The high temporal resolution in data acquisition, possible in the quick‐scanning EXAFS (QEXAFS) mode of operation, provides new challenges in efficient data processing methods. Here a new approach is developed that combines an easy to use interactive graphical interface with highly optimized and fully parallelized Python‐based routines for extracting, normalizing and interpolating oversampled time‐resolved XAS spectra from a raw binary stream of data acquired during operando QEXAFS studies. The programs developed are freely available via a Github repository.

The heterogenization of Wacker catalysts using chloride-free systems can potentially be a good alternative for the commercial homogeneous Wacker oxidation of ethylene, which utilizes excessive aqueous chloride solvents. However, the mechanism of the heterogeneous system has not been clarified, preventing the rational design of better catalysts. Here, we report a transient X-ray absorption spectroscopic (XAS) investigation of the heterogeneous Wacker oxidation over Pd-Cu/zeolite Y coupled with kinetic studies and chemometric analysis. Insight is obtained by operando quickXAS allowing the quantitative determination of rates and thereby revealing a rapid redox reaction involving copper. Our work demonstrates that copper is not only the site of oxygen activation, but is also involved in the formation of undesired carbon dioxide. Without detecting the presence of Cu(0) and Pd(I), our results suggest that two one-electron transfers to two Cu(II) ions to reoxidize Pd(0) is at work in this heterogeneous Wacker catalyst.