Abstract

Four inductively coupled plasma mass spectrometric methods: nebulization sample introduction with external calibration; hydride generation with external calibration; isotope dilution with nebulization; and isotope dilution with hydride generation, have been tested and compared. Multimode Sample Introduction System (MSIS™) was employed in either nebulization or hydride generation mode. Best limits of detection (below 0.1 μg L − 1 ) and accuracy were obtained for isotope dilution techniques in hydride generation and sample nebulization mode. A mixture of HNO 3 and H 2O 2 served both for microwave-assisted digestion as well as a medium for subsequent plumbane generation. Optimal reagent concentrations for hydride generation stage were 0.1 mol L − 1 HNO 3, 0.28 mol L − 1 H 2O 2 and 1.5% m/v NaBH 4. Critical effects of acidity, blanks and concomitants have been discussed. Analytical methods were validated by use of plant and water certified reference materials and spiked high-salt solutions (seawater and 20% m/v NaCl) at lead levels in nanograms per gram to micrograms per gram range.

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