Poly [azo(8hydroxyquinoline)] (PAHQ) was synthesized by alcoholic alkaline reduction of 2, 4 dinitro1-napthol. The polymers synthesized at time intervals were characterized by elemental analysis, IR spectra and thermogravimetric analysis. The number Average molecular weight () was determined by non-aqueous titration. Polymetric metal chelates of Cu+2, Co+2, Mn+2, Zn+2, Ni+2 with PAHQ polymer were prepared and characterized.