ABSTRACT
This paper describes a preconcentration method for Hg(2+) and MeHg(+) in water samples using sodium diethyldithiocarbamate immobilized in polyurethane foam (PU-NaDDC) and an extraction method for several mercury species in sediment samples, including MeHg(+), EtHg(+) and PhHg(+), which is simple, rapid, and uses a single organic solvent. Separation and measurement were done by high-performance liquid chromatography on-line with inductively coupled plasma mass spectrometry (HPLC/ICP-MS). Initially, the test of recovery was applied using procedures compatible with HPLC. Under the optimum extraction conditions, recoveries of 96.7, 96.3 and 97.3% were obtained for MeHg(+), EtHg(+), and PhHg(+), respectively, from n=4 spiked sediment samples. This study also demonstrates that the combination of solid-phase extraction on PU-NaDDC with HPLC separation and ICP-MS detection is an effective preconcentration procedure for simultaneous measurement of Hg(2+) and MeHg(+) at ultra-trace levels in water samples. The application of the proposed procedure to the determination of mercury species in drinking water sample was investigated. The proposed method clearly gave satisfactory average recoveries between 93.7 and 101.5%.
Subject(s)
Chromatography, High Pressure Liquid/methods , Fresh Water/analysis , Geologic Sediments/analysis , Mass Spectrometry/methods , Mercury Compounds/analysis , Organomercury Compounds/analysis , Brazil , Ethylmercury Compounds/analysis , Ethylmercury Compounds/isolation & purification , Fresh Water/chemistry , Geography , Geologic Sediments/chemistry , Linear Models , Mercury Compounds/isolation & purification , Methylmercury Compounds/analysis , Methylmercury Compounds/isolation & purification , Organomercury Compounds/isolation & purification , Phenylmercury Compounds/analysis , Phenylmercury Compounds/isolation & purification , Reproducibility of Results , RiversABSTRACT
A multiinjection strategy has been developed to increase the sampling throughput of the high-performance liquid chromatography determination of inorganic-mercury, methylmercury, ethylmercury and phenylmercury. The method involves the injection of samples each 3.5min, in spite of the fact that phenylmercury retention time corresponds to 9.04min. In the selected conditions, the sampling frequency was 11h(-1) in front of that of 6h(-1), obtained by conventional injection of each sample after the complete elution of Hg species. Additionally, the analytical reagents consumption was reduced drastically in almost 50%. The main characteristics of the chromatographic separation were maintained and only the resolution of phenylmercury was reduced from 10.3 to 1.7 and that of ethylmercury from 4.6 to 3.1.
ABSTRACT
The high salinization in some reservoirs of the Contas river basin (Bahia-Brazil) has been erroneously attributed only to concentration by evaporation. However, recent studies of this basin have shown that in period of intense rainfalls, occur an increase of the saline concentration in the flowing rivers of the reservoirs. The application of statistical methods (cluster and principal components analysis) have shown that this fact can be attributed to the discharge of saline waters from the small reservoirs of every drained area, provoked by inundation, is also an important factor in the salinization process. Thus the study of the geochemical variables: Na(+), K(+), Ca(2+), Mg(2+), Cl(-), SO(4)(2-) and CO(3)(2-), showed one group formed by Na(+) and Cl(-), attributed to the discharge of saline water provoked by inundation from a small reservoir, and a second group constituted by Ca(2+), Mg(2+), K(+) and SO(4)(2-), due to an increase provoked by the evaporation in the salinization process.
