全二维气相色谱-氢火焰离子化检测器定性定量分析柴油中的多环芳烃  

Qualitative and Quantitative Analysis of Polycyclic Aromatic Hydrocarbons in Diesel Oil by Comprehensive Two-Dimensional Gas Chromatography Combined with Hydrogen Flame Ionization Detector

作　　者：代静 李红俊 赵双宏 胡修德 叶农 DAI Jing;LI Hongjun;ZHAO Shuanghong;HU Xiude;YE Nong(l.Ningria Academy of Metrology&Quality Inspection(National Measurement and Testing Center for Coal Chemical Industry),Yinchuan 75041l,China;NingriaUniversity,Yinchuan 750021,China)

机构地区：[1]宁夏计量质量检验检测研究院(国家煤化工产业计量测试中心),银川750411 [2]宁夏大学,银川750021

出　　处：《理化检验（化学分册）》2023年第10期1180-1186,共7页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家标准化管理委员会标准化项目(20160284-T-159);国家市场监督管理总局科技计划项目(2019MK076);宁夏青年人才托举工程项目(TJGC2018047);宁夏大学省部共建煤炭高效利用与绿色化工国家重点实验室开放课题(2019-KF-35)。

摘　　要：提出了全二维气相色谱-氢火焰离子化检测器(GC×GC-FID)定性定量分析柴油中多环芳烃的方法。利用全二维气相色谱-飞行时间质谱法(GC×GC-TOF MS)确定柴油芳烃的4个族组成,分别为非芳烃、一环芳烃、二环芳烃和三环+芳烃,获得37种定性化合物;采用峰面积归一化法对多环芳烃进行定量。结果表明:柴油质控样中多环芳烃测定值的相对误差绝对值不大于5.0%;对柴油样品进行回收试验,回收率为95.7%~104%,测定值的相对标准偏差(n=6)为1.7%~4.3%。方法用于7种实际柴油样品分析,并与NB/SH/T 0806-2022进行比对,结果显示两种方法测定值的相对误差绝对值均不大于5.0%。A method for the qualitative and quantitative analysis of polycyclic aromatic hydrocarbons in diesel oil by comprehensive two-dimensional gas chromatography combined with hydrogen flame ionization detector(GCX GC-FID)was proposed.Four group-types of aromatic hydrocarbons in diesel oil were determined by comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry(GC X GC-TOF MS),which were nonaromatic hydrocarbons,monocyclic aromatic hydrocarbons,bicyclic aromatic hydrocarbons and tricyclic+aromatic hydrocarbons,and 37 qualitative compounds were obtained,in which polycyclic aromatic hydrocarbons were quantified by peak area normalization method.It was shown that the absolute value of relative error of polycyclic aromatic hydrocarbons in the diesel oil quality control sample was not greater than 5.0%.Test for recovery was made on diesel oil sample by standard addition method,giving results in the range of 95.7%-104%,and RSDs(n=6)of the determined values ranged from 1.7%to 4.3%.The method was applied to analyze 7 real diesel oil samples and compared with NB/SH/T 0806-2022,it was shown that the absolute values of relative errors of the determined values obtained by two methods were less than 5.0%.

关 键 词：全二维气相色谱 氢火焰离子化检测器 柴油 多环芳烃 定性定量 

分 类 号：O657.7[理学—分析化学]