In this study, cylindrical porous glass tablets were plated by palladium using electroless plating technique. Hypophosphite and Co(II) complexes were used as reducing agents in the prepared plating baths. Experiments were carried out in an especially designed glass vessel in which helium gas was continuously bubbled through the solution to create uniform concentration and to remove hydrogen gas from the surface for the case of hypophosphite-based procedure. XRF analysis of the upper layer of the composite membrane prepared by the hypophosphite-based bath showed a Pd/Si ratio of 4.6. SEM photographs indicated impregnation of Pd into the substrate upto 200 mu m. However, the thickness of the dense Pd layer was only about 15 mu m. SEM photographs and XRF results showed that hypophosphite-based bath was much more successful than the Co(II) complex-bath in Pd plating. Permeation experiments carried out at different temperatures showed that the contribution of surface diffusion to the permeation was significant at low temperatures and solution-diffusion mechanism was not important in the 40-200 degrees C temperature range for these membranes. The selectivity ratio for H-2/N-2 was found to be about 7 at 200 degrees C. (c) 2005 Elsevier B.V. All rights reserved.