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Characterization of large surface area polymer monoliths and their utility for rapid, selective solid phase extraction for improved sample clean up


Candish, E and Wirth, H-J and Gooley, AA and Shellie, RA and Hilder, EF, Characterization of large surface area polymer monoliths and their utility for rapid, selective solid phase extraction for improved sample clean up, Journal of Chromatography A, 1410 pp. 9-18. ISSN 0021-9673 (2015) [Refereed Article]

Copyright Statement

Copyright 2015 Elsevier B.V.

DOI: doi:10.1016/j.chroma.2015.07.065


While polymer monoliths are widely described for solid phase extraction (SPE), appropriate characterization is rarely provided to unravel the links between physical characteristics and observed advantages and disadvantages. Two known approaches to fabricate large surface area polymer monoliths with a bimodal pore structure were investigated. The first incorporated a high percentage of divinyl benzene (PDVB) and the second explored hypercrosslinking of pre-formed monoliths. Adsorption of probe analytes; anisole, benzoic acid, cinnamic acid, ibuprofen and cortisone were investigated using frontal analysis and the SPE performance was compared with particulate adsorbents. Frontal analysis of anisole described maximum adsorption capacities of 164mgg−1 and 298mgg−1 for hypercrosslinked and PDVB adsorbents, respectively. The solvated state specific surface area was calculated to be 341 and 518m2g−1 respectively. BET revealed a hypercrosslinked surface area of 817m2g−1, 2.5 times greater than in the solvated state. The PDVB BET surface area was 531m2g−1, similar to the solvated state. Micropores of 1nm provided the enhanced surface area for hypercrosslinked adsorbents. PDVB displayed a pore size distribution of 16nm. Frontal analysis demonstrated the micropores present size exclusion for the larger probes. Recovery of anisole was determined by SPE using 0.4 and 1.0mLmin−1. Recovery for PDVB remained constant at 90%0.103 regardless of the extraction flow rate suggesting extraction performance is independent of flow rate. A more efficient sample purification of saccharin in urine was yielded by PDVB due to selective permeation of the small pores.

Item Details

Item Type:Refereed Article
Keywords:sample preparation, porous polymer monolith, solid phase extraction, material characterization
Research Division:Chemical Sciences
Research Group:Analytical chemistry
Research Field:Separation science
Objective Division:Expanding Knowledge
Objective Group:Expanding knowledge
Objective Field:Expanding knowledge in the chemical sciences
UTAS Author:Candish, E (Ms Esme Candish)
UTAS Author:Gooley, AA (Dr Andrew Gooley)
UTAS Author:Shellie, RA (Associate Professor Robert Shellie)
UTAS Author:Hilder, EF (Professor Emily Hilder)
ID Code:105902
Year Published:2015
Web of Science® Times Cited:21
Deposited By:Austn Centre for Research in Separation Science
Deposited On:2016-01-20
Last Modified:2017-10-29

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