气相色谱法测定苯直接加氢烷基化产物组成

Determination of Main Products of Direct Hydroalkylation of Benzene by Gas Chromatography

建立了气相色谱法测定苯直接加氢烷基化反应产物的检测方法.色谱条件:AT.FFAP色谱柱(50 m×0.32 mm×0.50μm),氢火焰检测器,分流比为50∶1,进样器温度为180℃,检测器温度为200℃,柱温采用程序升温:初始温度80℃,恒温4 min后,以15℃/min的升温速率升至180℃,恒温8 min,进样量0.2μL.试验结果表明,甲基环戊烷、环己烷、环己烯、苯、环己基苯和二环己基苯可有效分离,检出限分别为1.4×10^(-7)、1.4×10^(-7)、1.4×10^(-7)、1.6×10^(-7)、2.7×10^(-7)和5.3×10^(-6) mg/L,检出限和定量限低,各物质线性关系良好,相关系数r均在0.996以上,各物质的相对标准偏差在0.62%~1.87%之间.方法操作简单,准确度高,可用于苯直接加氢烷基化反应产物的测定.

A gas chromatographic analysis method for the products from direct hydroalkylation of benzene has been established.The chromatographic conditions were as follows:AT.FFAP column(50 m×0.32 mm×0.50μm),hydrogen flame detector,split ratio:50∶1,injector temperature:180℃,detector temperature:200℃,column temperature programmed:initial temperature was kept at 80℃for 4 min,then heated to 180℃at 15℃/min and kept for 8 min.The injection volume was 0.2μL.Under these conditions,methyl cyclopentane,cyclohexane,cyclohexene,benzene,cyclohexylbenzene and dicyclohexylbenzene were effectively separated,and the detection limits were 1.4×10^(-7),1.4×10^(-7),1.4×10^(-7),1.6×10^(-7),2.7×10^(-7) and 5.3×10^(-6) mg/L,respectively,the limits of detection and quantification were low.The linear relationship of all substances was good.The correlation coefficient r was above 0.996.The method is simple and accurate,and can be used for the determination direct hydroalkylation of benzene of the reaction products.