Existing carbon-based adsorbents contain high internal surface areas and desirable pore structures, making them effective materials for gas purification, separation, and storage. A method for synthesizing a new class of carbon-based materials that could be attractive adsorbents for many environmental and energy applications was developed. Adsorption capacities of synthesized carbons were determined for methyl ethyl ketone using a gravimetric balance. The fixed-bed pyrolysis system showed several advantages in comparison to the ultrasonic spray pyrolysis system, e.g., elimination of the aerosol production step is eliminated. Carbons prepared by the fixed-bed method were highly microporous. This fixed-bed pyrolysis technique provided control for synthesizing carbons with properties that are pivotal to adsorption capacity including surface area and particle diameter. Environmental applications were determined by evaluating their adsorption performances using select adsorbates, e.g., VOC and mercury. This is an abstract of a paper presented at the 101st AWMA Annual Conference and Exhibition (Portland, OR 6/24-27/2008).