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

Rondahl, Stina Holmgren; Pointurier, Fabien; Ahlinder, Linnea; Ramebäck, Henrik; Marie, Olivier; Ravat, Brice; Delaunay, François; Young, Emma; Blagojevic, Ned; Hester, James R.; Thorogood, Gordon; Nelwamondo, Aubrey N.; Ntsoane, Tshepo P.; Roberts, Sarah K.; Holliday, Kiel S.

doi:10.1007/s10967-017-5666-3

Title: 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

Abstract

This work presents the results for identification of chemical phases obtained by several laboratories as a part of an international nuclear forensic round-robin exercise. In this work powder X-ray diffraction (p-XRD) is regarded as the reference technique. Neutron diffraction produced a superior high-angle diffraction pattern relative to p-XRD. Requiring only small amounts of sample, µ-Raman spectroscopy was used for the first time in this context as a potentially complementary technique to p-XRD. The chemical phases were identified as pure UO₂ in two materials, and as a mixture of UO₂, U₃O₈ and an intermediate species U₃O₇ in the third material.

Authors:

Rondahl, Stina Holmgren ^[1]; Pointurier, Fabien ^[2]; Ahlinder, Linnea ^[1]; Ramebäck, Henrik ^[3]; Marie, Olivier ^[2]; Ravat, Brice ^[4]; Delaunay, François ^[4]; Young, Emma ^[5]; Blagojevic, Ned ^[5]; Hester, James R. ^[5]; Thorogood, Gordon ^[5]; Nelwamondo, Aubrey N. ^[6]; Ntsoane, Tshepo P. ^[6]; Roberts, Sarah K. ^[7]; Holliday, Kiel S. ^[7]

Swedish Defence Research Agency (FOI), Umea (Sweden). CBRN Defence and Security
DAM, DIF, French Alternative Energies and Atomic Energy Commission (CEA), Arpajon (France)
Swedish Defence Research Agency (FOI), Umea (Sweden). CBRN Defence and Security ; Chalmers University of Technology, Goteborg (Sweden). Department of Chemistry and Chemical Engineering, Nuclear Chemistr
French Alternative Energies and Atomic Energy Commission (CEA), CEA-Centre de Valduc, Is-Sur-Tille (France)
Australian Nuclear Science and Technology Organisation (ANSTO), Lucas Heights (Australia)
South Africa Nuclear Energy Corporation (NECSA) Pelindaba, Pretoria (South Africa)
Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

Publication Date:: Wed Jan 24 00:00:00 EST 2018

Research Org.:: Lawrence Livermore National Laboratory (LLNL), Livermore, CA (United States)

Sponsoring Org.:: USDOE

OSTI Identifier:: 1424108

Report Number(s):: LLNL-JRNL-679185
Journal ID: ISSN 0236-5731; TRN: US1801905

Grant/Contract Number:: AC52-07NA27344

Resource Type:: Accepted Manuscript

Journal Name:: Journal of Radioanalytical and Nuclear Chemistry

Additional Journal Information:: Journal Volume: 315; Journal Issue: 2; Journal ID: ISSN 0236-5731

Publisher:: Springer

Country of Publication:: United States

Language:: English

Subject:: 38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEAR CHEMISTRY; 36 MATERIALS SCIENCE; XRD; µ-Raman Spectroscopy; Neutron diffraction; Phase identification; Nuclear forensics; Uranium oxide

Citation Formats


                    Rondahl, Stina Holmgren, Pointurier, Fabien, Ahlinder, Linnea, Ramebäck, Henrik, Marie, Olivier, Ravat, Brice, Delaunay, François, Young, Emma, Blagojevic, Ned, Hester, James R., Thorogood, Gordon, Nelwamondo, Aubrey N., Ntsoane, Tshepo P., Roberts, Sarah K., and Holliday, Kiel S. 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.  United States: N. p., 2018. 
Web.  doi:10.1007/s10967-017-5666-3.

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                    Rondahl, Stina Holmgren, Pointurier, Fabien, Ahlinder, Linnea, Ramebäck, Henrik, Marie, Olivier, Ravat, Brice, Delaunay, François, Young, Emma, Blagojevic, Ned, Hester, James R., Thorogood, Gordon, Nelwamondo, Aubrey N., Ntsoane, Tshepo P., Roberts, Sarah K., & Holliday, Kiel S. 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.  United States.  https://doi.org/10.1007/s10967-017-5666-3

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                    Rondahl, Stina Holmgren, Pointurier, Fabien, Ahlinder, Linnea, Ramebäck, Henrik, Marie, Olivier, Ravat, Brice, Delaunay, François, Young, Emma, Blagojevic, Ned, Hester, James R., Thorogood, Gordon, Nelwamondo, Aubrey N., Ntsoane, Tshepo P., Roberts, Sarah K., and Holliday, Kiel S. Wed .  
"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".  United States.  https://doi.org/10.1007/s10967-017-5666-3.  https://www.osti.gov/servlets/purl/1424108.

