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Title: Spatially Resolved Raman Spectroscopic Investigation of Uranyl Fluoride: A Case Study in the Importance of Instrument Optimization

Journal Article · · Applied Spectroscopy
ORCiD logo [1]; ORCiD logo [1]; ORCiD logo [1];  [1]; ORCiD logo [1]
  1. Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)
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Raman spectroscopy is an emerging technique for rapid and nondestructive analysis of nuclear materials for forensic and nonproliferation applications as it is a powerful tool for distinguishing multiple chemical forms of materials with similar stoichiometries. Recent developments in spectroscopic software have enabled rapid data collection with high-speed Raman spectroscopic mapping capabilities. However, some uranium-rich materials are susceptible to degradation in humid air and/or laser-induced phase transformations. To mitigate environmental or measurement-related sample degradation of potential samples of interest, we have taken a systematic approach to define optimized data collection parameters for high-throughput measurements of uranyl fluoride (UO2F2), which is an important intermediate material in the nuclear fuel cycle. First, we systematically describe the influence of optical magnification (5× to 100×), laser power, and exposure time on obtained signal for identical particles of UO2F2 and find that at low laser power and exposure times, comparable signal is obtained regardless of optical magnification. Second, we ensure sample integrity during data collection, and third, collect spectroscopic maps that employ optimized parameters to reduce the time required to obtain spatially resolved spectroscopic information. Reductions of 90% and 99% in measurement times are discussed as they relate to differences in resolving spectroscopic features of particles in identical mapping areas. Finally, during this work, we found that additional data processing options were needed and thus developed a customized Python script for importing, processing, analyzing, and visualizing Raman spectroscopic map data.

Research Organization:
Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)
Sponsoring Organization:
USDOE Laboratory Directed Research and Development (LDRD) Program
Grant/Contract Number:
AC05-00OR22725
OSTI ID:
2438955
Journal Information:
Applied Spectroscopy, Journal Name: Applied Spectroscopy Journal Issue: 8 Vol. 78; ISSN 0003-7028
Publisher:
Society for Applied SpectroscopyCopyright Statement
Country of Publication:
United States
Language:
English

References (19)

The Chemistry of the Actinide and Transactinide Elements book January 2006
An optimized methodology for the determination of the uranium chemical phases in micro-particles by Raman spectrometry within a scanning electron microscope journal December 2022
On the determination of uraniumoxygen bond lengths in dioxouranium(VI) compounds by Raman spectroscopy journal February 1989
Detection and identification of solids, surfaces, and solutions of uranium using vibrational spectroscopy journal November 2018
Exercise Celestial Skónis: Part 2 – Emerging technologies and State of Practice of nuclear forensic analyses demonstrated during the 6th collaborative materials exercise of the nuclear forensics International Technical Working Group journal July 2022
Exercise Celestial Skónis: Part 1 – History, purpose, design and results of traditional forensic examinations of the 6th Collaborative materials exercise of the nuclear forensics International Technical Working Group journal July 2022
Raman spectroscopy of uranium compounds and the use of multivariate analysis for visualization and classification journal June 2015
Characterizing the degradation of [(UO2F2)(H2O)]7 4H2O under humid conditions journal February 2020
Characterization of Uranium Particles Produced by Hydrolysis of UF 6 Using SEM and SIMS journal May 2007
Progress in Uranium Chemistry: Driving Advances in Front-End Nuclear Fuel Cycle Forensics journal February 2021
Ozone-Facilitated Formation of Uranyl Peroxide in Humid Conditions journal December 2022
Evidence of a Nonphotochemical Mechanism for the Solid-State Formation of Uranyl Peroxide journal May 2018
Structural Phase Transitions and Water Dynamics in Uranyl Fluoride Hydrates journal November 2015
Identification and Elemental Impurity Analysis of Heterogeneous Morphologies in Uranium Oxides Synthesized from Uranyl Fluoride Precursors journal May 2023
Formation of a uranyl hydroxide hydrate via hydration of [(UO 2 F 2 )(H 2 O)] 7 ·4H 2 O journal January 2019
Experimental and computational study of particle formation kinetics in UF 6 hydrolysis journal January 2020
Vibrational properties of anhydrous and partially hydrated uranyl fluoride journal January 2017
Micro-Raman Spectroscopy of Selected Solid U x O y F z Compounds journal March 1989
Applicability of Raman spectroscopy as a tool in nuclear forensics for analysis of uranium ore concentrates journal January 2013

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46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND TECHNOLOGY
Raman spectroscopic mapping
UO2F2
high-speed mapping
nuclear materials analysis
uranyl fluoride