A novel kind of polymeric surfactant based on carboxymethyl cellulose and poly(ethylene oxide) dodecyl ether acrylate (CMC-AR(12)EO(9)) was synthesized through ultrasonic irradiation. Aggregation behavior in aqueous solution at different temperatures and pH values was investigated by dynamic laser scattering and fluorescence probe. The results show that, with the increase of temperature, polymeric surfactants are favorable to form multimolecular micelles with narrower polydispersity of size distribution. At a higher temperature, the multimolecular micelles tend to aggregate bigger sized particles that are unstable and would be disaggregated at higher shear rate. At the elevated pH values, the size of micelles reduces drastically because of strong damage of alkali to aggregates, whereas nonpolar and insoluble domains formed by the hydrophobic blocks of polymeric surfactants are insensitive to pH changes. (c) 2005 Wiley Periodicals, Inc.