Volatile organic compounds (VOCs) comprise more than 60% of total hazardous air pollutants that are emitted by major industrial point sources. Adsorption by an activated carbon fiber has been recognized as one of the feasible regenerative control processes to separate and recover VOCs for reuse. The adsorption behavior of hexane and benzene in a single-component and in a mixture system onto activated carbon fabric cloth was studied. The adsorption capacities were evaluated using the Langmuir adsorption isotherm model. Depending upon the design of the experiment, we have concluded that internal diffusion controls the adsorption of benzene and n-hexane on activated carbon cloth.