A description of a systematic NMR methodology for the characterization
of polymers in solution is presented. The method utilizes a set of tw
o dimensional (2D) heteronuclear NMR correlation experiments. It is es
pecially optimized for polymers that have characteristic short spin-sp
in relaxation times. Microstructures of homopolymers and copolymers ar
e determined objectively since the analysis is based only on near neig
hbor correlations of all carbon and hydrogen atoms. Applications to po
ly(acrylic acid) and ethylene/vinyl acetate copolymer are presented.