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x‐ray absorption spectroscopy is a well‐suited technique to uncover the structure of heterogeneous catalysts under reaction conditions. Different aspects of in situ cell design suitable for dynamic and catalytic studies are discussed. In addition, criteria are presented that allow estimating the influence external and internal mass transfer. Starting with studies on gas‐solid reactions, including structure‐activity relationships, this concept is extended to liquid‐solid reactions, reactions at high pressure and in supercritical fluids. The following examples are discussed in more detail: partial oxidation of methane over Pt‐Rh/Al2O3, reduction of a Cu/ZnO catalyst, alcohol oxidation over Bi‐promoted Pd/Al2O3 in liquid phase and over Pd/Al2O3 in supercritical CO2, and batch reactions (e.g. CO2‐fixation over zinc‐based catalysts).

Time-Resolved and Operando XAS Studies on Heterogeneous Catalysts — From the Gas Phase Towards Reactions in Supercritical Fluids