Sedimentation equilibrium measurements were made on an amphiphilic statistical copolymer p(AMPS/C6) made of sodium 2-(acrylamido)-2-methylpropane-sulfonate (AMPS) and n-hexyl methacrylate (C6), dissolved in water-methanol mixtures with 0.2 M LiClO 4 and different methanol contents over a wide polymer concentration range. The experimental results were analyzed in terms of a micellar solution theory for amphiphilic polyelectrolytes to estimate the aggregation number m of the micelle and the internal free energy change Á m =m (per polymer chain) due to micellization. Both m and Á m =m decreased with increasing the methanol content in the solvent. In addition, dynamic light scattering for the same copolymer system indicated that p(AMPS/C6) formed a uni-core star-like micelle in water-methanol mixture with the methanol mole fractions of 0 and 0.06.KEY WORDS: Micelle / Amphiphilic Polymer / Statistical Copolymer / Sedimentation Equilibrium / Dynamic Light Scattering / Amphiphilic copolymers form micelles in aqueous media due to the strong hydrophobic interaction among the polymer chains.1 The micellization is important for their applications to the rheology modifier, emulsifier, drag delivery system, and so on, 2-4 because the micellization changes remarkably their solution properties. In the practical applications for those purposes, their aqueous solutions are often mixed with various additives, e.g., low molar mass organic compounds, salts, surfactants, and other polymers. Those additives can modify the micellization behavior of the polymers in aqueous media by interacting with the hydrophobic or hydrophilic moieties of the copolymer chain, so that it is essentially important to understand the effect of additives on the micellization behavior in aqueous solutions of amphiphilic copolymers.Recently, Hashidzume et al. 5 investigated the micellar structure of an amphiphilic statistical copolymer p(AMPS/C6), made of sodium 2-(acrylamido)-2-methylpropane-sulfonate (AMPS) and n-hexyl methacrylate (C6), in aqueous salt solution. The copolymer aggregation number m of the micelle and the number of hydrophobic cores per micelle depended on the copolymer molecular weight and hydrophobic monomer content. Furthermore, their hydrodynamic radius data indicated that the copolymer formed a uni-core star-like micelle at low copolymer molecular weights.Afterward, Nojima et al. 6 refined the data analysis for the p(AMPS/C6) micelle in aqueous salt solution by taking into account the association-dissociation equilibrium in the micellar solution. Using a micellar solution theory for amphiphilic polyelectrolytes, they estimated more precise m for the p(AMPS/C6) micelle in aqueous salt solution.In the present study, we have made sedimentation equilibrium and dynamic light scattering measurements on p(AMPS/C6) dissolved in water-methanol mixtures with 0.2 M LiClO 4 and different methanol mole fraction x methanol . Applying the micellar solution theory, we have estimated m and also the internal free energy change Á m =m due to micellization...