Department of Chemistry and Pharmaceutical Sciences, University of Ferrara , Italy.
Anal Chem. 2013 Jan 2;85(1):19-22. doi: 10.1021/ac303253b. Epub 2012 Dec 13.
The intrusion of water into the pores of hydrophobic materials is investigated by means of a dynamic flow system. The porous hydrophobic material is packed into a stainless steel chromatographic column, and water is flushed through by means of a high-pressure pump. Back-pressure control is provided by flow restrictors after the column. The applied pressure forces the water to penetrate the pores of the hydrophobic material. The water volume contained in the column, as a function of the applied pressure, reflects the degree of wetting of the solid by water. This volume is determined by measuring, through a mass spectrometer, the retention time of deuterium oxide injected in the column. The method is applied with alkyl-modified (n-octyl and n-octadecyl) and perfluorinated (alkyl and phenyl) silica surfaces. The information gathered by this study may contribute to explain the retention behavior of reversed-phase chromatographic columns when used under highly aqueous mobile-phase conditions.
采用动态流动系统研究水对疏水性材料孔隙的侵入。将多孔疏水性材料装入不锈钢色谱柱中，通过高压栗将水冲洗通过。在柱后通过流量限制器提供背压控制。所施加的压力迫使水渗透到疏水性材料的孔隙中。柱中所含的水体积（作为施加压力的函数）反映了固体被水润湿的程度。通过测量通过质谱仪注入柱中的重水的保留时间来确定该体积。该方法应用于烷基改性（正辛基和正十八烷基）和全氟化（烷基和苯基）硅胶表面。通过这项研究收集的信息可能有助于解释反相色谱柱在高水流动相条件下使用时的保留行为。
