The calcination and thermal degradation behaviors of surfactants in mesoporous silicas SBA-15 and MCM-41 were investigated by FT-IR, C-13 CP/MAS NMR, TG/DTA, and GPC. It was found that carboxylic acid-containing products were generated as active components in the mesopores of SBA-15 and MCM-41 from the triblock copolymer (PEO)(20)(PPO)(70)(PEO)(20) and cetyltrimethylammonium bromide (CTAB), respectively; the latter materials were used as templates. The carboxylic acid-containing mesoporous silica obtained showed a catalytic activity for hydrolysis of sucrose. The acidity was evaluated by means of NaOH titration. The acidity sensitively depended on both the calcination temperature and the atmosphere; the maximum appeared at 150 degrees C in air for SBA-15 where the highest activity was observed. However, the product in MCM-41 showed a lower catalytic activity than that in SBA-15. The SBA-15 product was easily leached from the mesopores of SBA-15 into the solution, but the degree of leaching for MCM-41 was considerably smaller than that for SBA-15. (C) 2009 Elsevier B.V. All rights reserved.