The analysis of organometallic compounds using SFC-ICPMS.

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dc.contributor.advisor Raynor, Mark W.
dc.contributor.advisor Cornell, David H.
dc.contributor.advisor Ross, Graham.
dc.creator Blake, Earl. 2011-12-21T07:53:06Z 2011-12-21T07:53:06Z 1994 1994
dc.description Thesis (M.Sc.-)-University of Natal, Durban, 1994. en
dc.description.abstract Supercritical fluid chromatography has recently been coupled to an ICPMS detector. The method has been shown to be suitable for the speciation and analysis of organometallic compounds at trace levels. This study has attempted to further the research initiated by other groups in this field by developing a new interface for coupling these two instruments. The new interface makes use of a modified join between the nebuliser and the torch in the ICP unit. The effect of the mobile phase on the plasma with time has been investigated and little spectral background interference has been observed. The chromatographic conditions were optimised using a flame ionisation detector and a series of tin, arsenic, iron, and mercury compounds were analysed using SFC-ICPMS. Mter focusing the ICP-MS on the element of interest, each compound was evaluated in terms of the change in peak intensity with change in concentration and the theoretical detection limits were compared to the practical detection limit. The restrictor temperature was determined using a rough calibration procedure with bench top experiments. The effect of the restrictor temperature on the peak intensity of each compound was then studied. All results were plotted and a theory for the observed trends and observations is proposed. The results obtained and the interface used have been compared to the results and interfaces of other groups and differences have been explained. Attempts to extract relevant compounds from topsoil using supercritical fluid extraction were made. Finally, sediment samples were collected from relevant points in Durban Bay and an attempt was made to extract these samples using supercritical fluid extraction. The extracted samples were analysed using SFC-ICPMS although little success was obtained. Reasons for the failure of this method on the real samples have been proposed. In the concluding section of this study SFC~ICPMS has been evaluated in terms of its future applicability and use as a viable analytical method. en
dc.language.iso en en
dc.subject Organometallic compounds. en
dc.subject Supercritical fluid chromatography. en
dc.subject Plasma spectroscopy. en
dc.subject Theses--Chemistry. en
dc.title The analysis of organometallic compounds using SFC-ICPMS. en
dc.type Thesis en

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