 · Analytical Chemistry (Washington); (USA) · OSTI ID:6067708

Carbon determination by the complex method of autoradiography-X-ray microanalysis
Journal Article · Tue Jan 31 23:00:00 EST 1995 · Industrial Laboratory · OSTI ID:391311

Related Subjects