建立了尿素醇解合成碳酸二乙酯反应的终产物碳酸二乙酯和中间产物氨基甲酸乙酯的气相色谱分析方法。采用SE-54色谱柱基线分离了碳酸二乙酯、氨基甲酸乙酯及其相关化合物,外标法定量测定了碳酸二乙酯和氨基甲酸乙酯,其相关系数分别为0.995 3和0.997 7;回收率分别为96.0%~104.0%和95.0%~102.5%。精密度实验表明,方法的标准偏差RSD分别为2.83%和2.95%,5次平行测定结果重复性良好。分析和计算结果准确可靠,这种分析方法可以作为催化剂筛选、反应条件考察的基准。
An accurate and reliable gas chromatographic method for analyzing diethyl carbonates(DEC) and ethyl carbonates(EC) is described.DEC and EC,as well as ethanol were well separated through a SE-54 chromatographic column.A good linear relationship of the concentration versus peak area was observed with the correlation coefficients of 0.995 3 and 0.997 7,respectively.The RSD,recovery for determining DEC were found to be 2.83 %,96.0 %~104.0 %,respectively,and that for EC 2.95 %,95.0 %~102.5 %,respectively.These results show pretty high accuracy,recovery and a high precision.