Abstract
A pre-concentration and determination methodology for mercury at trace levels in water samples was developed. Cloud point extraction was successfully employed for the pre-concentration of mercury prior to inductively coupled plasma optical emission spectrometry coupled to a flow injection with cold vapor generation system. The mercury was extracted as mercury-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol [Hg(II)-(5-Br-PADAP)] complex, at pH 9.2 mediated by micelles of the non-ionic surfactant polyethyleneglycolmono- p-nonylphenylether (PONPE 5). Cold vapor generation was developed from 100 μl of the extracted surfactant-rich phase by means of a stannous chloride (SnCl 2) solution as reluctant. An exhaustive study of the variables affecting the cloud point extraction with PONPE 5 and cold vapor mercury generation from the surfactant phase was performed. The 50-ml sample solution pre-concentration allowed us to raise an enrichment factor of 200-fold. The lower limit of detection obtained under the optimal conditions was 4 ng l −1. The precision for 10 replicate determinations at the 0.5-μg l −1 Hg level was 3.4% relative standard deviation (R.S.D.), calculated with the peak heights. The calibration graph using the pre-concentration system for mercury was linear with a correlation coefficient of 0.9998 at levels near the detection limits up to at least 50 μg l −1. The method was successfully applied to the determination of mercury in tap water samples.
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