采用SP-3420型氢离子火焰气相色谱仪、HP-5型毛细管色谱柱,以苯甲酸乙酯为内标物,对草酸二甲酯与苯酚酯交换反应的产物草酸二苯酯进行定量分析.通过绘制内标法标准曲线,确定了标准方程为y=1.6366x+0.0319,相关系数为0.997.准确度和回收率实验表明,该方法的测定值与实际值的相对标准偏差在1%到4%之间;回收率在98%~102%.精密度实验表明,5次平行测定结果重复性良好,相对标准偏差为0.28%.分析和计算结果准确可靠,可以作为催化剂筛选、反应条件考察的基准.
An accurate and reliable method for the analysis of products from the transesterification of dimethyl oxalate (DMO) with phenol was developed with SP-3420 flame ionization detection (FID) gas chromatogram and HP-5 chromatogram column. Ethyl benzoate was chosen as internal standard material. Gas chromatogram conditions, injection temperature and detector temperature were 250℃, and column temperature was under programmed temperature from 60℃ to 200℃ by 10℃/min with a hold time of 1 minute. By the curve of interhal standard, the expression was established, y = 1. 6366x +0.0319, r =0. 997. Thus the mass concentration of diphenyl oxalate (DPO) was able to be calculated, which was a primary data for conversion, yield and selectivity of the transesterification reaction. The method was estimated by accuracy, recovery and precision. The relative deviations between real values and measured values were from 1% to 4%, and recoveries were from 98% to 102%, which shows pretty high accuracy and recovery. The relative standard deviation among five parallel injections was 0.3%, which shows a high precision