The characterization of the acidity of zeolites and related materials is of great importance for applications of these materials, particularly in the petrochemical industry and environmental sciences. This chapter provides a comparison of the two most widely used techniques for the study of acid/base properties of zeolites, namely temperature-programmed desorption and adsorption calorimetry. The information needed to perform and interpret these experiments as well as advantages and limitations of these methods are summarized. The curves and data obtained for the two most studied zeolites Y and ZSM-5 are discussed, which can be particularly useful for young researchers in this field.A.