Solubilization of octafluoronaphthalene (OFN) by fluorocarbon and hydrocarbon surfactants in aqueous solutions has been examined to investigate the effects of mixing surfactants and added salt. Diethylammonium perfluorononanoate (DEAPFN) micelles have the most solubilization power toward OFN. The difference in micellar solubilization power will be caused by the hydrophobicity of ionic groups and micellar size. Large positive synergistic effects on solubilization behavior were observed in the DEAPFN-diethylammonium tetradecyl sulfate mixed micellar systems. Solubilization of OFN depended on the concentrations of added salt and the aggregation number, that is, the micellar size.