The preparation and characterisation of chelating sorbents suitable for the high efficiency separation of trace metals in complex samples, using a single column and isocratic elution, is described. Hydrophobic, neutral polystyrene divinylbenzene resins were either impregnated with chelating dyes or dynamically modified with heterocyclic organic acids, using physical adsorption and chemisorption processes respectively. A hydrophilic silica substrate was covalently bonded with a chelating aminomethylphosphonic acid group, to assess the chelating potential of this molecule. These substrates were characterised in terms of metal retention capability (selectivity coefficients and capacity factors), separation performance, column efficiency and suitability for analytical applications. Chelating molecules with different ligand groups were found to have unique selectivity patterns dependant upon the conditional stability constants of the chelate. Other factors, including mobile phase constituents - complexing agents, ionic strength and pH, column length and column capacity were additionally investigated to examine their effect upon the separation profiles achieved. The promising metal separation abilities illustrated by a number of these chelating columns were exploited for the determination of trace toxic metals in complex sample matrices using High Performance Chelation Ion Chromatography (HPCIC). This included the determination of beryllium in a certified stream sediment, uranium in seawater and a certified stream sediment, and cadmium, lead and copper in a certified rice flour. The results for each analysis fell within the certified limits, and reproducibility was good. The optimisation of post column detection systems using chromogenic ligands additionally gave good detection limits for the metals in each separation system.
| Identifer | oai:union.ndltd.org:bl.uk/oai:ethos.bl.uk:311708 |
| Date | January 2000 |
| Creators | Shaw, Matthew James |
| Publisher | University of Plymouth |
| Source Sets | Ethos UK |
| Detected Language | English |
| Type | Electronic Thesis or Dissertation |
| Source | http://hdl.handle.net/10026.1/1938 |
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