Abstract

A simple and robust flow injection system which permits low sample and reagent consumption is described for rapid and reliable hydride generation atomic absorption spectrometric determination of selenium, arsenic and bismuth. The system, which composed of one peristaltic pump and one four channel solenoid valve, used water as the carrier streams for both sample and NaBH 4 solution. Rapid off-line pre-reduction of the analytes was achieved by using hydroxylamine hydrochloride for selenium and a mixture of potassium iodide and ascorbic acid for arsenic and bismuth. Transition metal interference was eliminated with the addition of thiourea and EDTA into the NaBH 4 solution and significant sensitivity enhancement was observed for selenium in the presence of thiourea in the reductant solution. Under optimised conditions, the method achieved detection limits of 0.2 ng mL −1 for Se, 0.5 ng mL −1 for As and 0.3 ng mL −1 for Bi. The method was very reproducible, achieving relative standard deviations of 6.3% for Se, 3.6% for As and 4.7% for Bi, and has a sample throughput of 360 h −1. Successful application of the method to the quantification of selenium, arsenic and bismuth in a certified reference river sediment sample is reported.

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