Random copolymerization have been performed for three binary systems using 1-methoxy-2-methyl-1-trimethylsilyloxy propene(initiator) and tetrabutylammonium bibenzoate(catalyst) in tetrahydrofuran solution. The copolymer compositions were determined by elementary analysis for nitrogen and the results evaluated by the Kelen-Tudos method, The monomer pairs concerned are (1) acrylonitrile(AN) and methyl methacrylate(MMA), (2) AN and ethyl methacrylate(EMA), (3) AN and butyl methacrylate(BMA), The reactivity ratios determined in this study are: (1) r(AN)=10.22, r(MMA)=0.07; (2)r(AN)= 5.68, r(EMA)=0.16; (3) r(AN)=8.59, r(BMA)=0.09