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@article{osti_1424108,

  title        = {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},

  author       = {Rondahl, Stina Holmgren and Pointurier, Fabien and Ahlinder, Linnea and Ramebäck, Henrik and Marie, Olivier and Ravat, Brice and Delaunay, François and Young, Emma and Blagojevic, Ned and Hester, James R. and Thorogood, Gordon and Nelwamondo, Aubrey N. and Ntsoane, Tshepo P. and Roberts, Sarah K. and Holliday, Kiel S.},

  abstractNote = {This work presents the results for identification of chemical phases obtained by several laboratories as a part of an international nuclear forensic round-robin exercise. In this work powder X-ray diffraction (p-XRD) is regarded as the reference technique. Neutron diffraction produced a superior high-angle diffraction pattern relative to p-XRD. Requiring only small amounts of sample, µ-Raman spectroscopy was used for the first time in this context as a potentially complementary technique to p-XRD. The chemical phases were identified as pure UO2 in two materials, and as a mixture of UO2, U3O8 and an intermediate species U3O7 in the third material.},

  doi          = {10.1007/s10967-017-5666-3},

  journal      = {Journal of Radioanalytical and Nuclear Chemistry},

  number       = 2,

  volume       = 315,

  place        = {United States},

  year         = {Wed Jan 24 00:00:00 EST 2018},

  month        = {Wed Jan 24 00:00:00 EST 2018}

}

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https://doi.org/10.1007/s10967-017-5666-3

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Title: 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

Abstract

Citation Formats

Echidna—the new high-resolution powder diffractometer being built at OPAL journal, November 2006

Raman spectra of stoichiometric and hyperstoichiometric uranium dioxide journal, September 2003

In situ Raman monitoring of materials under irradiation: study of uranium dioxide alteration by water radiolysis journal, May 2012

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Raman spectrum of U4O9: a new interpretation of damage lines in UO2: Raman spectrum of U4O9 journal, October 2011

An intelligent background-correction algorithm for highly fluorescent samples in Raman spectroscopy journal, October 2009

Identification of the chemical forms of uranium compounds in micrometer-size particles by means of micro-Raman spectrometry and scanning electron microscope journal, September 2010

The determination of electrochemical reactivity and sustainability on individual hyper-stoichiometric UO2+x grains by Raman microspectroscopy and scanning electrochemical microscopy journal, August 2009

Surface reactions of uranium oxide powder, thin films and single crystals journal, March 2010

Surface reactions of uranium oxide powder, thin films and single crystals journal, March 2010

An intelligent background-correction algorithm for highly fluorescent samples in Raman spectroscopy journal, October 2009

A phase study on the tie line of U3O7PuO2 journal, December 1971

Oxidation of UO2 fuel pellets in air at 503 and 543 K studied using X-ray photoelectron spectroscopy and X-ray diffraction journal, February 1988

Thermal expansion and phase transformations of the U3O8−z phase in air journal, January 1977

Structures of UO2, UO2+x andU4O9 by neutron diffraction journal, January 1964

Raman Microprobe Spectroscopy of Uranium Dioxide Single Crystals and Ion Implanted Polycrystals journal, December 1990

Raman Microprobe Spectroscopy of Uranium Dioxide Single Crystals and Ion Implanted Polycrystals journal, December 1990

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Determination of uranium metal concentration in irradiated fuel storage basin sludge using selective dissolution journal, December 2013

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Establishing reactor operations from uranium targets used for the production of plutonium journal, August 2009

Characterisation of uranium oxides by micro-Raman spectroscopy journal, January 1987

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The reaction of water on polycrystalline UO2: Pathways to surface and bulk oxidation journal, June 2005

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Crystallography Open Database – an open-access collection of crystal structures journal, May 2009

Crystallography Open Database (COD): an open-access collection of crystal structures and platform for world-wide collaboration journal, November 2011

Raman spectroscopy characterization of actinide oxides (U1−yPuy)O2: Resistance to oxidation by the laser beam and examination of defects journal, October 2010

The kinetics of dissolution of UO2 under reducing conditions and the influence of an oxidized surface layer (UO2+x): Application of a continuous flow-through reactor journal, March 1991

Applicability of Raman spectroscopy as a tool in nuclear forensics for analysis of uranium ore concentrates journal, January 2013

Echidna—the new high-resolution powder diffractometer being built at OPAL
journal, November 2006

Raman spectra of stoichiometric and hyperstoichiometric uranium dioxide
journal, September 2003

In situ Raman monitoring of materials under irradiation: study of uranium dioxide alteration by water radiolysis
journal, May 2012

A phase study on the tie line of U3O7PuO2
journal, December 1971

Raman spectrum of U4O9: a new interpretation of damage lines in UO2: Raman spectrum of U4O9
journal, October 2011

