One of the simplest and powerful Controlled Radical Polymerization (CRP) techniques is atom transfer radical polymerization. It has been widely studied and utilized since new polymeric materials synthesis using novel structures can be achieved by polymerizing many monomers under simple conditions. Polymers with low polydispersity and controlled molecular weight can be obtained using the ATRP technique since it has synthetic flexibility and simplicity. Polymerizations were performed to prepare two ABA triblock copolymers with three monomers in two different batches where A=2-diethylamino ethyl methacrylate (DEA) B=2-Hydroxyethyl Methacrylate (HEMA) in the first batch. In contrast, A (i.e., DEA) was replaced by methyl methacrylate (MMA) in the second batch. Therefore, the resulting two-triblock copolymers were DEAHEMA- DEA and MMA-HEMA-MMA. This process was carried out using transition metal catalyst Cu (I) Br, 2, 2′-bipyridine (bpy) as a ligand and diethyl meso-2, 5-dibromoadipate as a bifunctional ATRP initiator in Methanol at room temperature. The resulting block copolymers were analyzed for polymer conversion using a 500MHz Bruker Avance 1H NMR spectrophotometer in deuterated Methanol (CD3OD) and micelle formation, which was analyzed by changing solvents (D2O and CDCl3).