Characterization of surface of trifluorophenylketoiminepropyl stationary phase coated porous layer open tubular columns

A series of 3 fluorinated adsorbents were prepared by bonding 4,4,4-trifluoro-1-phenyl-1,3-ketoiminepropyl silane onto 5 μm Nucleosil silica. The first one contained sole fluoroketoimine groups, while the other two adsorbents were derivatives of the first one with copper(II) chloride and copper(II) acetylacetonate bound through the fluoroketoimine groups. A description of syntheses of these adsorbents is given and the course of each stage of the syntheses is characterized by elemental analysis, surface area determination, UV–vis, EPR, ICP-OES, IR, 29Si NMR, 13C NMR and thermogravimetric analysis. For the columns coated with the adsorbents obtained the donor–acceptor character of the adsorption layer was established and the enthalpy of adsorption was determined for a selected group of hydrocarbons. The evenness of capillary column walls coating and mechanical stability of the stationary phases was evaluated on the basis of the flow restriction factor and SEM images. Efficiency of the columns obtained and their comparison with commercial counterparts are presented.

► Changes occurring on silica during the synthesis of phases for columns are monitored.
► Thermodynamic characteristics of adsorbents for capillary columns are determined.
► Quality and mechanical stability of obtained layer in PLOT columns are specified.
► Some examples of separation of organic compounds on obtained columns are presented.