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Effect of hypercrosslinking conditions on pore size distribution and efficiency of monolithic stationary phases
Author(s) -
Urban Jiří,
Škeříková Veronika
Publication year - 2014
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201400730
Subject(s) - divinylbenzene , chemistry , alkylation , styrene , solvent , alkyl , catalysis , alkylbenzenes , volume (thermodynamics) , reactivity (psychology) , mass transfer , monolithic hplc column , chemical engineering , chromatography , organic chemistry , copolymer , high performance liquid chromatography , polymer , medicine , physics , alternative medicine , pathology , engineering , quantum mechanics
Three dihalogenic solvents differing in the length of alkyl chain (1,2‐dichloroethane, 1,4‐dichlorobutane, and 1,6‐dichlorohexane) with three Friedel–Crafts alkylation catalysts varying in reactivity (AlCl 3 , FeCl 3 , and SnCl 4 ) have been used to prepare hypercrosslinked poly(styrene‐ co ‐vinylbenzyl chloride‐ co ‐divinylbenzene) columns. Hydrodynamic characteristics as well as column efficiency and mass transfer resistance were tuned by the combination of swelling solvent and alkylation reaction catalyst in the modification mixture. The column swelled in 1,6‐dichlorohexane and hypercrosslinked in the presence of AlCl 3 provided the highest column efficiency and enabled fast isocratic separations of small molecules in a RP mode. To uncover factors controlling the efficiency of hypercrosslinked monolithic columns, we have studied pore volume distribution of prepared columns. We found that column efficiency increases with the higher pore volume of pores smaller than 2 nm.