The solubility of poly(phenyl glycidyl ether) s (PPGEs) depends on the stereoregularity．Different solvents and temperatures (CDCl3／300 K or TCE-d2／350 K) were used in 13C-NMR characterization of these polymers. It was necessary to investigate first the effect of temperature on the 13C—NMR spectra of PPGEs．It was found that all the 13C-NMR signals of PPGE were shifted to the lower magnetic field with the increase of the temperature．The temperature sensitivity of the 13C-NMR chemical shifts for different carbon atoms was different．The pendent CH2 group was most sensitive to the temperature．The change of the 13C-NMR chemical shift for the pendent CH2 group was mainly caused by the temperature change

and the effects of the solvent kind and the stereoregularity of the polymer were of minor importance．The change of temperature did not make any significant influence on the result of the stereoregularity calculation according to the 13C-NMR spectra for PPGEs．Utilizing the different temperature-sensitivity of 13C-NMR signals for different groups

it is possible to separate the overlapped signals by choosing an appropriate temperature．This method was found especially useful in the 13C-NMR characterization of complex polymer samples．