In this study, a syringe was filled with silica gel loaded with 3-aminopropyltriethoxysilane, for the separation and preconcentration of copper, cadmium and chromium prior to their determination by graphite furnace atomic absorption spectrometry (GFAAS) in seawater. For this purpose, a syringe was filled with 0.5 g of modified silica gel and the sample solution was drawn into the syringe and ejected back again. The analyte elements were quantitatively retained at pH 5. Then, the elements sorbed by the silica gel were eluted with 2.0 M of HCl and determined by GFAAS. At optimum conditions, the recovery of Cu, Cd and Cr were 96-98%. Detection limits (3delta) were 6.6, 7.5 and 6.0 micro g L(-1) for Cu, Cd and Cr, respectively. The elements could be concentrated by drawing and discharging several portions of sample successively but eluting only once. Cu, Cd and Cr added to a seawater sample were quantitatively recovered (>95%) in the range of the 95% confidence level. The method proposed in this paper was compared with a column technique. Optimum experimental conditions, reproducibility, precision and recoveries of both techniques are the same, but the syringe technique is much faster, easier and more practical than the column technique. It is a portable system and allows one to make the sorption process in the source of sample. In addition, the risk of contamination is less than in the column technique.
Silica gels modified with 3-aminopropyltriethoxysilane or 3-mercaptopropyltrimethoxysilane groups have been developed for the preconcentration of copper and cadmium prior to their determination by flame atomic absorption spectrometry. The surface areas of the modified silica gels were determined by the Brunauer-Emmett-Teller (BET) method to be 290 m2 g-l of the amino-modified silica and 410 m2 g-1 of the thiol-modified silica. Batch and column methods were used for the separation and concentration of copper and cadmium. These metals were quantitatively retained on both the modified gels in slightly acidic media. In the batch method, the effects of pH, shaking time and type of buffer on the adsorption of copper and cadmium were investigated. In the batch and column procedures both copper and cadmium adsorbed on the silicas were quantitatively recovered (relative standard deviation of 2-6%) using 2 mol dm-3 hydrochloric acid even in the presence of sodium chloride up to a concentration of 1 .O%.
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