Adamantyl-group containing mixed-mode acrylamide-based continuous beds for capillary electrochromatography. Part II. Characterization of the synthesized monoliths by inverse size exclusion chromatography and scanning electron microscopy

• Characterization of the domain size of acrylamide-based continuous beds by SEM.
• Measurement of pore size distributions and exclusion pore sizes by ISEC.
• The impact of the concentration of AS on morphology, pore size distribution, and pore volumes is studied.
• For monoliths with small domain size a trimodal pore size distribution is confirmed.
• An excellent capillary-to-capillary, day-to-day, and run-to-run repeatability is reached.

In our previous article we have described the synthesis of a new amphiphilic monolithic stationary phase by in situ free radical copolymerization of cyclodextrin-solubilized N-adamantyl acrylamide, piperazinediacrylamide, methacrylamide and vinylsulfonic acid in aqueous medium in pre-treated fused silica capillaries of 100 μm I.D. In the present work, we study the morphology of different monolithic stationary phases synthesized under variation of the concentration of ammonium sulfate in the polymerization mixture. The pore size distribution is determined with inverse size exclusion chromatography (ISEC) using the retention data of a series of polystyrene standards with narrow molecular size distribution and known average molar mass ranging from 1560 to 2 010 000 g mol−1. The impact of the concentration of the lyotropic salt ammonium sulfate in the polymerization mixture on the formed morphology, the pore size distribution, and the fractional volume of mesopores and macropores is determined. The homogeneity and uniformity of the formed monolith over the length of the capillary and the covalent attachment to the confining walls are confirmed. Repetition of the synthesis procedure shows that these morphology parameters are well controlled as there is an excellent capillary-to-capillary, day-to-day, and run-to-run reproducibility reached for the electroosmotic mobility and the retention factor determined with alkylphenones in the reversed-phase mode.