Synthesizing Poly(N-Acrylolmorpholine) (PNAM) and Poly(N-Isopropylacrylamide) (PNIPA) copolymers using RAFT polymerization method. In the following, MALDI-TOF MS combined with MARA was used. Using MALDI-TOF MS, it provided a high-resolution view of the molecular composition and the structure of the synthesized copolymers, which make them possible to be characterized. At the end of the experiment, the molecular weights of the designed and the ones obtained after the analysis were compared, resulting in a strong positive correlation between both molecular weight values. Therefore, this strong positive correlation between the actual and theoretical data indicates the accuracy and precision of our synthesis and analytical techniques.