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The isosteric enthalpy of adsorption (∆ads h) of CO2 in three different micro and mesoporous materials was evaluated in this work. These materials were a microporous material with functional groups of nitrogen and oxygen (CMFs, carbon microfibers), a mesoporous material with silanol groups (SBA-15, Santa Barbara Amorphous), and a mesoporous material with amine groups (SBA15_APTES, SBA-15 amine-functionalized with (3-Aminopropyl)-triethoxysilane). The temperature interval explored was between 263 K and 303 K, with a separation of 5 K between each one, so a total of nine CO2 isotherms were obtained. Using the nine isotherms and the Clausius–Clapeyron equation, the reference value for ∆adsh was found. The reference value was compared with those ∆adsh obtained, considering some arrangement of three or five CO2 isotherms. Finally, it was found that at 298 K and 1 bar, the total amount of CO2 adsorbed is 2.32, 0.53, and 1.37 mmol g−1 for CMF, SBA-15, and SBA-15_APTES, respectively. However, at a coverage of 0.38 mmol g−1, ∆adsh is worth 38, 30, and 29 KJ mol−1 for SBA-15_APTES, CMFs, and SBA-15, respectively. So, physisorption predominates in the case of CMF and SBA-15 materials, and the ∆adsh values significantly coincide regardless of whether the isotherms arrangement used was three or five. Meanwhile, in SBA15_APTES, chemisorption predominates as a consequence of the arrangements used to obtain ∆adsh. This happens in such a way that the use of low temperatures (263–283 K) tends to produce higher ∆adsh values, while the use of high temperatures (283–303 K) decreases the ∆adsh values. [ABSTRACT FROM AUTHOR]