The design and testing of kinetically-appropriate operando spectroscopic cells for investigating heterogeneous catalytic reactions

This tutorial review discusses some of the current designs of reaction cells used for operando spectroscopy (X-ray absorption, UV-vis, Raman, transmission FTIR and DRIFTS) and the relation to the apparent reaction kinetics. Beam effects, the control of the catalyst bed temperature and bed by-pass are some of the potential problems that may lead to flawed activity measurements. Finally, four examples are given in which a good agreement was obtained between the activity of a powdered catalyst measured in a conventional reactor and in a spectroscopic cell. It is proposed that such comparison between reactors should become a standard procedure, to ensure the correctness of the data collected over typically non-ideal spectroscopic reaction cells.