Organically modified clay was used to adsorb volatile organic compounds from a gaseous phase. The organoclay was prepared by adsorbing hexadecyltrimethylammonium (HDTMA) on the surface of montmorillonite particles. Two volatile organic compounds (VOCs), chlorobenzene and trichloroethylene, were adsorbed to the organoclay using a fixed adsorption bed. The adsorption was carried out at various inlet concentrations of gaseous VOCs in a carrier gas (nitrogen). The adsorption behavior of VOCs was investigated using natural clay and two types of organoclays, which had different HDTMA loadings. Adsorption breakthrough curves were obtained, and the adsorption data were modeled with two adsorption isotherms. Desorption of VOCs was also conducted using pure nitrogen, and the desorption profiles were fitted with two different theoretical models. It was found that the organoclay possesses significant adsorption capacity towards VOCs and the uptake depends on the degree of HDTMA loading on clay surface.