In situ characterization of catalysts provides important information on the catalyst and the understanding of its activity and selectivity for a specific reaction. TPX techniques for catalyst characterization reveal the role of the support on the stabilization and dispersion of the active sites. However, these can be altered at high temperature since sintering of active species can occur as well as possible carbon deposition through the Bosch reaction, which hinders the active species and deactivates the catalyst. In situ characterization of the spent catalyst, however, may expose the causes for catalyst deactivation. For example, a simple TPO analysis on the spent catalyst may produce CO and CO2 via a reaction with O2 at high temperature and this is a strong indication that deactivation may be due to the deposition of carbon during the Sabatier reaction. Other TPX techniques such as TPR and pulse chemisorption are also valuable techniques when they are applied in situ to the fresh catalyst and then to the catalyst upon deactivation.