首页> 外文期刊>Chromatographia >Synthesis and Applications of a Novel 3,4-Bis(2-Fluoro-5-Trifluoromethyl Phenyl)-2,5-Diphenyl Phenyl Grafted Polysiloxane Stationary Phase
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Synthesis and Applications of a Novel 3,4-Bis(2-Fluoro-5-Trifluoromethyl Phenyl)-2,5-Diphenyl Phenyl Grafted Polysiloxane Stationary Phase

机译:新型3,4-双(2-氟-5-三氟甲基苯基)-2,5-二苯基接枝聚硅氧烷固定相的合成及应用

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摘要

A novel polyphenyl-grafted polysiloxane stationary phase named 3,4-bis(2-fluoro-5-(trifluoromethyl)phenyl)-2,5-diphenyl phenyl grafted polysiloxane stationary phase (FFMP) was synthesized through a Diels-Alder reaction with a high column efficiency (average number of plates: 3700 plates/m; achieved by naphthalene at 120 A degrees C) and simultaneously coated on fused silica capillary tubes to prepare a gas chromatographic column with excellent performance. The column performance test results indicated that the FFMP columns could work properly up to 360 A degrees C, as evidenced by the chromatogram of the polyethylene pyrolysis mixture. The thermogravimetric analysis curve showed that the decomposition temperature of the FFMP was up to 380 A degrees C. The FFMP columns were also applied in the separation and analysis of multimixtures, such as Grob test mixtures, benzene mixtures and fatty acid esters, and as well as a medium polar stationary phase (according to the results of McReynolds constants, the sum of a dagger I was 779.) The FFMF columns exhibited excellent separation selectivity for these substances because of the conjugated system formed by the polyphenyl side chain connected by single bonds. This conjugated system can promote the delocalization of pi-electrons as well as enhance the forces of pi-pi interaction, and the dipole-induced dipole action between the FFMP stationary phase and the analytes.
机译:通过DIEL-Alder反应合成了名为3,4-双(2-氟-5-(二氟甲基)苯基)固定相(FFMP)的新型多苯基接枝的聚硅氧烷固定相。高柱效率(平均板数:3700平板/ m;通过120℃的萘实现,并同时涂布在熔融的石英毛细管上,以制备具有优异性能的气相色谱塔。柱性能测试结果表明FFMP柱可以正常工作,高达360℃,如聚乙烯热解混合物的色谱图所证明。热重分析曲线表明,FFMP的分解温度高达380℃。FFMP柱也用于多叠,例如GROB测试混合物,苯混合物和脂肪酸酯的分离和分析中,以及苯混合物和脂肪酸酯。作为中等极性静止相(根据McReynolds常数的结果,匕首I的总和为779.)FFMF柱由于由单键连接的多苯基侧链形成的共轭系统,这些物质表现出优异的分离选择性。该缀合系统可以促进PI-电子的临近分化以及增强PI-PI相互作用的力,以及FFMP固定相和分析物之间的偶极子诱导的偶极子作用。

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