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Continuous tubular flow reactor for XAFS studies of organometallic reactions: Possibilities and limitations for studies of the Soai reaction

Luanga N Nchari1, Guy A Hembury1, Angela M Beesley1, David J Meehan2, Nikolaos Tsapatsaris1, Matthew Hudson1, Matthew Thomason2 and Sven L M Schroeder1,2

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A computer-controlled continuous tubular flow reactor system has been commissioned that permits time-resolved in situ XAFS measurements of organometallic reactions. The system was commissioned by Zn K-edge measurements of products formed during the Soai reaction. XANES data are shown that illustrate the quality of the data that can be achieved. The XANES spectra are compatible with the presence of dimer, trimer or other oligomeric alkoxide species in the Soai process. It is shown how heterogeneity in the Soai reaction system leads to considerable complications with the measurements due to the formation of floating particles of the aldehyde/iPr2Zn adduct formed in the reaction; additionally, decomposition of iPr2Zn with residual air and moisture leads to deposits on cell walls.


PACS

82.80.Ej X-ray, Mössbauer, and other gamma-ray spectroscopic analysis methods

82.65.+r Surface and interface chemistry; heterogeneous catalysis at surfaces

82.30.Lp Decomposition reactions (pyrolysis, dissociation, and fragmentation)

78.70.Dm X-ray absorption spectra

78.47.-p Spectroscopy of solid state dynamics

Subjects

Condensed matter: electrical, magnetic and optical

Surfaces, interfaces and thin films

Chemical physics and physical chemistry

Dates

Issue 1 (2009)



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