Synthesis of New Polycyclic Phenyl Group Graft Polysiloxane as GC Stationary Phase and Its Chromatographic Performance Evaluation

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.