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Electrocatalytic hydrogenation of furfural on metal surfaces has become an important research subject due to the potential of the reaction product 2‐methylfuran as a renewable energy resource. Identifying effective determinants in this reaction process requires a thorough investigation of the complex electrode‐electrolyte interactions, which considers a variety of the influential components. In this work, in operando electrochemical Raman Spectroscopy and Molecular Dynamics simulations were utilized to investigate different characteristics of the interface layer in the electrocatalytic hydrogenation of furfural. Hereby, the influence of applied potentials, electrode material, and electrolyte composition were investigated in detail. The studied parameters give an insight into furfural's binding situation, molecular orientation, and reaction mechanism.
Electrochemical Raman spectroscopy can provide valuable insights into electrochemical reaction mechanisms. However, it also shows various pitfalls and challenges. This paper gives an overview of the necessary theoretical background, crucial practical considerations for successful measurement, and guidance for in situ/in operando electrochemical Raman spectroscopy. Several parameters must be optimized for suitable reaction and measurement conditions. From the experimental side, considerations for the setup, suitable signal enhancement methods, choice of material, laser, and objective lens are discussed. Different interface phenomena are reviewed in the context of data interpretation and evaluation.