Over the past decades, there have been worldwide efforts to synthesize new types of ordered porous materials for catalysis, separations, etc. Among those, mesoporous material with microporous walls are promising in a sense that while mesopores act as channels for the reactant transport with little diffusion limitation, micropores in the wall act as active sites for reactions or storage of the molecules. In this study, we focused on the SBA-15 material, which is a highly ordered mesoporous silica material with micropores present in the wall. We have studied the synthesis of the material by manipulating various factors that are known to have influence on the porous characteristic of the material. We have aimed our studies particularly on the micropores present in the material. Unlike zeolite materials, which have regular, well characterized pore structures, micropores in the SBA-15 are not ordered, thus may have a very broad pore size distribution. We have synthesized sets of mesoporous silica materials that have characteristics similar to those reported in the literature. Using microwave heating, we were able to synthesize the target material within a short period of time, about 10 to 12-fold reduction of the conventionally known synthesis time. The synthesized materials were initially characterized using XRD and SEM. Adsorption studies were then undertaken on the materials to determine the surface area and pore structure. The interpretation of micropores has heretofore been problematic and the models are ambiguous. Relatively simply ordered, 1-dimensional channel type, zeolite materials were also studied; MTW, MTT, TON, ATS, VET frameworks. Adsorption isotherms of these materials were obtained and simple empirical models were developed to determine the pore size distribution. Further, a sequential adsorption technique, using n-nonane as a preadsorbate, was used to evaluate the realistic external surface areas of zeolite materials and mesopore surface areas of micro-mesoporous materials. Applying this technique to “multidimensional pore system” will provide another way to obtain the realistic surface area and mesopore size distribution.