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X-ray spectroscopy for chemistry in the 2-4 keV energy regime at the XMaS beamline: ionic liquids, Rh and Pd catalysts in gas and liquid environments, and Cl contamination in γ-Al2O3.
Thompson, Paul B J; Nguyen, Bao N; Nicholls, Rachel; Bourne, Richard A; Brazier, John B; Lovelock, Kevin R J; Brown, Simon D; Wermeille, Didier; Bikondoa, Oier; Lucas, Christopher A; Hase, Thomas P A; Newton, Mark A.
Afiliación
  • Thompson PB; XMaS, UK CRG, ESRF, 71 Avenue des Martyrs, 38043 Grenoble, France.
  • Nguyen BN; School of Chemistry, University of Leeds, Leeds LS2 9JT, UK.
  • Nicholls R; School of Chemistry, University of Leeds, Leeds LS2 9JT, UK.
  • Bourne RA; School of Chemistry, University of Leeds, Leeds LS2 9JT, UK.
  • Brazier JB; Department of Chemistry, Imperial College London, South Kensington Campus, London SW7 2AZ, UK.
  • Lovelock KR; Department of Chemistry, Imperial College London, South Kensington Campus, London SW7 2AZ, UK.
  • Brown SD; XMaS, UK CRG, ESRF, 71 Avenue des Martyrs, 38043 Grenoble, France.
  • Wermeille D; XMaS, UK CRG, ESRF, 71 Avenue des Martyrs, 38043 Grenoble, France.
  • Bikondoa O; XMaS, UK CRG, ESRF, 71 Avenue des Martyrs, 38043 Grenoble, France.
  • Lucas CA; Department of Physics, University of Liverpool, Oliver Lodge Laboratory, Liverpool L69 7ZE, UK.
  • Hase TP; Department of Physics, University of Warwick, Gibbet Hill Road, Coventry CV4 7AL, UK.
  • Newton MA; Department of Physics, University of Warwick, Gibbet Hill Road, Coventry CV4 7AL, UK.
J Synchrotron Radiat ; 22(6): 1426-39, 2015 Nov.
Article en En | MEDLINE | ID: mdl-26524308
The 2-4 keV energy range provides a rich window into many facets of materials science and chemistry. Within this window, P, S, Cl, K and Ca K-edges may be found along with the L-edges of industrially important elements from Y through to Sn. Yet, compared with those that cater for energies above ca. 4-5 keV, there are relatively few resources available for X-ray spectroscopy below these energies. In addition, in situ or operando studies become to varying degrees more challenging than at higher X-ray energies due to restrictions imposed by the lower energies of the X-rays upon the design and construction of appropriate sample environments. The XMaS beamline at the ESRF has recently made efforts to extend its operational energy range to include this softer end of the X-ray spectrum. In this report the resulting performance of this resource for X-ray spectroscopy is detailed with specific attention drawn to: understanding electrostatic and charge transfer effects at the S K-edge in ionic liquids; quantification of dilution limits at the Cl K- and Rh L3-edges and structural equilibria in solution; in vacuum deposition and reduction of [Rh(I)(CO)2Cl]2 to γ-Al2O3; contamination of γ-Al2O3 by Cl and its potential role in determining the chemical character of supported Rh catalysts; and the development of chlorinated Pd catalysts in `green' solvent systems. Sample environments thus far developed are also presented, characterized and their overall performance evaluated.
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Texto completo: 1 Colección: 01-internacional Base de datos: MEDLINE Idioma: En Revista: J Synchrotron Radiat Asunto de la revista: RADIOLOGIA Año: 2015 Tipo del documento: Article País de afiliación: Francia Pais de publicación: Estados Unidos

Texto completo: 1 Colección: 01-internacional Base de datos: MEDLINE Idioma: En Revista: J Synchrotron Radiat Asunto de la revista: RADIOLOGIA Año: 2015 Tipo del documento: Article País de afiliación: Francia Pais de publicación: Estados Unidos