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Abstract: CdS nanoparticles, prepared in reverse micellar systems, were immobilized onto two types of thiol-modified periodic mesoporous organosilicates (PMOS), t-PMOS(I) and t-PMOS(II) by a simple procedure via the addition of t-PMOS and mild stirring. A particle-sieving effect of the t-PMOS was observed, in that the immobilization of the CdS nanoparticles was decreased with increasing the nanoparticle size. The resulting CdS-PMOS(I) and CdS-PMOS(II) were then used as photocatalysts for the generation of H2 from 2-propanol aqueous solution. CdS-PMOS(II), which was more stable against photoirradiation, showed higher photocatalytic activity, compared to CdS-PMOS(I). The quantity of H2 generated on the PMOS-immobilized CdS nanoparticles was greater than that obtained from mesoporous silica (MCM-41)-immobilized CdS nanoparticles (CdS-L-FM41). [Copyright &y& Elsevier]