Arenesulfonic mesoporous materials [SBA(R), 0.05 B R (incorporation ratio) B0.15] have been prepared by the co-condensation of tetraethoxysilane (TEOS) and 2-(4-chlorosulfonylphenyl) ethyltrimethoxysilane (CSPTMS) in acidic solutions of Pluronic P123. The extent of the surface functionalisation and the nature of the interactions between sulfonic groups and the surface in SBA(0.05) and SBA(0.15) samples were investigated by FT-IR spectroscopy using two probes of different basic strengths. It was shown that carbon monoxide (CO, at 77 K) can be used as a good probe to study the surface functionalisation through the m C=O vibration at 2,158 cm -1 corresponding to its interaction with free silanol groups. Ammonia (NH 3 , at 423 K) is able to disturb the strong interactions of Si-OH-H 3 OS by forming the d NH -NH 4 ? which allowed to emphasise that SO 3 H groups of the less functionalised material SBA(0.05) are less acidic since the number of the acid groups is less important than in SBA(0.15).