气相色谱法测定车用汽油中含氧化合物和苯胺类化合物

发布时间：2018-03-05 11:09

本文选题：气相色谱　切入点：中心切割　出处：《色谱》2017年05期 　论文类型：期刊论文

【摘要】：利用中心切割技术和双毛细管色谱柱系统,采用两次进样的方式,建立了气相色谱测定车用汽油中含氧化合物和苯胺类化合物的分析方法。第一次进样分析,组分首先进入非极性DB-1色谱柱(30 m×0.32 mm×1.0μm),按沸点由低到高的顺序分离,通过电磁阀切换将沸点小于2-己酮的组分切割至强极性GS-OxyPLOT色谱柱(10 m×0.53 mm×10μm)或CP-Lowox色谱柱(10 m×0.53 mm×10μm),其余重烃组分通过阻尼柱进入FID检测器。在GS-OxyPLOT或CP-Lowox色谱柱上,烃类组分与含氧化合物分离并进入检测器检测,消除了大量的烃类组分对含氧化合物测定的影响。第二次进样分析,设定电磁阀切换时间为间-甲基苯胺从非极性色谱柱流出的时间,苯胺类化合物在GS-OxyPLOT或CP-Lowox色谱柱上与烃类和含氧化合物分离并进入检测器检测。以乙二醇二甲基醚为内标化合物进行内标法定量。实现了在一套系统上同时测定车用汽油中添加的甲基叔丁基醚(MTBE)、甲醇、甲缩醛、乙酸仲丁酯、乙酸乙酯、苯胺、邻/间/对-甲基苯胺和N-甲基苯胺的含量,各组分的检测范围为0.01%~10%(质量分数),回收率为86.0%~102.6%。该法可以为车用汽油的质量控制提供有效的检测手段。
[Abstract]:A method for the determination of oxygenated compounds and aniline compounds in gasoline by gas chromatography was established by means of central cutting technique and double capillary column system. The components first entered the nonpolar DB-1 column (30 m 脳 0.32 mm 脳 1.0 渭 m) and separated in the order of boiling point from low to high. The components with boiling point less than 2-hexanone were cut to a strong polar GS-OxyPLOT column (10 m 脳 0.53 mm 脳 10 渭 m) or CP-Lowox column (10 m 脳 0.53 mm 脳 10 渭 m) by solenoid valve. The rest of the heavy hydrocarbon components entered the FID detector by damping column. The separation of hydrocarbon components from oxygenated compounds and their entry into the detector eliminates the influence of a large number of hydrocarbon components on the determination of oxygenated compounds. Setting the switching time of the solenoid valve for the outflow of m-methylaniline from the non-polar column, Aniline compounds were separated from hydrocarbons and oxygenated compounds on GS-OxyPLOT or CP-Lowox column and detected by detector. The internal standard quantity was determined by using ethylene glycol dimethyl ether as internal standard compound. Methyl tert-#china_person0# ether (MTBEBEN) and methanol were added to gasoline. Contents of methylal, secondary butyl acetate, ethyl acetate, aniline, o-m-p-methylaniline and N-methylaniline, The detection range of each component is 0. 01% and 10%. The recovery rate is 86. 0% and 10. 6%. This method can provide an effective method for the quality control of automobile gasoline.
【作者单位】：中国石油化工股份有限公司石油化工科学研究院;
【基金】：国家标准化管理委员会标准化项目(20131688-T-469)~~
【分类号】：O657.71;TE626.21

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