Topics in Catalysis

, Volume 52, Issue 10, pp 1350–1359 | Cite as

Linking Simultaneous In Situ WAXS/SAXS/Raman with Raman/ATR/UV–vis Spectroscopy: Comprehensive Insight into the Synthesis of Molybdate Catalyst Precursors

  • Ursula Bentrup
  • Jörg Radnik
  • Udo Armbruster
  • Andreas Martin
  • Jork Leiterer
  • Franziska Emmerling
  • Angelika Brückner
Original Paper

Abstract

A new setup is presented which enables simultaneous wide- and small-angle X-ray scattering (WAXS/SAXS) and Raman spectroscopic experiments during the synthesis of Mo-based mixed oxide catalyst precursors at the μ-spot beamline at the Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung (BESSY). Furthermore, we report about the separate monitoring of the same reactions under comparable conditions by simultaneous combined ATR/UV–vis/Raman spectroscopic measurements. For testing the performance of both experimental setups two syntheses were described comprising the precipitation of metal molybdates by mixing solutions of metal nitrates and ammonium heptamolybdate. Additionally, the effect of H3PO4 admixture on precipitation was investigated. The combined evaluation of spectroscopic and WAXS/SAXS data allows the discrimination between different molybdate species appearing in solution and precipitate. Furthermore, these molybdate species could be assigned to separate phases of different crystallinity.

Keywords

In situ WAXS/SAXS Raman ATR UV–vis Mixed oxide catalyst Synthesis 

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Copyright information

© Springer Science+Business Media, LLC 2009

Authors and Affiliations

  • Ursula Bentrup
    • 1
  • Jörg Radnik
    • 1
  • Udo Armbruster
    • 1
  • Andreas Martin
    • 1
  • Jork Leiterer
    • 2
  • Franziska Emmerling
    • 2
  • Angelika Brückner
    • 1
  1. 1.Leibniz-Institut für Katalyse e.V. an der Universität RostockRostockGermany
  2. 2.Bundesanstalt für Materialforschung und -prüfungBerlinGermany

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