Characterization of C18-bonded liquid chromatographic stationary phases by Raman spectroscopy:: the effect of temperature

被引:63
作者
Doyle, CA
Vickers, TJ
Mann, CK
Dorsey, JG [1 ]
机构
[1] Florida State Univ, Dept Chem, Tallahassee, FL 32306 USA
[2] Univ Cincinnati, Dept Chem, Cincinnati, OH 45221 USA
关键词
stationary phases; LC; Raman spectroscopy; temperature effects; mobile phase composition;
D O I
10.1016/S0021-9673(00)00174-6
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
This study represents the first time that both the mobile phase composition and the temperature are simultaneously controlled to examine silica-bonded octadecylsilyl (C-18) ligands spectroscopically at typical liquid chromatographic (LC) mobile phase flow-rates and back-pressures. Raman spectroscopy is used to characterize the behavior of the C-18 bonded ligands equilibrated at temperatures from 45 to 2 degrees C in neat, single-component, mobile phase solvents including: water, acetonitrile, methanol, and chloroform. In addition, the effect of stationary phase ligand bonding density is examined by using two different monomeric reversed-phase liquid chromatographic (RPLC) stationary phases, a 2.34 and a 3.57 mu mol m(-2) Microporasil C-18 stationary phase, under identical conditions. The direct, on-column, spectroscopic analysis used in this study allows direct evaluation of the temperature-dependent behavior of the bonded C-18 ligands. The temperature-dependent ordering of the stationary phase ligands is examined to determine if the ligands undergo a phase transition from a less-ordered "liquid-like" state at higher temperatures to a more-ordered "solid-like" state at lower temperatures. A discrete phase transition was not observed, but rather a continual ordering as temperature was lowered. (C) 2000 Elsevier Science B.V. All rights reserved.
引用
收藏
页码:41 / 59
页数:19
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