In my diploma work, I synthesized poly(N-acryloylmorpholine), poly(diacetoneacrylamide) homopolymers and NAM/DAAM random copolymers applying RAFT, in other words, polymerization of reversible addition-fragmentation chain transfer technique. Methods were adopted and modified to synthesize well defined polymers in a diverse array of chemical composition and molecular mass. The structure of produced polymers was determined by MALDI-TOF MS. Distinct factors like concentration of monomers, chain transfer agent, initiator for polymerization were investigated to optimize a synthetic method. Using the collecting data of PNAM, PDAAM homopolymers and NAM/DAAM random copolymer sample peaks, I calculated Mw(weight average molecular weight), Mn(number average molecular weight) as well as PDI(polydispersity index) of them. I calculated the homopolymers' polymerization degree for exact peaks from PNAM and PDAAM samples. MR1 and m/z ratio data confirmed the chemical composition of NAM/DAAM random copolymers using IsotopePattern.