An intelligent background-correction algorithm for highly fluorescent samples in Raman spectroscopy
journal, October 2009

Identification of the chemical forms of uranium compounds in micrometer-size particles by means of micro-Raman spectrometry and scanning electron microscope
journal, September 2010

The determination of electrochemical reactivity and sustainability on individual hyper-stoichiometric UO2+x grains by Raman microspectroscopy and scanning electrochemical microscopy
journal, August 2009

Surface reactions of uranium oxide powder, thin films and single crystals
journal, March 2010

Surface reactions of uranium oxide powder, thin films and single crystals
journal, March 2010

An intelligent background-correction algorithm for highly fluorescent samples in Raman spectroscopy
journal, October 2009

A phase study on the tie line of U3O7PuO2
journal, December 1971

Oxidation of UO2 fuel pellets in air at 503 and 543 K studied using X-ray photoelectron spectroscopy and X-ray diffraction
journal, February 1988

Thermal expansion and phase transformations of the U3O8−z phase in air
journal, January 1977

Structures of UO2, UO2+x andU4O9 by neutron diffraction
journal, January 1964

Raman Microprobe Spectroscopy of Uranium Dioxide Single Crystals and Ion Implanted Polycrystals
journal, December 1990

Raman Microprobe Spectroscopy of Uranium Dioxide Single Crystals and Ion Implanted Polycrystals
journal, December 1990

Characterisation of uranium oxides by micro-Raman spectroscopy
journal, January 1987

Raman spectroscopy characterization of actinide oxides (U1−yPuy)O2: Resistance to oxidation by the laser beam and examination of defects
journal, October 2010

Characterization of Uranium Oxides Using in Situ Micro-Raman Spectroscopy
journal, September 2000

Determination of uranium metal concentration in irradiated fuel storage basin sludge using selective dissolution
journal, December 2013

The kinetics of dissolution of UO2 under reducing conditions and the influence of an oxidized surface layer (UO2+x): Application of a continuous flow-through reactor
journal, March 1991

Uranium Speciation As a Function of Depth in Contaminated Hanford Sediments - A Micro-XRF, Micro-XRD, and Micro- And Bulk-XAFS Study
journal, February 2009

Plutonium–uranium mixed oxide characterization by coupling micro-X-ray diffraction and absorption investigations
journal, September 2011

Identification of the chemical forms of uranium compounds in micrometer-size particles by means of micro-Raman spectrometry and scanning electron microscope
journal, September 2010

Oxidation states of uranium in depleted uranium particles from Kuwait
journal, January 2005

Investigation of the polymorphs and hydrolysis of uranium trioxide
journal, August 2012

The determination of electrochemical reactivity and sustainability on individual hyper-stoichiometric UO2+x grains by Raman microspectroscopy and scanning electrochemical microscopy
journal, August 2009

Recognition of uranium oxides in soil particulate matter by means of μ-Raman spectrometry
journal, November 2008

Uranium Speciation As a Function of Depth in Contaminated Hanford Sediments - A Micro-XRF, Micro-XRD, and Micro- And Bulk-XAFS Study
journal, February 2009

Crystallography Open Database (COD): an open-access collection of crystal structures and platform for world-wide collaboration
journal, November 2011

The reaction of water on polycrystalline UO2: Pathways to surface and bulk oxidation
journal, June 2005

Investigation of ammonium diuranate calcination with high-temperature X-ray diffraction
journal, September 2014

Determination of uranium metal concentration in irradiated fuel storage basin sludge using selective dissolution
journal, December 2013

Establishing reactor operations from uranium targets used for the production of plutonium
journal, August 2009

Structures of UO2, UO2+x andU4O9 by neutron diffraction
journal, January 1964

Establishing reactor operations from uranium targets used for the production of plutonium
journal, August 2009

Characterisation of uranium oxides by micro-Raman spectroscopy
journal, January 1987

Certification of Standard Reference Material 1976B
journal, August 2015

The reaction of water on polycrystalline UO2: Pathways to surface and bulk oxidation
journal, June 2005

Investigation of the polymorphs and hydrolysis of uranium trioxide
journal, August 2012

Oxidation states of uranium in depleted uranium particles from Kuwait
journal, January 2005

Crystallography Open Database – an open-access collection of crystal structures
journal, May 2009

Crystallography Open Database (COD): an open-access collection of crystal structures and platform for world-wide collaboration
journal, November 2011

Raman spectroscopy characterization of actinide oxides (U1−yPuy)O2: Resistance to oxidation by the laser beam and examination of defects
journal, October 2010

The kinetics of dissolution of UO2 under reducing conditions and the influence of an oxidized surface layer (UO2+x): Application of a continuous flow-through reactor
journal, March 1991

Applicability of Raman spectroscopy as a tool in nuclear forensics for analysis of uranium ore concentrates
journal, January 2013