This paper deals with the monitoring cyclo-addition of CO;to methyl methacrylate(MMA)-glycidyl methacrylate (GMA) copolymers using spectral(;H-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;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;fixation (>90%).The peak intensity changes in the;H-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.