The determination of copper, iron and nickel in edible oils was carried out using emulsion sample preparation followed by analysis by ICP-AES. Response surface methodology was applied in order to find the optimum emulsion and surfactant concentrations. The optimum amount of oil in the emulsion was in the range ca. 2-35% in most of the surfactants studied, except for Triton X-100, which showed a maximum response above 35% oil. The surfactant concentration in the emulsion varied between 0.5 and 9%. Good agreement was found between calibration curves for emulsified aqueous standards solutions and oil-in-water emulsions for most elements studied with Tween 80, ethoxynonylphenol and Triton X-100. The best agreement for all elements was shown when Tween 80 was used. Hence emulsified aqueous standard solutions could be used for the determination of these elements in emulsified edible oil samples using ICP-AES. Recoveries ranged from 90 to 110% for most of the elements studied, with relative standard deviations lower than 8%. the use of surfactants to enhance the sample transport process.

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A direct hydride generation nebulizer (DHGN) was explored for introduction of the sample in inductively coupled plasma-optical emission spectrometry (ICP-OES) using radially viewed mode. This simple hydride generation system was constructed in our laboratory and requires similar plasma operating conditions to conventional nebulizer-spray-chamber arrangements. This work was focused on the optimization of the operating conditions for hydride generation and evaluation of the main analytical figures of merit for the determination of As, Sb and Se. The excitation conditions of the ICP-OES instrument operated with the DHGN were also explored. Results showed that the analytical performance of the new system for the determination of As, Sb and Se was superior to that of conventional nebulization systems. The DHGN also enabled the determination of elements that do not form volatile hydrides, but with less sensitivity than conventional nebulization systems. Evaluation of the plasma robustness showed that gases generated in hydride generation do not significantly affects the plasma discharge. Similar to conventional hydride generation techniques, analysis with DHGN was susceptible to non-spectroscopic interferences produced by transition metals. Finally, the utility of the DHGN in practical ICP-OES studies was demonstrated in the determination of trace elements in an oyster tissue standard reference material.

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A new nebulizer system is described that extends the analytical capability of the inductively coupled plasma technique to include the simultaneous determination of two elements Sb and Sn (hydride-forming), with two conventional elements, V and Zn. The main advantage of this system is its simultaneous determination of elements that form volatile hydrides and elements that do not, without any instrumental changes. Optimization of reaction and instrumental conditions was performed to characterize the new system. The performance of the new nebulizer system was evaluated by studying the effect of some transition metals (Ni, Cu, Co, and Fe, 1-1000 mg L(-1)) on the Sb, Sn, V, and Zn emission signals (1 mg L(-1)). Interferences from transition metal ions were found to be insignificant for determination of the four elements in presence of L: -cysteine. Long-term and short-term stability was also evaluated. The precision, expressed as RSD for 15 replicate measurements was 0.7% for Sb, 1.7% for Sn, 2.5% for V, and 2.3% for Zn at 200 microg L(-1) of each analyte. The detection limits obtained were 0.52, 1.3, 3.2, and 4.7 microg L(-1) for Sb, Sn, V, and Zn, respectively. Spike and recovery experiments were performed on the NIST 1643c trace metals in water standard reference material and results were in agreement with the certified values.

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