8-Hydroxy-4-azoquinolinephenylmethacrylate (8H4AQPMA) was prepared and polymerized in ethyl methyl ketone (EMK) at 65 degrees C using benzoyl peroxide as free radical initiator. Poly(8-hydroxy-4-azoquinolinephenylmethacrylate) poly(8H4AQPMA) was characterized by infrared and nuclear magnetic resonance techniques. The molecular weight of the polymer was determined by gel permeation chromatography. Cu(II) and Ni(II) complexes of poly(8H4AQPMA) were prepared. Elemental analysis of polychelates suggests that the metal-ligand ratio is about 1:2. The polychelates were further characterized by infrared spectra, X-ray diffraction, spectral studies, and magnetic moments. Thermal analyses of the polymer and polychelates were carried out in air. (c) 2005 Wiley Periodicals, Inc.