In order to design effective adsorption systems for energy storage and gas purification it is necessary to develop novel adsorbent materials that are tailor-made on a nanoscale. It is critical to characterize not only the materials physical characteristics and gas phase thermodynamics, but also the mass transfer fundamentals of these novel systems. In addition, it is important to understand how both thermodynamics and mass transport impact the performance of fixed-bed systems. This research addresses these areas by examining three specific topics: the synthesis and characterization of novel nanoporous molecularly engineered adsorbent materials including templated carbons, metal organic frameworks (MOFs), and zeolite imidazolate frameworks (ZIFs); the determination of mass transport mechanisms in nanoporous materials via concentration-swing frequency response; and the sensitivity analysis and subsequent optimization of fixed bed adsorption systems.