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Title: Structural investigations of Pu{sup III} phosphate by X-ray diffraction, MAS-NMR and XANES spectroscopy

Abstract

PuPO{sub 4} was prepared by a solid state reaction method and its crystal structure at room temperature was solved by powder X-ray diffraction combined with Rietveld refinement. High resolution XANES measurements confirm the +III valence state of plutonium, in agreement with valence bond derivation. The presence of the americium (as β{sup −} decay product of plutonium) in the +III oxidation state was determined based on XANES spectroscopy. High resolution solid state {sup 31}P NMR agrees with the XANES results and the presence of a solid-solution. - Graphical abstract: A full structural analysis of PuPO{sub 4} based on Rietveld analysis of room temperature X-ray diffraction data, XANES and MAS NMR measurements was performed. - Highlights: • The crystal structure of PuPO{sub 4} monazite is solved. • In PuPO{sub 4} plutonium is strictly trivalent. • The presence of a minute amount of Am{sup III} is highlighted. • We propose PuPO{sub 4} as a potential reference material for spectroscopic and microscopic studies.

Authors:
 [1];  [1];  [1];  [2];  [1];  [3]; ; ;  [1]
  1. European Commission, Joint Research Centre, Institute for Transuranium Elements, P.O. Box 2340, D-76125 Karlsruhe (Germany)
  2. CEA, DEN, DEC/SESC, F-13108 Saint Paul Lez Durance Cedex (France)
  3. Synchrotron SOLEIL, 91190 Saint-Aubin (France)
Publication Date:
OSTI Identifier:
22486803
Resource Type:
Journal Article
Resource Relation:
Journal Name: Journal of Solid State Chemistry; Journal Volume: 230; Other Information: Copyright (c) 2015 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.; Country of input: International Atomic Energy Agency (IAEA)
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; ABSORPTION SPECTROSCOPY; CRYSTAL STRUCTURE; MONAZITES; NMR SPECTRA; PHOSPHORUS 31; PLUTONIUM PHOSPHATES; POWDERS; RESOLUTION; SOLID SOLUTIONS; SOLIDS; TEMPERATURE RANGE 0273-0400 K; VALENCE; X-RAY DIFFRACTION; X-RAY SPECTROSCOPY

Citation Formats

Popa, Karin, Raison, Philippe E., E-mail: philippe.raison@ec.europa.eu, Martel, Laura, Martin, Philippe M., Prieur, Damien, Solari, Pier L., Bouëxière, Daniel, Konings, Rudy J.M., and Somers, Joseph. Structural investigations of Pu{sup III} phosphate by X-ray diffraction, MAS-NMR and XANES spectroscopy. United States: N. p., 2015. Web. doi:10.1016/J.JSSC.2015.07.002.
Popa, Karin, Raison, Philippe E., E-mail: philippe.raison@ec.europa.eu, Martel, Laura, Martin, Philippe M., Prieur, Damien, Solari, Pier L., Bouëxière, Daniel, Konings, Rudy J.M., & Somers, Joseph. Structural investigations of Pu{sup III} phosphate by X-ray diffraction, MAS-NMR and XANES spectroscopy. United States. doi:10.1016/J.JSSC.2015.07.002.
Popa, Karin, Raison, Philippe E., E-mail: philippe.raison@ec.europa.eu, Martel, Laura, Martin, Philippe M., Prieur, Damien, Solari, Pier L., Bouëxière, Daniel, Konings, Rudy J.M., and Somers, Joseph. 2015. "Structural investigations of Pu{sup III} phosphate by X-ray diffraction, MAS-NMR and XANES spectroscopy". United States. doi:10.1016/J.JSSC.2015.07.002.
@article{osti_22486803,
title = {Structural investigations of Pu{sup III} phosphate by X-ray diffraction, MAS-NMR and XANES spectroscopy},
author = {Popa, Karin and Raison, Philippe E., E-mail: philippe.raison@ec.europa.eu and Martel, Laura and Martin, Philippe M. and Prieur, Damien and Solari, Pier L. and Bouëxière, Daniel and Konings, Rudy J.M. and Somers, Joseph},
abstractNote = {PuPO{sub 4} was prepared by a solid state reaction method and its crystal structure at room temperature was solved by powder X-ray diffraction combined with Rietveld refinement. High resolution XANES measurements confirm the +III valence state of plutonium, in agreement with valence bond derivation. The presence of the americium (as β{sup −} decay product of plutonium) in the +III oxidation state was determined based on XANES spectroscopy. High resolution solid state {sup 31}P NMR agrees with the XANES results and the presence of a solid-solution. - Graphical abstract: A full structural analysis of PuPO{sub 4} based on Rietveld analysis of room temperature X-ray diffraction data, XANES and MAS NMR measurements was performed. - Highlights: • The crystal structure of PuPO{sub 4} monazite is solved. • In PuPO{sub 4} plutonium is strictly trivalent. • The presence of a minute amount of Am{sup III} is highlighted. • We propose PuPO{sub 4} as a potential reference material for spectroscopic and microscopic studies.},
doi = {10.1016/J.JSSC.2015.07.002},
journal = {Journal of Solid State Chemistry},
number = ,
volume = 230,
place = {United States},
year = 2015,
month =
}