Abstract
An operando DRIFT-MS system (Diffuse Reflectance Infrared Fourier Transform Spectroscopy coupled with Mass Spectrometry) was designed and set up to study the oxidative steam reforming of ethanol reaction (OSRE). This reaction involves the mixture of water, ethanol and oxygen to produce mainly hydrogen, which is a rather attractive energy carrier. Spectroscopic monitoring of the process is a key tool to contribute to the understanding of: i) the dynamics on the catalyst surface, ii) the reaction mechanism and iii) the effect of the solid's properties on the catalytic process. In this sense, this document sets forth the experimental design that allows to carry out the study under operando DRIFT-MS conditions through time for the OSRE reaction. Selection criteria for parameters, materials, configuration, and experimental conditions are included, particularly optimizing the parameters of particle size and the dilution factor with KBr as well as the temperature and flow conditions for carrying out the reaction.•Clear signals of the adsorbed species in IR that do not present interference by water in the reaction atmosphere.•Simple assembly and online product detection by MS that allow to follow the change in the products of the OSRE reaction according to the temperature.•Controlled entry of gases and quantification by loop injection.