The applicability of glycerinedimethacrylaturethanetriethoxysilane (GUS)-based ORMOCER (organic-inorganic hybrid copolymers) resin for the fabrication of free-standing ORMOCER-zeolite Beta (BEA) nanocomposite membrane was studied in detail. A series of ORMOCER/zeolite Beta nanocomposite membranes having different zeolite loadings (20-40 wt.%) were prepared by solution casting method followed by UV-curing, and characterized by thermal analysis (TG/DSC), scanning electron microscopy (SEM) and N-2 sorption and single gas (H-2, He and N-2) permeation measurements. The SEM studies revealed that zeolite Beta crystallites were homogeneously distributed within the ORMOCER matrix. There were no visible voids or defects between the ORMOCER matrix and the zeolite Beta crystallites, even at a very high zeolite loading (40 wt.%), as revealed by the high resolution SEM images. The ORMOCER-zeolite Beta nanocomposite membrane with 40wt.% zeolite loading showed a nearly 16-times increase in H-2 and He permeabilities in comparison to the pure ORMOCER membrane. (C) 2009 Elsevier B.V. All rights reserved.