A gas chromatographic method, with an OV-101 capillary column, was established for analyzing the products and the distillates from the transesterificatin of dimethyl carbonate ( DMC) with phenol quantitatively. The products were analyzed simultaneously using ethyl benzoate ( EB) as internal standard. A good linear relationship of the mass percent of DMC, diphenyl carbonate ( DPC) and anisole versus the peak area ratio of DMC to EB, DPC to EB as well as anisole to EB was observed. The regression equation of DMC DPC and anisole were Y = 48. 92X + 0. 69, Y = 32. 82X - 1. 75, and Y = 13. 17X + 0. 07 with the correlation coefficient of 0. 9976, 0. 9972 and 0. 997 8, respectively. The distillates of DMC and methanol were quantified using acetone as the internal standard. The linear regression equations of DMC and methanol were Y = 150. 57X + 0. 37 and Y = 71. 20X - 0. 07 with the correlation coefficient of 0. 9985 and 0. 9996 respectively. The precision experiments showed that the relative standard deviations of the analytes were less than 2. 0% ( n = 4). According to the results of the accuracy experiments,, the internal standard method was exact with the relative standard deviation of the analytes ranging from 0. 3% to 1. 5%.