Skip to Content
Merck
  • Characterization of large surface area polymer monoliths and their utility for rapid, selective solid phase extraction for improved sample clean up.

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 (2015-08-04)
Esme Candish, Hans-Jürgen Wirth, Andrew A Gooley, Robert A Shellie, Emily F Hilder
ABSTRACT

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 518m(2)g(-1) respectively. BET revealed a hypercrosslinked surface area of 817m(2)g(-1), 2.5 times greater than in the solvated state. The PDVB BET surface area was 531m(2)g(-1), similar to the solvated state. Micropores of 1nm provided the enhanced surface area for hypercrosslinked adsorbents. PDVB displayed a pore size distribution of 1-6nm. 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.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Iron(III) chloride, anhydrous, powder, ≥99.99% trace metals basis
Sigma-Aldrich
Hydrochloric acid solution, ~6 M in H2O, for amino acid analysis
Sigma-Aldrich
Acetonitrile solution, contains 0.1 % (v/v) trifluoroacetic acid, suitable for HPLC
Sigma-Aldrich
Acetonitrile solution, contains 0.05 % (v/v) trifluoroacetic acid
Sigma-Aldrich
Phosphoric acid solution, NMR reference standard, 85% in D2O (99.9 atom % D), NMR tube size 4.2 mm × 8 in. , WGS-5BL Coaxial NMR tube
Sigma-Aldrich
Acetonitrile solution, contains 0.1 % (v/v) formic acid, suitable for HPLC
Sigma-Aldrich
Styrene, ReagentPlus®, contains 4-tert-butylcatechol as stabilizer, ≥99%
Sigma-Aldrich
Methanol, anhydrous, 99.8%
Supelco
Hydrochloric acid solution, volumetric, 0.1 M HCl (0.1N), endotoxin free
Sigma-Aldrich
Hydrochloric acid solution, 1.0 N, BioReagent, suitable for cell culture
Sigma-Aldrich
Ibuprofen, meets USP testing specifications
Sigma-Aldrich
Ibuprofen, ≥98% (GC)
Sigma-Aldrich
Cortisone, ≥95%
Sigma-Aldrich
Hydrochloric acid, 36.5-38.0%, BioReagent, for molecular biology
Supelco
Ibuprofen
Sigma-Aldrich
Hydrochloric acid solution, 0.5 M
Sigma-Aldrich
Hydrochloric acid, suitable for arsenic determination, 35.0-37.0%
Sigma-Aldrich
Hydrochloric acid solution, 0.1 M
Sigma-Aldrich
Hydrochloric acid, suitable for determination of toxic metals, ≥35.0%
Sigma-Aldrich
Hydrochloric acid solution, 0.2 M
Sigma-Aldrich
Hydrochloric acid solution, 0.02 M
Sigma-Aldrich
Hydrochloric acid solution, 0.05 M
Sigma-Aldrich
Iron(III) chloride, CP
Sigma-Aldrich
Hydrochloric acid, SAJ first grade, 35.0-37.0%
Sigma-Aldrich
Hydrogen chloride – ethanol solution, 3% in ethanol
Sigma-Aldrich
Hydrochloric acid solution, 6 M
Sigma-Aldrich
Methanol, JIS special grade, ≥99.8%
Sigma-Aldrich
Hydrochloric acid, JIS special grade, 35.0-37.0%
Sigma-Aldrich
Hydrochloric acid, SAJ super special grade, ≥35.0%
Sigma-Aldrich
Hydrochloric acid solution, 0.01 M