Mesostructured carbon (MSC) has been synthesized by the carbonization of assynthesized mesocellular siliceous foam (MCF)/P123 nanocomposite followed by the dissolution of the silica using 10 wt.% HF solution. SEM, TEM, and BET instruments were used to characterize the mesostructured carbon. Batch experiments were performed to evaluate its ability to adsorb natural organic matter (NOM) in various pH levels. MSC showed enhanced adsorption capacity for NOM than the commercial activated carbons. MSC possessed approximately 3.3 and 2.2 times greater the solid-water partitioning coefficient of NOM, Kd, at pH 7 than coal-based and coconutbased activated carbons, respectively. This increased Kd of MSC resulted from mesoporous structures in the range of 4-6 nm on the surface. The Kd value decreased with increasing initial pH levels, which is considered to be due to ionization of functional groups of NOM.