两种多苯基苯基接枝聚硅氧烷气相色谱固定相的合成及色谱性能研究
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摘要
本文研究了两类新型稠环芳烃接枝聚硅氧烷固定相的合成,并系统评价了它们的色谱性能、应用于实际样品的分离。
合成新型固定相：首先合成了四苯基环戊二烯酮和2-甲基-3,4-二苯基环戊二烯酮,又采用开环聚合的方法合成了乙烯基含量分别为10%、20%和30%的甲基乙烯基硅生胶,最后通过高温下的Diels-Alder反应,将上述两类环戊二烯酮单体接枝到聚硅氧烷侧链上,得到四苯基苯基接枝聚硅氧烷和2-甲基-3,4-二苯基苯基接枝聚硅氧烷。在反应中控制投料比例,使乙烯基有少量剩余,以利于制备交联毛细管柱,提高色谱柱耐温性。另外,通过四苯基环戊二烯酮和四甲基二乙烯基二硅氧烷的D-A反应得到1-四苯基苯基-3-乙烯基-1,1,3,3-四甲基-二硅氧烷,又合成含氢量不同的含氢硅油,最后通过硅氢加成反应得到主链与接枝基团之间带有间隔基的四苯基苯基接枝聚硅氧烷,也可作为毛细管气相色谱固定相。
色谱柱的评价：采用静态法将四苯基苯基接枝聚硅氧烷和2-甲基-3,4-二苯基苯基接枝聚硅氧烷固定相涂渍到毛细管柱内,发现两类固定相均易于涂渍、涂渍效率高。系统评价了其色谱性能,并与商业柱OV-17(50%苯基聚硅氧烷固定相色谱柱)作了对比。涂渍新型固定相的色谱柱柱效高,当接枝量为20%时属于中等极性色谱柱,接枝量为30%时,极性接近于OV-17,对Grob分离良好,对各类物质均能进行分离分析,柱重现性好,温度使用范围宽,为60-360℃。
将上述色谱柱用于苯类取代物、稠环芳烃等实际样品的分离,实验证明,四苯基苯基接枝聚硅氧烷和2-甲基-3,4-二苯基苯基接枝聚硅氧烷为两类具有优异选择性的气相色谱固定相,由于侧链芳香环高度集中,在色谱分离中与溶质可产生较强的诱导作用和色散力作用,适用于分析各类非极性及极性溶质,在进行多环芳烃等环境污染物的分析中能够得到广泛的应用。
In this paper, two new grafted polysiloxane GC stationary phase were synthesized. Evaluation of their chromatographic properties and separation applied to real samples were tested.
Synthesis of new stationary phase:firstly,2,3,4,5-tetraphenylcyclopenta-2,4-dienone and 2-methyl-3,4-diphenylcyclopenta-2,4-dienone were synthesized, then the methyl-vinyl-silicone rubber with different content of vinyl(10%、20%、30%) were prepared, at last, methyl-vinyl-silicone rubber with different content of vinyl were reacted with 2,3,4,5-tetraphenylcyclopenta-2,4-dienone and 2-methyl-3,4-diphenylcyclopenta-2,4-dienone through Diels-Alder reaction. It can obtain tetraphenyl phenyl polysiloxane and 2-methyl-3,4-diphenyl phenyl polysiloxane through the above experiment. By ways of control the feed ratio, make a small amount of residual vinyl, the stationary phase can be used of cross-linked capillary column to improve the temperature resistance.1-tetraphenyl-phenyl-3-viny-1-1,1,3,3-tetramethyl disiloxane was obtained through Diels-Alder reaction between 2,3,4,5-tetraphenylcyclopenta-2,4-dienone and tetramethyl divinyl disiloxane, then the dimethylpolysiloxane conataining 10%～30% Si-H groups was synthesized, lastely, silicon hydrogen addition reaction can take place in the above two reactants and obtain tetraphenyl phenyl graft polysiloxane with interval which can also be used as the GC stationaty phase.
The evaluation of the new stationary phase:. The two new stationary phases were easily coated on the capillary columns in the static coating method. The performance of the columns were evaluated and compared with OV-17(50% phenyl-dimethyl-polysiloxane). The high column efficiency was shown in the columns coated with the new stationary phases. When the graft group was 20%, the column showed medium polarity and the polarity was silimar with OV-17, when the content was 30%, The separatioan of Grob test mixture was very well in the columns and showed good reproducibility. The new stationry phase had a wide temperature range, about 60～360℃.
The new columns were used in actual sample separation like benzene and polycyclic aromatic compounds, the separation of replaced can be separated better than OV-17 in the new columns. Because of the induction and dispersion forces from the grafted group, excellent chromatographic performance was shown in the two new stationary phases.. It is suitable for tetraphenyl phenyl polysiloxane and 2-methyl-3,4-diphenyl phenyl polysiloxane to be used as GC stationary phase.
