Determination of Components in Fraction of C7~C9 of the Coal-Liquefied and Hydrogenated Oil by GC-MS in Combination with the Method of Live Database
摘 要
采用中心切割二维气相色谱,以PONA色谱柱为一维预分析柱与氢火焰离子检测器连接,以DB-35MS色谱柱为二维分析柱与MS连接,对煤直接液化加氢改质油中C7~C9馏分进行了分离与分析,并将质谱谱库检索和活数据库法相结合对60种组分进行了定性分析。同时采用标准物质和烃类化合物在PONA柱上的保留规律对上述定性结果作了验证。还采用面积归一化方法对油样中各化合物进行了定量分析和碳数分布以及族组成分析,其中C8及C9的化合物含量分别为32.3%和51.7%,主要族组成为环烷烃(77.3%)和正构烷烃(9.63%)。
Abstract
Components with C7-C9 in fractions of oil prepared by direct coal liquefaction and hydrogenation were separated and analyzed by the central-cutting 2D gas chromatography using the PONA chromatographic column as 1D priliminary analytical column with FID, and the DB-35MS column as 2D analytical column which is connected with MS; and combining with application of method of live database and searching of MS database, 60 compounds were identified. The results of the identification were further verified by the regularities of retention of hydrocarbons on the PONA column and by referring to standard materials. Quantification analysis of components with various carbon numbers and grouping of various hydrocarbons were carried out by the area normalization. It was shown that relative contents of compounds with C8 and C9 were found to be 32.3% and 51.7% respectively, and that the main groups of hydrocarbons found were cyclic hydrocarbons (77.3%) and alkanes with normal structures (9.63%).
中图分类号 O657.63
所属栏目 工作简报
基金项目 神华煤液化油元素分布及杂原子组分分析研究(SHJT-11-08)
收稿日期 2013/7/13
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备注李群花(1987-),女,河北邢台人,硕士研究生,主要从事煤直接液化油的单体烃组成研究。
引用该论文: LI Qun-hua,JIANG Yuan-bo,HU Hui-lian,WU Ting,DU Yi-ping,LI Ke-jian. Determination of Components in Fraction of C7~C9 of the Coal-Liquefied and Hydrogenated Oil by GC-MS in Combination with the Method of Live Database[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2014, 50(9): 1086~1091
李群花,姜元博,胡慧廉,吴婷,杜一平,李克健. 气相色谱-质谱结合活数据库法测定煤直接液化加氢改质油中C7~C9馏分的组成[J]. 理化检验-化学分册, 2014, 50(9): 1086~1091
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【2】MEUSINGER R. Qualitative and quantitative determination of oxygenates in gasoline using 1H nuclear magnetic resonance spectroscopy[J]. Analytical Chimica Acta,1999,391:277-288.
【3】DOBLE P, SANDERCOCK M, PASQUIER E D. Classification of premium and regular gasoline by gas chromatography/mass spectrometry, principal component analysis and artificial neural networks[J]. Forensic Science International, 2003,132:26-39.
【4】HAMILTON J F, LEWIS A C. Monoaromatic complexity in urban air and gasoline assessed using comprehensive GC and fast GC-TOF/MS[J]. Atmospheric Environment, 2003,37:589-602.
【5】CHENG Xing-xiao, HUANG Lu-ning, FU Xing-guo. Investigation of the components in RFCC gasoline affecting the accuracy of potentiometric titration by GC-MS and GC-IR[J]. Fuel Processing Technology, 2004,85:379-390.
【6】关亚风,李灵娥,周良模.毛细管气相色谱活数据库定性[J].色谱, 1995,13(5):351-357.
【7】GUAN Ya-feng, KIRALY J, RIJKS J A. Interactive retention index database for compound identification in temperature-programmed capillary gas chromatography[J]. Journal of Chromatography, 1989,472:129-143.
【8】GUAN Ya-feng, ZHOU Liang-mo. Live retention database for identification in multi-step temperature-programmed capillary gas chromatography[J]. Journal of Chromatography, 1991,552:187-195.
【9】GUAN Ya-feng, ZHU Dao-qian, ZHOU Liang-mo, et al. Design and use of a thermal conductivity detector at pressure for temperature-programmed capillary gas chromatography[J]. Journal of Chromatography, 1993,655:243-247.
【10】李灵娥,关亚风,周良模.20种农药的标准Kovats指数及其在程序升温下的活数据库定性[J].分析化学, 1995,23(1):14-19.
【11】王华,刘文民,徐媛,等.色谱与色谱/质谱法相结合分析热裂解汽油C9馏分[J].色谱, 2006,24(6):615-618.
【12】薛慧峰,赵家林,刘满仓,等.用气相色谱-质谱和气相色谱-红外联用技术分析热裂解汽油C9馏分中的组成[J].分析化学, 2004,32(9):1145-1150.
【13】常薇,李旭祥.乙烯副产C9馏分的GC/MS分析[J].纺织高校基础科学学报, 2004,17(1):49-51.
【14】李长秀,刘颖荣,杨海鹰,等.气相色谱法测定汽油烃类组成分析技术的应用现状与发展[J].色谱, 2004,22(5):521-527.
【15】杜国华,杨海鹰,顾洁,等.PLS方法辅助TLC/FID技术测定石油沥青的族组成[J].理化检验-化学分册, 2004,40(12):715-717.
【16】毕延根,卢艳.薄层色谱-氢火焰离子检测分析重质油的族组成[J].理化检验-化学分册, 2003,39(5):280-282.
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