Synthesis And Separation Characteristics Of Two Fluoro Tetraphenyl-phenyl Polysiloxane Stationary Phases For Capillary Gas Chromatography

After more than 60 years of development, chromatographic separation technology has become a necessary testing methods in various fields. In order to meet the needs of development of chromatography technology, we need to synthesize a gas chromatographic stationary phase which has the high column efficiency, a wide range of using temperature and the high polarity. The previous study shows that the column can exhibited superior separation capability may due to the high content of aromatic rings introduced onto the side chain of polysiloxanes, could produce a large aromatic π-conjugate structure, it was not only able to strengthen both the dipole-induced dipole interactions and dispersive interactions with polar solutes, but also the dispersive interaction with nonpolar solutes. We synthesize and characteristic two fluoro tetraphenyl-phenyl polysiloxane stationary phases. In this paper, the main job has four aspects:1 This paper introduces the development process of gas chromatography. The types of gas chromatographic stationary phase, the development of gas chromatography technology, the application of gas chromatography technology was reviewed respectively. Including five different types of stationary phase ranging from polydimethylsiloxane to polymethylphenyl siloxane and the rapid growth of the comprehensive two-dimensional gas chromatography, high-speed gas chromatography, gas chromatography-mass spectrometry. Moreover, the applications of gas chromatography technology in different fields was also discussed.2 The synthesis of two types of multi-phenyl grafted polysiloxanes containing fluoro. The methyl vinyl polysiloxanes with 10%,15% 20% vinyl contents were prepared by combining the D4 and D4Vi in the catalysis of tetramethylammonium; two kinds of cyclopentadienones containing fluoro were synthesized through benzoin condensation, catalytic oxidation and the react with dibenzyl ketone while using 3,5-Difluorobenzaldehyde and 4-Fluoro-3-phenoxybenzaldehyde as raw materials, respectively. Finally,3,4-di(3,5-difluoro phenyl)-2,5-diphenyl phenyl polysiloxane (FFP-10, FFP-20) and 3,4-di(3-phenoxy-4-fluoro phenyl)-2,5-diphenyl phenyl polysiloxane (DPFP-10, DPFP-15) were synthesized through Diels-Alder reaction between methyl vinyl polysiloxane and cyclopentadienones containing fluoro at high temperature.3 The preparation and evaluation of capillary gas chromatography column. The FFP-10, FFP-20 and DPFP-10, DPFP-15 stationary phase were coated on the inner of capillary columns by the static method, respectively. After aging at high temperature, the polarity, column efficiency, working temperature range, etc. were evaluated. The results showed that both these two kinds of stationary phase has high column efficiency, belongs to the medium polarity column and shows good temperature resistance.4 The separation of the actual samples. In order to provide a further evidence for these column have good selectivity performance, the aromatic isomers, substituted benzene mixtures, polycyclic aromatic hydrocarbons, fatty acid ester, fatty alcohols, etc. were examined. These stationary phases had a great applied prospects.