With the increasing demand for novel process analytical technologies in recent years, Raman spectroscopy has been one of the powerful choices for in-situ reaction monitoring. In this paper, we discuss the use of in-situ Raman spectroscopy and the novel multivariate data analysis method, Band-Target Entropy Minimization (BTEM), to monitor the polymerization of methacrylamide using potassium persulfate (KPS) as the initiator. Kinetic studies were carried out varying the following conditions: initial monomer concentration, initial KPS concentration and polymerization temperature. In-situ Raman spectroscopy is employed to continuously measure the contents of the reaction mixture for a few hours. The collected reaction spectra are then subjected to BTEM to elucidate the pure component spectra, the concentration profiles of the components and the conversion of the monomer. The conversion data is then used together with optimization tools to obtain kinetic parameters for the polymerization.