For the past decade, active research on inorganic membranes has been carried out. Inorganic membranes have many advantages compared with organic membranes due to their chemical and thermal stability and high mechanical strength.Almost all asymmetric membranes are made by the sol-gel method [1]. This method is based on the hydrolysis, condensation and polymerization of metal alkoxides following sintering [2]. Sol is coated on the outer surface or inner surface of a porous support tube, which has a large pore size, and becomes a gel after drying. By the conventional sol-gel method, which involves deposition of particulate sol and calcination at a relatively high temperature (above 573 K), it is difficult to obtain a porous membrane with pore size less than 2 nm [3].However, we found that microporous xerogel membrane with pore diameter less than 1 nm coated on porous glass support could be obtained by a novel sol-gel method. This xerogel, prepared by evaporation of solvent from wet gel, is distinguished from ordinary porous ceramic green bodies by its small pore size and correspondingly enormous surface area. This method is peculiar in its application of low water content and low heat treatment temperature. The gas selectivity factor (ratio of the permeation rate) of the membrane attained about 20 for the He/N 2 system and about 50 for the CO2/Na system at 298 K.In this letter, we report the preparation of this novel microporous xerogel membrane and its gas separation characteristics.Xerogel layer was prepared using the sol-gel method. The silicate sol composition was tetraethoxysilane (TEOS):C2HsOH:H20:HC1 = 1:20:2:0.01 in molar ratio. Commercially available reagent grade chemicals were used. The mixture was stirred for several hours at room temperature to obtain homogeneous sol. Porous glass tubes with pore diameter of 4 nm, outer diameter of 5 mm, inner diameter of 4 mm and length of approximately 12 cm were used as the support. Support tubes, with one end closed, were dipped in the sol, withdrawn at a rate of 3 mlTIS -1, then dried at room temperature. After the dip-coating procedure had been repeated three times, the tubes were heated to 423 K at a rate of 0.5 Kmin -I and maintained at that temperature for 2 h, then cooled to room temperature. These coating and heating procedures were repeated twice and final specimens were obtained. The membrane were stored 0261-8028