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%。
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-5 MS 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).
作者
赵佳佳
李群花
欧阳福生
姜元博
高山松
ZHAO Jiajia;LI Qunhua;OUYANG Fusheng;JIANG Yuanbo;GAO Shansong(Research Center of Petroleum Processing,East China University of Science and Technology,Shanghai 200237,China;DCL National Engineering Lab,China Shenhua Coal to Liquid and Chemical Shanghai Research Institute,Shanghai 201108,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2019年第2期178-186,共9页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
