草酸二甲酯与苯酚酯交换合成碳酸二苯酯反应产品的内标法测定  

Internal Standard Qualitative Analysis for the Products from Transesterification of Dimethyl Oxalate with Phenol

作　　者：王刚[1] 王胜平[1] 马新宾[1] 

机构地区：[1]天津大学化工学院绿色合成与转化教育部重点实验室,天津300072

出　　处：《分析化学》2006年第3期393-395,共3页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金资助项目(No.20276050);天津市科技攻关培育资助项目(No.033103511)

摘　　要：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

关 键 词：草酸二甲酯 草酸二苯酯 内标法 气相色谱分析 

分 类 号：TQ245.2[化学工程—有机化工]