Carboxymethyl-beta-cyclodextrin (CMCD) has been used to enhance Fenton (Fe2+ + H2O2 --> Fe3+ + HO. + OH-) degradation of hydrophobic organic pollutants in aqueous systems. It has been proposed that the enhancement was due to the formation of a pollutant/CMCD/Fe2+ ternary complex which enabled the degradation catalyst, Fe2+, to be closer to the target pollutant molecule so as to favor the degradation reaction. To investigate this theory, aqueous solutions containing CMCD, Fe2+, and anthracene or 2-naphthol were studied using fluorescence and NMR techniques. The fluorescence quenching results showed that in aqueous solution (pH > 3) anthracene or 2-naphthol was quenched more efficiently by Fe2+ in the presence of CMCD. When the less efficient quenchers Cd2+ or Ca2+ were added to the anthracene/CMCD/Fe2+ solution, the fluorescence was restored by displacing Fe2+ from its binding site near the pollutant. NMR spectra showed evidence of formation of a 2-naphthol/CMCD binary complex. Peak broadening of 2-naphthol when Fe2+ was added to the 2-naphthol/CMCD solution indicated binding of Fe2+ to the binary complex. Peak sharpening via iron displacement resulted from addition of Cd2+ or Ca2+ to the 2-naphthol/CMCD/Fe2+ solutions, further confirming the binding of Fe2+ to form the ternary complex. These results indicate that the pollutant/CMCD/Fe2+ ternary complex is formed in aqueous solution.