The self-diffusion coefficient, D-m, interaction parameter, k(f), and hydrodynamic radius, R(h)(m), of the acrylic ester of omega-methoxy polyethylene glycol macromonomer micelles were determined by a cyclic voltammetric technique using Co(sep)Cl-3 as the redox-active electrochemical probe. A self-diffusion coefficient of the above macromonomer was also determined by Fourier transform pulsed gradient spin-echo (FT-PGSE) NMR technique. It has been found that the D-m is useful in measuring the critical micelle concentration of the macromonomer.