Multielement chromatographic profiling of environmental pollution.

This thesis describes the evaluation of the first commercially available Hewlett Packard gas chromatograph - microwave induced plasma - atomic emission detector (GC-MIP-AED) for application to qualitative and quantitative analysis. The technique was applied to a range of environmentally significant samples.A general introduction to the development of the technique and its suitability for environmental applications is discussed and a number of typical applications are reviewed.A fundamental study of the capabilities of the GC-MIP-AED was undertaken. It became apparent that the manufacturers pre-programmed recipes for the different elemental channels required optimising to eliminate ghost emission signals from other sources such as carbon molecular emission. After the optimisation of these elemental recipes for C, S, N, O, Pb and Cl had been achieved the ability of the instrument to perform multielement heteroatom profiling of a range of pollutants with a high degree of selectivity was established. Samples included oils, leaded and unleaded petrols, and coal pyrolyzates. A critical assessment of the instruments capabilities with respect to these applications and other operational issues is also described.The instruments ability to perform quantitative analysis was then studied highlighting a number of problem areas, such as, variable repeatability and limits of detection, relating to the automatic injection facilities. When the appropriate injection liner and injection technique were used, the limit of detection on all the elemental channels monitored was greatly improved.The study was then extended to utilise the GC-MIP-AED for the multielemental analysis of organomercury, organolead and organotin compounds. The instrumental conditions were optimised for each element individually with respect to instrumental operating parameters, repeatability, limit of detection, linearity of response, and also the chosen extraction and derivatisation technique. All parameters were then optimised for the analysis of organomercury, organolead and organotin compounds within a single chromatographic injection for environmental applications including sediment, fish tissue and water samples.The overall objective of this thesis was to identify and evaluate the multielement capabilities of the analytical technique for qualitative and quantitative application to samples of environmental relevance, in particular simultaneous multielement organometallic speciation.