碳酸二甲酯与苯酚酯交换法反应精馏合成碳酸二苯酯的定量分析

采用OV-101毛细管色谱柱分别对碳酸二甲酯与苯酚酯交换法反应精馏塔底产物和塔顶馏分进行了定量分析。以苯甲酸乙酯为内标物，一次性同时分析了塔釜产物中各组分含量。碳酸二甲酯、碳酸二苯酯和苯甲醚与内标物的峰面积比与各标准品的质量百分比浓度呈良好的线性关系，回归方程分别为Y=48．92X＋0．69、Y=32．82X-1．75和Y=13．17X＋0．07，相关系数分别为0．9976，0．9972和0．9978；以丙酮为内标，对塔顶馏分进行了定量分析。DMC的回归方程为Y=150．57X＋0．37，相关系数为0．9985；甲醇的回归方程为Y=71.20X-0.07，相关系数为0．9996。精密度实验表明，4次平行测定结果重复性良好，各待测物的相对标准偏差都小于2．00％；准确度结果表明，各待测物真实值与测定值的相对标准偏差在0．33％～1．50％之间，该法准确可靠。

The Quantitative Analysis of Reactive Distillation Products from Transesterification of Phenol with Dimethyl Carbonate

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 0.9978, 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%.