Well defined amphiphilic diblock copolymers of poly(styrene-b-vinylbenzylphosphonic acid) (PS-b-PVBPA) were prepared by controlled radical polymerization technique, two-step hydrolysis reactions using trime-thylsilyl bromide from the corresponding phosphonic ethyl ester. By indirect, backward pH titration of the block copolymer, a good titration curve of a dibasic acid was observed. The IEC values obtained from both backward pH titration and volumetric back titration were almost identical. Thermal gravimetric analysis (TGA) of the phosphonic acid containing block copolymer showed a high thermal stability up to $400^{circ}C$.