This paper deals with the monitoring cyclo-addition of CO_2 to methyl methacrylate(MMA)-glycidyl methacrylate (GMA) copolymers using spectral(~1H-NMR and FTIR) and chemical(elemental analysis and titration) methods.Thus, poly(MMA-co-GMA),was first prepared via solution polymerization.The copolymer was then treated with CO_2 gas flow in the presence of cetyltrimethyl ammoniumbromide as a catalyst.In terms of the carbonation reaction time,the terpolymer poly(MMA-co-GMA-co-2-oxo-l,3-dioxolane-4-yl-methyl methacrylate) was prepared in various yield of CO_2 fixation (>90%).The peak intensity changes in the ~1H-NMR and FTIR spectra provided excellent demonstrative techniques to monitor the carbonation reaction progression.In a comparative analytical viewpoint,the NMR and elemental analysis were recognized to be the most accurate ways to follow the cyclo-addition reaction progression.However,titration was recognized to be the most preferred method,because it is a very inexpensive,facile and available method with a reasonable costaccuracy balance. This paper deals with the monitoring of cyclo-addition of CO_2 to methyl methacrylate (MMA) -glycidyl methacrylate (GMA) copolymers using spectral (~ 1H-NMR and FTIR) and chemical (elemental analysis and titration) methods.Thus, poly (MMA- co-GMA), was first prepared via solution polymerization. The copolymer was then treated with CO 2 gas flow in the presence of cetyltrimethyl ammoniumbromide as a catalyst. In terms of the carbonation reaction time, the terpolymer poly (MMA-co-GMA-co 2-oxo-l, 3-dioxolane-4-yl-methyl methacrylate was prepared in various yield of CO 2 fixation (> 90%). The peak intensity changes in the ~ 1H-NMR and FTIR spectra provided excellent demonstrative techniques to monitor the carbonation reaction. In a comparative analytical viewpoint, the NMR and elemental analysis were recognized to be the most accurate ways to follow the cyclo-addition reaction progression. However, titration was recognized to be the most preferred method, because it is a very inexpensive, facile and a vailable method with a reasonable costaccuracy balance