合成新型固定相：首先合成了四苯基环戊二烯酮和2-甲基-3,4-二苯基环戊二烯酮,又采用开环聚合的方法合成了乙烯基含量分别为10%、20%和30%的甲基乙烯基硅生胶,最后通过高温下的Diels-Alder反应,将上述两类环戊二烯酮单体接枝到聚硅氧烷侧链上,得到四苯基苯基接枝聚硅氧烷和2-甲基-3,4-二苯基苯基接枝聚硅氧烷。在反应中控制投料比例,使乙烯基有少量剩余,以利于制备交联毛细管柱,提高色谱柱耐温性。另外,通过四苯基环戊二烯酮和四甲基二乙烯基二硅氧烷的D-A反应得到1-四苯基苯基-3-乙烯基-1,1,3,3-四甲基-二硅氧烷,又合成含氢量不同的含氢硅油,最后通过硅氢加成反应得到主链与接枝基团之间带有间隔基的四苯基苯基接枝聚硅氧烷,也可作为毛细管气相色谱固定相。
色谱柱的评价：采用静态法将四苯基苯基接枝聚硅氧烷和2-甲基-3,4-二苯基苯基接枝聚硅氧烷固定相涂渍到毛细管柱内,发现两类固定相均易于涂渍、涂渍效率高。系统评价了其色谱性能,并与商业柱OV-17(50%苯基聚硅氧烷固定相色谱柱)作了对比。涂渍新型固定相的色谱柱柱效高,当接枝量为20%时属于中等极性色谱柱,接枝量为30%时,极性接近于OV-17,对Grob分离良好,对各类物质均能进行分离分析,柱重现性好,温度使用范围宽,为60-360℃。
将上述色谱柱用于苯类取代物、稠环芳烃等实际样品的分离,实验证明,四苯基苯基接枝聚硅氧烷和2-甲基-3,4-二苯基苯基接枝聚硅氧烷为两类具有优异选择性的气相色谱固定相,由于侧链芳香环高度集中,在色谱分离中与溶质可产生较强的诱导作用和色散力作用,适用于分析各类非极性及极性溶质,在进行多环芳烃等环境污染物的分析中能够得到广泛的应用。
In this paper, two new grafted polysiloxane GC stationary phase were synthesized. Evaluation of their chromatographic properties and separation applied to real samples were tested.
Synthesis of new stationary phase:firstly,2,3,4,5-tetraphenylcyclopenta-2,4-dienone and 2-methyl-3,4-diphenylcyclopenta-2,4-dienone were synthesized, then the methyl-vinyl-silicone rubber with different content of vinyl(10%、20%、30%) were prepared, at last, methyl-vinyl-silicone rubber with different content of vinyl were reacted with 2,3,4,5-tetraphenylcyclopenta-2,4-dienone and 2-methyl-3,4-diphenylcyclopenta-2,4-dienone through Diels-Alder reaction. It can obtain tetraphenyl phenyl polysiloxane and 2-methyl-3,4-diphenyl phenyl polysiloxane through the above experiment. By ways of control the feed ratio, make a small amount of residual vinyl, the stationary phase can be used of cross-linked capillary column to improve the temperature resistance.1-tetraphenyl-phenyl-3-viny-1-1,1,3,3-tetramethyl disiloxane was obtained through Diels-Alder reaction between 2,3,4,5-tetraphenylcyclopenta-2,4-dienone and tetramethyl divinyl disiloxane, then the dimethylpolysiloxane conataining 10%～30% Si-H groups was synthesized, lastely, silicon hydrogen addition reaction can take place in the above two reactants and obtain tetraphenyl phenyl graft polysiloxane with interval which can also be used as the GC stationaty phase.
The evaluation of the new stationary phase:. The two new stationary phases were easily coated on the capillary columns in the static coating method. The performance of the columns were evaluated and compared with OV-17(50% phenyl-dimethyl-polysiloxane). The high column efficiency was shown in the columns coated with the new stationary phases. When the graft group was 20%, the column showed medium polarity and the polarity was silimar with OV-17, when the content was 30%, The separatioan of Grob test mixture was very well in the columns and showed good reproducibility. The new stationry phase had a wide temperature range, about 60～360℃.
The new columns were used in actual sample separation like benzene and polycyclic aromatic compounds, the separation of replaced can be separated better than OV-17 in the new columns. Because of the induction and dispersion forces from the grafted group, excellent chromatographic performance was shown in the two new stationary phases.. It is suitable for tetraphenyl phenyl polysiloxane and 2-methyl-3,4-diphenyl phenyl polysiloxane to be used as GC stationary phase.
引文
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