煤焦油沥青中多环芳烃的柱层析分离及其GC-MS分析

Column chromatographic separation of polycyclic aromatic hydrocarbons in coal tar pitch and its GC /MS analysis

室温下用等体积的二硫化碳-丙酮混合溶剂对煤焦油沥青进行超声辐射萃取,煤焦油沥青中多环芳烃(PAHs)被混合溶剂萃取,用硅胶吸附萃取物,以石油醚为洗脱液洗脱硅胶,采用柱层析法对煤焦油沥青中多环芳烃进行了分离.在定量收取的洗脱液中分别析出了白色晶体、白色粉状物质和无色晶体(分别标记为M1,M2,M3),用气相色谱-质谱联用仪(GC/MS)分别对M1,M2,M3进行了分析.结果表明,M1中主要为3个环的多环芳烃和杂环化合物,M2中主要为4个环的多环芳烃和杂环化合物,M3中全部为4～5个环的多环芳烃.

Coal tar pitch was extracted with isometric carbon disulfide - acetone mixed solvent under ultrasonic radiation and room temperature. Polycyclic aromatic hydrocarbons （PAHs） in coal tar pitch were extracted by mixed solvent. The extracts were absorbed by silica gel. The silica gel was eluted with petroleum ether, PAHs in coal tar pitch were separated by using column chromatographic method. A white crystal, a white powder and a colorless crystal （marked as M1, M2, M3 respectively） appeared in three eluents, and M1 ,M2 and M3 were analyzed with GC -MS respectively. The results showed that M1 was mainly composed of 3 - ring PAHs and heterocyclic compounds, M2 was mainly composed of 4 - ring PAHs and heterocyclic compounds, and Ms was composed of 4 - ring or 5 - ring PAHs.