The homopolymers and triblock copolymers were studied by CD spectroscopy in solution. The CD spectra of all chiral polymers showed notable CE in methanol, and CD spectra of chiral triblock copolymers retained clear CE in water as well. It indicates that chiral polymers (including chiral block) form secondary structure in solution. Both A-pEtEtOx-A and A-pPrMeOx-A series copolymers formed rather heterogeneous self-assemblies in aqueous solution.