Volume 40, Issue 8 pp. 1703-1709
SHORT COMMUNICATION

Monolithic stationary phases with a longitudinal gradient of porosity

Jiří Urban

Corresponding Author

Jiří Urban

Department of Analytical Chemistry, Faculty of Chemical Technology, University of Pardubice, Pardubice, Czech Republic

Current address: Dr. Jiří Urban, Department of Chemistry, Faculty of Science, Masaryk University, 625 00 Brno, Czech Republic.

Email: [email protected]

Correspondence

Dr. Jiří Urban, Department of Analytical Chemistry, Faculty of Chemical Technology, University of Pardubice, Studentská 573, Pardubice, Czech Republic, CZ-532 10.

Fax: +420466037068

Emails: [email protected];

[email protected]

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Tomáš Hájek

Tomáš Hájek

Department of Analytical Chemistry, Faculty of Chemical Technology, University of Pardubice, Pardubice, Czech Republic

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Frantisek Svec

Frantisek Svec

The Molecular Foundry, E.O. Lawrence Berkeley National Laboratory, Berkeley, CA, USA

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First published: 22 February 2017
Citations: 10

Conflict of interest: The authors have declared no conflict of interest.

Abstract

The duration of the hypercrosslinking reaction has been used to control the extent of small pores formation in polymer-based monolithic stationary phases. Segments of five columns hypercrosslinked for 30–360 min were coupled via zero-volume unions to prepare columns with segmented porosity gradients. The steepness of the porosity gradient affected column efficiency, mass transfer resistance, and separation of both small-molecule alkylbenzenes and high-molar-mass polystyrene standards. In addition, the segmented column with the steepest porosity gradient was prepared as a single column with a continuous porosity gradient. The steepness of porosity gradient in this type column was tuned. Compared to a completely hypercrosslinked column, the column with the shallower gradient produced comparable size-exclusion separation of polystyrene standards but allowed higher column permeability. The completely hypercrosslinked column and the column with porosity gradient were successfully coupled in online two-dimensional liquid chromatography of polymers.