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气相色谱法测定苯直接加氢烷基化产物组成
引用本文:陈世萍,景孝廉,林丽芹,陈乐俊,朱琳熙,王星竹.气相色谱法测定苯直接加氢烷基化产物组成[J].分析测试技术与仪器,2021,27(4):292-296.
作者姓名:陈世萍  景孝廉  林丽芹  陈乐俊  朱琳熙  王星竹
作者单位:泉州师范学院 化工与材料学院,福建 泉州 362000
基金项目:泉州市科技项目2019C060R福建省自然科学基金2021J01964
摘    要: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×0.50 μm), 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0.2 μL. 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.

关 键 词:  环己烷  环己烯  甲基环戊烷  环己基苯  气相色谱
收稿时间:2021-10-11

Determination of Main Products of Direct Hydroalkylation of Benzene by Gas Chromatography
Affiliation:Collage of Chemical Engineering and Material Science Quanzhou Normal University, Quanzhou 362000, Fujian China
Abstract: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×0.50 μm), 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 0.2 μL. 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.
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