TY - JOUR A1 - Bentrup, U. A1 - Radnik, J. A1 - Armbruster, U. A1 - Martin, A. A1 - Leiterer, Jork A1 - Emmerling, Franziska A1 - Brückner, A. T1 - Linking simultaneous in situ WAXS/SAXS/Raman with Raman/ATR/UV-vis spectroscopy: comprehensive insight into the synthesis of molybdate catalyst precursors JF - Topics in catalysis N2 - 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. KW - In situ KW - WAXS/SAXS KW - Raman KW - ATR KW - UV-vis KW - Mixed oxide catalyst KW - Synthesis PY - 2009 DO - https://doi.org/10.1007/s11244-009-9309-y SN - 1022-5528 VL - 52 IS - 10 SP - 1350 EP - 1359 PB - Springer Science + Business Media CY - Dordrecht AN - OPUS4-19794 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -