Adsorption is an important technique that significances the characteristics of porous solid materials and fine powders. The importance of porous solid materials and fine powders has been recognized when porous coal used for various applications such as catalysis, separation, isolation, sensors, chromatography, etc. Herein, the synthesis of mesoporous activated carbon derived from agricultural waste using TiO2. The TiO2-modified carbon was characterized employing scanning electron microscope (SEM), attenuated total reflection-Fourier transform infrared (ATR-FTIR) spectroscopy, powder X-ray diffraction (pXRD), Brunauer–Emmett–Teller (BET) surface area analyzer and X-ray photoelectron spectroscopy (XPS). The obtained results suggested that the TiO2-modified carbon could be a potential material for various application like dye removal, metal removal and allied areas. This book chapter describes the commonly used classifications of porous bulk materials and also reported here the characterization of porous solid materials and fine powders with special reference to the evaluation of the surface area, pore size distribution and thermodynamic parameters of the different mesoporous material, at various scales of resolution using relevant techniques. These materials comprise several levels of structures that of the mesopores, micropores as well as macropores. The apparent topography analysis of these materials, of various pore diameters, synthesized in our laboratory has been determined at various scales with the help of various characterization techniques.