Hollow fiber based liquid-phase microextraction for the determination of mercury traces in water samples by electrothermal atomic absorption spectrometry

Highlight: ► Hg (II) traces are preconcentrated by means of a three-phase liquid microextraction system. ► PAN and ammonium iodide are used in the donor and acceptor phase, respectively. ► Hollow-fiber pores are continuously fed with toluene placed in the lumen. ► Mercuric ions can be measured in waters below the μg L−1 level. - Abstract: A three-phase liquid microextraction procedure for the determination of mercury at low concentrations is discussed. To the aqueous sample placed at pH 7 by means of a phosphate buffer, 0.002% (m/v) 1-(2-pyridylazo)-2-naphthol (PAN) is incorporated, and the mixture submitted to microextraction with a hollow-fiber impregnated with toluene and whose lumen contains a 0.05 mol L−1 ammonium iodide solution. The final measurement of the extract is carried out by electrothermal atomic absorption spectrometry (300 °C and 1100 °C for the calcination and atomization temperatures, respectively). The pyrolytic graphite atomizer is coated electrolytically with palladium. An enrichment factor of 270, which results in a 0.06 μg L−1 mercury for the detection limit is obtained. The relative standard deviation at the 1 μg L−1 mercury level is 3.2% (n = 5). The reliability of the procedure is verified by analyzing waters as well as six certified reference materials.