ABSTRACT
Abstract A method for determination of trace mercury in water was established. The trace mercury in water was adsorbed quantitatively by activated carbon, and then determined by electrical pyrolysis atomic absorption spectrometry. In comparison with the detection methods of total mercury in water at present, the method avoids the steps of digestion, reduces the mercury pollution and the loss of the mercury, and is simple in operation. The effects of particle size of activated carbon, acid treatment method, acid medium and enrichment time on the enrichment efficiency were investigated. The effect of the pyrolysis temperature and the interfering ions on the determination results was investigated. Three standard addition procedures including activated carbon blank addition, solution blank addition and environmental water samples addition were studied. Regression correlation coefficients of three standard curves drawn by the three methods reached 0 . 9999 . The slope of the three standard curves had no difference by statistical test, indicating that the determination of mercury in environmental water samples under the experiment conditions was not interfered by the coexistent elements, which showed that the activated carbon blank addition method could be directly used for preparing standard curve of the method. The water samples containing 5 ng/L and 50 ng/L mercury were determined by the method, and the relative standard deviation were 7. 2% and 4. 2% (n=11), respectively, with a detection limit of 1. 2 ng/L. The recovery experiment was carried out after adding 10 ng/L mercury to the surface water and tap water samples, and the recoveries were between 92. 0% and 103. 0%. Analysis results were compared with ICP-MS as control and the deviation of the two methods were between 2 . 9% and 3 . 4%, indicating that the method was accurate and reliable, and had good precision.
ABSTRACT
A sequential extraction procedure has been proposed for the evaluation of the speciation of heavy metals including Cd,Cu,Pb and Zn in sediments from mariculture area,and the speciation of heavy metals was separated and defined as acid soluble fraction,reducible fraction,fraction bound organic matter,fraction bound sulfides and residual fraction. Matrix effects of high salinity on the determination of heavy metals in sediments were eliminated by matrix matching and internal standard methods when inductively couple plasma optical emission spectroscopy (ICP-OES) and mass spectroscopy (ICP-MS) were used,respectively. The results showed that the measured values of marine sediment reference materials were consistent with the standard values when the digestion solutions were determined after dilution. The extraction results of the prepositional extraction procedure and European Community Bureau of Reference Program (BCR) procedure were compared and the selectivity of extractants was investigated. The preliminary studies indicated that this sequential extraction procedure was applicable for evaluating the speciation of heavy metals in sediment with organic substances pollution and eutrophication,especially for fraction bound organic matter and fraction bound sulfides.