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A novel laboratory setup for combined operando X‐ray diffraction and Raman spectroscopy of catalytic solids with online product analysis by gas chromatography is presented. The setup can be used with a laboratory‐based X‐ray source, which results in important advantages in terms of time‐on‐stream that can be measured, compared to synchrotron‐based experiments. The data quality was much improved by the use of a relatively high‐energy MoK α  radiation instead of the more conventional CuK α  radiation. We have applied the instrument to study the long‐term deactivation of Co/TiO 2  Fischer–Tropsch synthesis (FTS) catalysts. No sign of Co sintering or bulk oxidation was found during the experiments. However, part of the metallic Co was converted into cobalt carbide (Co 2 C), at elevated pressure (10 bar). Furthermore, graphitic‐like coke species are clearly formed during FTS at atmospheric pressure, whereas at elevated pressure fluorescence hampered the interpretation of the measured Raman spectra.

chemcatchem

Combined Operando X‐ray Diffraction/Raman Spectroscopy of Catalytic Solids in the Laboratory: The Co/TiO 2  Fischer–Tropsch Synthesis Catalyst Showcase