A recent pathway for obtaining regular mesoporous materials (silicas and carbons) in one step was explored in this work using TEOS, P123 and sucrose as a starting base template. The synthesis was catalyzed by H 2 SO 4 . The mesoporous carbon was obtained by carbonization of the previous mixture and the removal of the silica template. In contrast, when the composite mixture was heated in air, a mesoporous silica was obtained. The results showed that the “one-pot” method presented some difficulties in controlling the synthesis variables. All the silica samples presented a more regular pore-size distribution than the respective carbon replicate. The specific surface areas (A BET ) of the prepared materials were in the range 500–600 m 2 /g for the silica samples and within the range 1000–1200 m 2 /g for the carbon samples.