GC-MS Determination of 55 Aromatics in Hydrogen-Donor Solvent for Direct Coal Liquefaction
摘 要
煤直接液化供氢溶剂样品经固相萃取和不同溶剂洗脱而分离为饱和烃、芳烃和胶质等3种组分。将所得芳烃组分进行气相色谱分离,由于所用色谱柱为弱极性毛细管色谱柱,得到了按沸点从低到高的规律出峰的55种芳烃的总离子流色谱图。在此基础上,经NIST谱库检索与标准谱库对比,运用ASPEN PLUS中数据库进行沸点检索,并结合保留指数文献对比,最终识别了这55种芳烃并计算其在HP-5MS色谱柱上的保留指数。采用高分辨气相色谱-质谱联用仪对各化合物的结构式和相对分子质量进行测定。用面积归一化法进行定量,确定了此55种芳烃的相对含量,芳烃碳数分布主要集中在C10~C16,占已测定芳烃总量的92.20%;芳烃类型主要为环烷苯类,占46.87%,其次为二环烷苯类和苊类,分别占19.13%,10.67%。
Abstract
The sample of hydrogen-donor solvent for direct coal liquefaction was treated by SPE and eluted with different eluants to separate the components into 3 parts, i.e. alkanes, aromatics and glue. Through GC separation for the aromatics on weakly polar capillary chromatographic column, a TIC chromatogram of 55 aromatics was obtained with their peaks appeared in the order of their boiling points from lower values to higher values. On the base of the GC data, searchings were made successively into NIST spectra data base, the data base of standard spectra, and the data base of boiling points in ASPEN PLUS, and with the reference to researches on the retention indexes. Finally, the 55 compounds were recognized clearly, with their retention indexes on the HP-5MS chromatographic column calculated. Structural formula and values of relative molecular mass of these compounds were determined by the hyphenation of high resolution GC and MS. Quantification of the 55 compounds was performed by normalization of areas, and their relative contents were found. Carbon numbers of these aromatics were mainly in the range of C10 to C16, attaining to 92.20% of the total of the aromatics. These aromatics were mainly dropping into the category of cycloalkylbenzenes (46.87%), and secondly into the categories of dicycloalkylbenzenes and acenaphthenes (19.13% and 10.67% respectively).
中图分类号 O657.63 DOI 10.11973/lhjy-hx201902010
所属栏目 工作简报
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收稿日期 2018/4/24
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备注赵佳佳,硕士研究生,主要从事煤直接液化供氢溶剂组成的研究工作
引用该论文: ZHAO Jiajia,LI Qunhua,OUYANG Fusheng,JIANG Yuanbo,GAO Shansong. GC-MS Determination of 55 Aromatics in Hydrogen-Donor Solvent for Direct Coal Liquefaction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2019, 55(2): 178~186
赵佳佳,李群花,欧阳福生,姜元博,高山松. 气相色谱-质谱法测定煤直接液化供氢溶剂中55种芳烃[J]. 理化检验-化学分册, 2019, 55(2): 178~186
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【4】刘文,张小军.质谱法测定柴油中多环芳烃[J].广州化工, 2015,43(4):139-141.
【5】刘泽龙,李云龙,高红,等.四极杆GC/MS测定石油馏分烃类组成的研究及其分析软件的开发[J].石油炼制与化工, 2001,32(3):44-48.
【6】李群花,姜元博,胡慧廉,等.气相色谱-质谱结合活数据库法测定煤直接液化加氢改制油中C7~C9馏分的组成[J].理化检验-化学分册, 2014,50(9):1086-1090.
【7】PASADAKIS N, VAROTSIS N. A novel approach for the quantitation of the hydrocarbon groups in heavy petroleum fractions by HPLC-RI analysis[J]. Energy & Fuels, 2000,14(6):1184-1187.
【8】MEUSINGER R. Qualitative and quantitative determination of oxygenates in gasoline using 1H nuclear magnetic resonance spectroscopy[J]. Analytica Chimica Acta, 1999,391:277-288.
【9】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, 2003,37:589-603.
【10】白金锋.煤加氢液化制芳烃化合物的研究[D].大连理工大学:大连, 2000.
【11】朱继升,NORCIO LAWRENCE P, KUGLER EDWIN L,等.两种烟煤的液化及液化油的组成特征研究[J].燃料化学学报, 2001,29(3):214-218.
【12】樊文俊,吴美香,郝建树,等.紫外光谱法分析煤直接液化油族组成[J].光谱学与光谱分析, 2015,35(7):1938-1943.
【13】宫万福,田松柏,付晓恒.分析技术在煤液化油分析中的应用[J].洁净煤技术, 2004,10(2):47-52.
【14】蔺华林,张德祥,彭俊,等.神华煤直接液化循环油的分析表征[J].燃料化学学报, 2007,35(1):104-108.
【15】戚一文,方云进.物性估算在ASPEN PLUS软件中的应用[J].浙江化工, 2007,38(1):9-11.
【16】WHITE C M, HACKETT J, ANDERSON R R, et al. Linear temperature programmed retention indices of gasoline range hydrocarbons and chlorinated hydrocarbons on cross-linked polydimethylsiloxane[J]. Journal of High Resolution Chromatography, 1992,15(2):105-120.
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