Department of Chemistry, Wayne State University, Detroit, MI 48202, USA.
J Chromatogr A. 2012 Nov 30;1266:124-30. doi: 10.1016/j.chroma.2012.09.104. Epub 2012 Oct 3.
A combination of gas chromatography and liquid-liquid partitions in totally organic biphasic systems is used to determine descriptor values for compounds of low volatility suitable for characterizing open tubular columns at high temperatures. The descriptor database of varied compounds includes several difficult to determine by conventional techniques due to their low water solubility or stability. The descriptor database facilitates an expansion of the descriptor space and compound variation for characterizing separation systems. As an application the descriptor database is used to determine the system constants for SPB-Octyl, HP-5, Rxi-5Sil MS, Rtx-440, and Rtx-OPP for the temperature range 200-300°C. As an example of the broader affect of temperature on column selectivity the variation of the system constants for Rtx-440 over the temperature range 60-300°C is described in detail. These studies demonstrate the persistence of polar interactions to the highest temperature studied and that at high temperatures selectivity differences persist for moderately polar stationary phases.
采用气相色谱法和完全有机双相体系中的液-液分配相结合的方法,测定适用于高温下描述开管柱的低挥发性化合物的描述符值。由于其低水溶性或低稳定性,常规技术难以测定的多种化合物的描述符数据库包括在内。描述符数据库有助于扩展描述符空间和化合物变化,以描述分离系统。作为应用,该描述符数据库用于确定在 200-300°C 的温度范围内 SPB-Octyl、HP-5、Rxi-5Sil MS、Rtx-440 和 Rtx-OPP 的系统常数。作为温度对柱选择性更广泛影响的一个例子,详细描述了 Rtx-440 在 60-300°C 温度范围内的系统常数的变化。这些研究表明,在研究的最高温度下仍然存在极性相互作用,并且在高温下,对于中等极性固定相,选择性差异仍然存在。