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

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