School of Earth Sciences - Theses

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    Detection of uranium(VI) in groundwater using a field electroanalytical technique
    Dwyer, Athene Tracy ( 1999)
    In this thesis electroanalytical methods are investigated and a new method developed to determine uranium(VI) in groundwater samples. Differential pulse polarography, differential pulse voltammetry and adsorptive stripping voltammetry methods, with appropriate mercury drop electrodes, were optimised using the adsorptive chelate 2,5-dichloro-3,6-dihydroxy-l,4-benzoquinone (chloranilic acid). An alternative adsorptive stripping voltammetry method, with a hanging mercury drop electrode, was optimised using the chelate 8-hydroxyquinoline (oxine). The liquid mercury requirements of these techniques limit their use in the field. Therefore, mercury film electrode methods that are potentially better suited to field conditions are investigated. Chloranilic acid was found to be a suitable chelating agent for uranium determination in combination with a hanging mercury drop electrode, but the reduction of chloranilic acid was a concern. A new mercury film electrode determination method using chloranilic acid was developed but was found to result in the deterioration of the MFE to the extent of rendering the method unsuitable for uranium determination. An adsorptive stripping voltammetry, MFE method with oxine was investigated. The inability to remove the uranyl-oxine reaction products from the MFE created a memory effect that contributed to a lack of accuracy and precision when performing standard addition determinations. This interference was a significant factor in the inability to reliably measure a uranium response using an adsorptive stripping potentiometry method with oxine. The technique of square wave adsorptive stripping voltammetry with oxine in combination with a hanging mercury drop electrode was found to be the most appropriate method for uranium determination. The method was fast, sensitive, precise and accurate when analysing standard solutions. A low detection limit of 2.7 µg/L was achieved. Groundwater and surface water samples were analysed by the AdSV, HMDE method with oxine. The mineral spring water samples from Daylesford, Victoria, were high in ionic content and contained interfering ions. The unacidified samples contained high concentrations of dissolved C02 that needed to be removed prior to sample analysis to prevent pH changes during analysis. Of six unacidified samples uranium was found in only one sample, the Tipperary Spring sample at 4.9 µg/L U(VI). Interference prevented confirmation of this concentration in the acidified Tipperary Spring sample. The construction of a linear standard addition plot with a positive x-intercept was a common outcome for both the unacidified and the acidified spring samples. The uranium concentration was determined in three surface water samples collected from the Ranger Uranium Mine in the Northern Territory. Matrix interference in these surface water samples resulted in non-linearity for two standard addition determinations. A third sample was successfully analysed to give a concentration of 23 µg/L U(VI), which is in good agreement with an independent determination. The unselective nature of oxine was found to result in significant interference when analysing environmental samples by the AdSV, HMDE method with oxine. This method was found to be inappropriate for field analysis of environmental samples. However, in a laboratory environment the AdSV, HMDE method with oxine was the best performing method when determining uranium in standard solutions.