Sensitive determination of mercury in tap water by cloud point extraction pre-concentration and flow injection-cold vapor-inductively coupled plasma optical emission spectrometry

摘要

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 polyethyleneglycomono-p-nonylphenylether (PONPE 5). Cold vapor generation was developed from 100 #mu#l 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 deection obtained under the optimal conditions was 4 ng l~(-1). The precision for 10 replicate determinations at the 0.5-#mu#g l~(-1) Hg level was 3.4% relative standard deviation (R.S.D.), calculated with the peak heights. The calibration grpah using the pre-concentration system for mercury was linear with a correlation coefficient of 0.9998 at levels near the detection lmits up to at least 50 #mu#g l~(-1). The method was successfully applied to the determination of mercury in tap water samples.