Ottiger Stefan, Kluge Johannes, Rajendran Arvind, Mazzotti Marco
ETH Zurich, Institute of Process Engineering, Sonneggstrasse 3, 8092 Zurich, Switzerland.
J Chromatogr A. 2007 Aug 24;1162(1):74-82. doi: 10.1016/j.chroma.2007.01.115. Epub 2007 Feb 5.
The separation of the enantiomers of 1-phenyl-1-propanol by supercritical fluid chromatography on a chiral stationary phase, which consists of cellulose tris (3,5-dimethylphenylcarbamate) coated on a silica support (Chiralcel-OD), is studied under overloaded, non-linear chromatographic conditions. Pulse experiments are performed at a temperature of 30 degrees C using supercritical CO(2) modified with methanol as a mobile phase. The parameters of the binary Langmuir adsorption isotherm are determined by the inverse method, comparing experimental and simulated peak responses. Isotherm parameters are derived for modifier concentrations between 1 and 5% (w/w) and operating pressures between 125 and 185 bar, and the dependency of the isotherm parameters, namely the Henry constant and the saturation capacity, on operating conditions is investigated.
研究了在过载、非线性色谱条件下,使用涂覆在硅胶载体(Chiralcel-OD)上的三(3,5-二甲基苯基氨基甲酸酯)纤维素作为手性固定相,通过超临界流体色谱法分离1-苯基-1-丙醇对映体。在30℃温度下,使用用甲醇改性的超临界CO₂作为流动相进行脉冲实验。通过比较实验峰响应和模拟峰响应的反演方法确定二元朗缪尔吸附等温线的参数。得出了改性剂浓度在1%至5%(w/w)之间以及操作压力在125至185巴之间的等温线参数,并研究了等温线参数(即亨利常数和饱和容量)对操作条件的依赖性。