Free-radical copolymerization of 4-nitrophenyl methacrylate (NPMA) with styrene (STY) was carried out at 65°C in 2-butanone by using benzoyl peroxide (BPO) as initiator. NPMA was characterized by spectral and microelemental analysis. Homoand copolymers were characterized by IR, 1 H-, and 13 C-NMR studies and their copolymer compositions were evaluated by 1 H-NMR spectroscopic technique. The copolymer reactivity ratios were calculated using Fineman-Ross, Kelen-Tü dos, and extended Kelen-Tudos methods. The Q,e values for NPMA were determined by Alfrey-Price Q,e rule. Thermal properties of the homo-and copolymers were studied by thermogravimetric analysis and differential scanning calorimetry methods.