两种气相色谱固定相的研究  

Study on two kinds of GC stationary phase

作　　者：齐素华[1] 艾萍[2] 李方楼[2] 袁黎明[2] 张光毅[1] 

机构地区：[1]徐州医学院生物化学与分子生物学教研室,徐州221002 [2]云南师范大学化学化工学院,昆明650092

出　　处：《分析试验室》2006年第2期69-73,共5页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金资助项目(30160092);高等学校优秀青年教师教学科研奖励计划资助

摘　　要：使用硫杂冠醚、穴醚[2.2.2]作气相色谱固定相制备毛细管柱,考察两种固定相的使用比例、极性、热稳定性,并对甲苯-苯、乙苯-甲苯、甲基苯酚(o/p)、二氯苯(o/p,m)、硝基氯化苯(m,o)、苯-环己烷、庚醇-辛醇、苯胺-N,N二甲基苯胺等混合样品进行色谱分离。实验结果表明:两种固定相在OV-1701中的比例均为15%时有较好的分离效果,都属于中等极性的固定相。硫杂冠醚、穴醚[2.2.2]的平均极性分别为815、832,其中硫杂冠醚固定相的热稳定性较好,有较高的使用温度(185℃),而穴醚[2.2.2]的最高使用温度为120℃,因此穴醚[2.2.2]的使用温度受到一定的限制。从它们较好的分离性能看,固定相硫杂冠醚、穴醚[2.2.2]均具有较好的应用前景。1, 4, 7, 10, 13, 16-Hexathiacyclooctadecane and4, 7, 13, 16, 21, 24-Hexaoxa-1, 10-diazabicyclo [8. 8.8] hexacosane were used as Gas Chromatography （GC） stationary phases. Their proper concentrations, polarities, heat-durabilities and chromatographic properties were studied. They were mixed with OV-1701 to improve their filmformabilities. The concentration of OV-1701 is the same in two stationary phases, with the ratio of stationary phase to OV-1701 kept as 15 % consistently. The samples including halogenated hydrocarbons, aromatics, ketones, phenols, alcohols, and aniline derivatives were separated. The results are as foUowing： （1） The two stationary phases were medium polarities, the averages of 1,4, 7, 10, 13, 16-Hexathiacyclooctadecane and 4, 7, 13, 16, 21, 24-Hexaoxa- 1, 10-diazabicyclo [8.8.8]-hexacosane were 815 and 832, respectively. （2） The temperature for 1,4, 7, 10, 13, 16- Hexathiacycl-ooctadecane was limited under 185℃ while that of 4, 7, 13, 16, 21, 24-Hexaoxa-1, 10-diazabicyclo [8.8.8] hexacosane is 120℃. （3） They had fine chromatographic separation factors （a） to some compounds. For example, the a value of dichlombenzene （m, p） on 1, 4, 7, 10, 13, 16-Hexathiacyclooctadecane stationary phase was 1.27, which is bigger than 1.19 on OV-1701, and nitrochlombenzene （m, o） was better separated on 1,4, 7, 10, 13, 16-Hexathiacyclooctadecane （1.32） than on OV-1701 （1.09）. At 120℃, the separation factors （a values） of toluene/benzene, ethylbenzene/toluene and dimethylbenzene/toluene measured on the 4, 7, 13, 16, 21, 24- Hexaoxa-1, 10-diazabicyclo [ 8.8.8 ] hexacosane stationary phase were bigger than those obtained on OV-1701 respectively. Above data indicate that the two stationary phases have fine chromatographic properties and they are promising GC stationary phases.

关 键 词：硫杂冠醚 穴醚[2.2.2] 气相色谱 固定液 色谱性能 

分 类 号：O658.1[理学—分析化学]