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.
Date of Award | 2000 |
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Original language | English |
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Awarding Institution | |
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THE FABRICATION AND STUDY OF METAL CHELATING STATIONARY PHASES FOR THE HIGH PERFORMANCE SEPARATION OF METAL IONS
Shaw, M. J. (Author). 2000
Student thesis: PhD