International audienceTOF-SIMS (time of flight secondary ion mass spectrometry) has been used to analyse the surface composition of monophasic hybrid organic-inorganic materials (MHOIM). Gels of type RSiO1.5 obtained from monosilylated precursors RSi(OR')(3), (with R' = Me, Et and R = hydrogen, alkyl, halogenoalkyl, alkenyl, aromatic and ferrocenyl units) have been analysed and in each case, characteristic mass fragment ions of R groups have been detected and clearly identified owing to the high mass resolution of TOF-SIMS. The large variety of precursors used allows one to conclude that the monosilylated precursors lead, as expected, to solids in which the organic moiety is located at the surface. Thus TOF-SIMS appears to be an efficient tool for the detection of groups located at the surface of amorphous hybrid systems

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