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The influence of the synthesis pressure on the chromatographic properties of poly(divinylbenzene-co-ethylvinylbenzene-co-2-hydroxyethyl methacrylate) monolithic columns
Authors:K. N. Smirnov  I. A. Dyatchkov  A. V. Pirogov  O. A. Shpigun
Affiliation:1.Division of Analytical Chemistry, Department of Chemistry,Moscow State University,Moscow,Russia
Abstract:Monolithic columns based on copolymer of divinylbenzene (DVB), ethylvinylbenzene (EVB), and 2-hydroxyethyl methacrylate (HEMA) were prepared and applied to the separation of low-molecular-weight aromatic compounds. The monoliths were synthesized via thermally initiated free-radical polymerization in confines of stainless steel tubes with dimensions of 100 × 4.3 mm. In order to compensate for the polymer shrinkage during the synthesis and prevent the monolith from detachment from the column wall, the polymerization was conducted under nitrogen pressure. The excess pressure was varied from 0 bar to 9 bar. The synthesis under pressure was shown to improve the peak shapes and column efficiency in comparison with the synthesis in the closed tube. The optimum pressure for poly(DVB-co-EVB-co-HEMA) monoliths was found to be 3 bar. The efficiency of the column obtained at 3 bar is 13 500 TP/m for propylbenzene (k′ = 6) and 38 300 TP/m for uracil (k′ = 0).
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