A new regular ABA-type triblock copolymer has been synthesized by polycondensation of the acid chloride of carboxy-terminated butadience-acrylonitrile rubber (CTBN) with hydroxyterminated polyethylene isophthalate (PEI) oligomer. This block copolymer was characterized by elemental (nitrogen) analysis, vapor pressure osmometry, viscometry, and IR and NMR spectroscopy. Quantitative estimation of block segments has been carried out by measuring the area under peaks assigned to various protons in the NMR spectrum of the polymer. NMR spectral analysis has been found to agree well with the nitrogen analysis of the polymer. The solubility and solution viscosity behavior of the polymer has also been studied.