The removal of volatile organic compounds (VOCs) has been an urgent task all over the world because they are the main substances for environmental problems. Removal by adsorption technique is the most convenient method. Until now, adsorption by activated carbon has been studied in many cases. However, activated carbon has a fire risk and requires a large amount of energy to regenerate the adsorbent. Therefore, siliceous materials have been expected as novel adsorbents instead of activated carbon. We have been able to synthesize porous silica having super-micropores of about 0.8 nm by using collagen fibril as a template. In the present study, the author evaluates toluene dynamic adsorption/ desorption properties of this super-microporous silica (SMPS) as well as the characterization studies. It was found that SMPS showed very high dynamic adsorption/desorption properties in comparison with other siliceous materials such as mesoporous silica MCM-41, commercial microporous silica gel, and HY zeolite. SMPS synthesized by using collagen fibril as a template can be expected as a novel VOCs adsorbent.