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The photophysical and solution properties of naphthalene-labeled styrene/N,N-dimethyl maleimido propylammonium propane sulfonate copolymer, poly(SDMPAPS)/NA, were studied in terms of fluorescence, cloud point, and viscosity measurements. The ratio of intensities of the excimer and monomer fluorescence (I E/I M) was shown as a function of polymer concentration in deionized water. The value of I E/I M decreases with an increase in the salt concentration. The addition of anionic surfactants to the aqueous solution of poly(SDMPAPS)/NA can either induce or break the interpolymer aggregation. When the electrolyte concentration increases, the Stern−Volmer quenching constant (K sv) also increases. The phase behavior of poly(SDMPAPS)/NA shows an upper critical solution temperature around 17 °C. The intrinsic viscosity of the poly(SDMPAPS)/NA in the presence of different salts reflects the influence of these salts on the hydrodynamic volume of the polymer chain for poly(SDMPAPS)/NA. A model of the interaction between poly(SDMPAPS)/NA and surfactant in aqueous solution is proposed.