气相色谱法测定甘油氯化反应中产品及中间体含量

GC quantitative analysis of the product and intermediates of glycerol chlorination

使用气相色谱进行甘油制备环氧氯丙烷过程中产品以及中间体的定量分析。色谱柱为Dexsil-300填充柱,色谱分离在程序升温条件下进行。分别采用了面积归一化法、校正因子法与内标法对甘油、二氯丙醇以及一氯丙二醇进行了定量,并进行了比较。结果表明,使用Dexsil-300填充柱与毛细柱相比,分析时间短;内标法与其它两种方法相比,不受其它副产物影响,准确性高,重现性好。甘油、二氯丙醇及一氯丙二醇含量测定的相对标准偏差分别为1.06%,1.17%以及1.18%,回收率分别在98.70%～101.11%,98.17%～102.56%以及97.61%～102.88%之间,能够准确的反映反应进行的程度。

GC quantitative analysis of the product and intermediates of glycerol chlorination was studied.Packed column Dexsil-300 and temperature-programmed was used.The quantitative analysis were done through different methods of area normalization,correction factor and internal standard.Compared to the capillary column,packed column shortened the analysis time.Among the quantitative analysis methods,the internal standard method was the most accurate.It was not affected by the other by-product and with exact accuracy and repeatability.The RSD were 1.06%,1.17% and 1.18% and the recovery were 98.70%~101.11%,98.17%~102.56% and 97.61%~102.88%.The internal standard method can reflect the degree of the reaction.