The composition and structure of polyester materials were determinded by AV 500 NMR spectrometer.The sequence structure and its distribution of the polyester, the main part of the polyester materials which consist of mphthalic acid,pphthalic acid,sebacic acid,glycol,neopentylglycol,were also obtained using 2D NMR technique. The experiment showed that the composition of the mixture can be determined directly without separation.