Qualitative and Quantitative Analysis of Polycyclic Aromatic Hydrocarbons in Diesel Oil by Comprehensive Two- Dimensional Gas Chromatography Combined with Hydrogen Flame Ionization Detector
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%。
Abstract
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 (GC×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×GC-TOF MS), which were non-aromatic 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%.
中图分类号 O657.7 DOI 10.11973/lhjy-hx202310012
所属栏目 工作简报
基金项目 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)
收稿日期 2022/5/28
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备注代静,工程师,硕士,主要从事煤化工产品检验检测、新方法研究等相关工作
引用该论文: DAI Jing,LI Hongjun,ZHAO Shuanghong,HU Xiude,YE Nong. Qualitative and Quantitative Analysis of Polycyclic Aromatic Hydrocarbons in Diesel Oil by Comprehensive Two- Dimensional Gas Chromatography Combined with Hydrogen Flame Ionization Detector[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2023, 59(10): 1180~1186
代静,李红俊,赵双宏,胡修德,叶农. 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[J]. 理化检验-化学分册, 2023, 59(10): 1180~1186
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【8】张祎玮,祝馨怡,刘泽龙,等.液相色谱及质谱法测定柴油芳烃适用性研究[J].石油炼制与化工, 2018,49(6):87-92.
【9】JENNERWEIN M K, ESCHNER M, GRÖGER T, et al. Complete group-type quantification of petroleum middle distillates based on comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC×GC-TOFMS) and visual basic scripting[J]. Energy & Fuels, 2014,28(9):5670-5681.
【10】BERRIER K L, FREYE C E, BILLINGSLEY M C, et al. Predictive modeling of aerospace fuel properties using comprehensive two-dimensional gas chromato-graphy with time-of-flight mass spectrometry and partial least squares analysis[J]. Energy & Fuels, 2020,34(4):4084-4094.
【11】花瑞香,阮春海,王京华,等.全二维气相色谱法用于不同石油馏分的族组成分布研究[J].化学学报, 2002,60(12):2185-2191.
【12】阮春海,叶芬,孔宏伟,等.石油样品全二维气相色谱分析的分离特性[J].分析化学, 2002,30(5):548-551.
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