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The adsorption of gases in porous solids such as zeolites and activated carbons, has been widely applied in cases of separation, purification and bottling of gases (Ruthven et al. 1994; Yang, 1997; Bastos-Neto et al. 2005a; Figueroa et al., 2008; Belmabkhout and Sayari, 2009). This potential is reflected not only in increasing the number of technical and scientific articles and patents, but also in the world market growth in plants for air separation and purification processes of hydrogen and natural gas and many others (Zimmermann and Keller, 2003). Due to the various applications of porous adsorbents, many research groups in various parts of the world have sought to develop and improve these materials to improve performance in these specific applications (Bastos-Neto et al. 2005b; Arou et al., 2008; Prauchner and Rodriguez-Reinoso, 2008; Rivers and Smith, 2009). In the procedures for obtaining porous solids, it is necessary to control the various process variables such as preparation, carbonization temperature and time, type and concentration of activating agents, among others, since these activation parameters determine the chemical and physical properties of adsorbents. The textural characteristics are the most important properties of the adsorbents, since it indicates the implementation and performance of the solid obtained (Giraldo and Moreno, 2005). In addition, chemical properties also determine the adsorption properties of adsorbent and solid-fluid interactions. Nature of surface groups, hydrophobic or hydrophilic character and acidic or basic behavior are some of the relevant chemical properties of the adsorbents in adsorption processes. Since the physical and chemical properties of an adsorbent determine the application and performance of the same, it is necessary to determine precisely the parameters that characterize these materials such as surface area, microporosity, pore size distribution, heats of adsorption, among others. Several experimental techniques are used to characterize porous materials, for example, mercury porosimetry, adsorption of liquid nitrogen, x-ray diffraction, etc.. The technique most commonly used to characterize the texture of carbon adsorbents (ie surface area, properties of molecular sieve, size distribution of pores, etc.). Is the physical adsorption of gases and vapors. However, immersion calorimetry, with molecular probes of various molecular dimensions, and gas adsorption microcalorimetry techniques are also applied to characterize this type of solid (Denoyel et al., 1993, Gonzalez et al. 1995; Rouquerol et al. 1999, Navarrete et al., 2004; Garcia-Cuello et al., 2009). The aim of this

Calorimetric: A Tecnique Useful in Characterization of Porous Solid