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  • Open tubular anion exchange chromatography. Controlled layered architecture of stationary phase by successive condensation polymerization.

Open tubular anion exchange chromatography. Controlled layered architecture of stationary phase by successive condensation polymerization.

Analytical chemistry (2007-06-21)
Petr Kubán, Purnendu K Dasgupta, Christopher A Pohl
RESUMEN

The preparation and performance of a multilayered stationary phase for open tubular anion exchange chromatography in relatively large bore (75 microm diameter) columns are described. The inner surface of a fused-silica capillary tube is coated with up to 25 successive porous polymeric layers formed by condensation polymerization of a primary amine with a diepoxide. Each layer of the anion exchange stationary phase consists of copolymer of methylamine (MA) and 1,4-butanedioldiglycidyl ether (BDDE). The polymer layers are sufficiently porous or permeable; each successive layer of the stationary phase incrementally increases the observed column capacity and chromatographic performance in the open tubular mode. Even though the column inner diameter is far from optimum for open tubular liquid chromatography, we demonstrate the baseline separation of a suite of inorganic anions (F-, Cl-, NO2-, Br-, NO3-) in a 5 m x 75 microm column coated with 25 layers of the anion exchange polymer using 1 mM KOH eluent and suppressed contactless conductometric detection at a flow rate of 1 microL/min (operating pressure of approximately 1 bar) with a plate count of >30,000. Strategies for construction of microsuppressor devices used in open tubular ion chromatography are discussed.

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Sigma-Aldrich
1,4-butanediol diglicidil éter, ≥95%
Sigma-Aldrich
1,4-butanediol diglicidil éter, technical grade, 60%