Simultaneous separation and preconcentration of Cr(III), Cu(II), Cd(II) and Pb(II) from environmental samples prior to inductively coupled plasma optical emission spectrometric determination
ABSTRACT We have developed a new method of the separation, preconcentration, and determination of Cr(III), Cu(II), Cd(II) and Pb(II) ion in water samples. It is based on the use of activated carbon that was modified with rhodamine 6G to yield a solid-phase sorbent. The experimental conditions for adsorption were optimized. Cr(III), Cu(II), Cd(II) and Pb(II) can be quantitatively adsorbed at pH 4, and adsorbed Cr(III), Cu(II), Cd(II) and Pb(II) can be completely eluted with 1M hydrochloric acid. The maximum adsorption capacity is 37.8, 47.8, 56.5 and 41.7 mg g(-1) for Cr(III), Cu(II), Cd(II) and Pb(II). Cr(III), Cu(II), Cd(II) and Pb(II) ions were then determined by inductively coupled plasma optical emission spectrometry. The detection limit (3σ) is under 0.35 ng mL(-1), and the relative standard deviation is lower than 3.5% (n=11). Common potentially interfering ions do not interfere with the adsorption and determination of the analytes. The method displays selectivity, sensitivity and reproducibility, and was successfully applied to the determination of biological and water samples.
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ABSTRACT: A gas-diffusion flow injection method with amperometric detection for the indirect detn. of copper on a silver electrode was developed. The flow through system was equipped with two injection valves and a gas-diffusion unit. In the first step, a signal of a cyanide soln. was recorded. In the subsequent step, the signal of cyanide in the presence of copper was measured. Interferences (Cd(II), Co(II), Ag(I), Ni(II), Fe(III), Hg(II) and Zn(II)) were investigated and successfully removed. The calibration graph was linear in the range 1-90 μmol dm-3 of copper with a correlation coeff. of 0.993. The regression equation is I = (0.0455 ± 0.0015)c + (0.4611 ± 0.0671), where I is the relative signal decrease in μA and c is concn. in μmol dm-3. Relative std. deviation for six consecutive injections of 30 μmol dm-3 copper(II) was 1.47 % and for 1 μmol dm-3 copper(II), it was 3.40 %. The detection limit, calcd. as 3 s/m (where s is a std. deviation of nine measurement of a reagent blank and m is theJournal of the Serbian Chemical Society 01/2012; 77(11-11):1641-1647. DOI:10.2298/JSC120616090L · 0.87 Impact Factor
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ABSTRACT: A new, simple and rapid method based on dispersive liquid-liquid microextraction (DLLME) was developed for extracting and preconcentrating copper (Cu), nickel (Ni), lead (Pb) and cadmium (Cd) in water samples prior to flame atomic absorption spectrometry (FAAS) analysis. 1-(2-thiazolylazo)-naphthol (TAN) was used as chelating reagents, and non-ionic surfactant Triton X-114 and CCl(4) as disperser solvent and extraction solvent, respectively. Some influential factors relevant to DLLME, such as the concentration of TAN, type and volume of disperser and extraction solvent, pH and ultrasound time, were optimized. Under the optimal conditions, the calibration curve was linear in the range of 10-800 μg L(-1) for Cu and Ni, 10-500 μg L(-1) for Pb, and 10-1,000 μg L(-1) for Cd, respectively. The limits of detection for the four metal ions were below 0.5 μg L(-1), with the enhancement factors of 105, 66, 28 and 106 for Cu, Ni, Pb and Cd, respectively. The relative standard deviations (RSD, n = 6) were 2.6-4.1%. The proposed method was applied to determination of Cu, Ni, Pb and Cd in water samples and satisfactory relative recoveries (93.0-101.2%) were achieved.Water Science & Technology 11/2012; 67(2):247-53. DOI:10.2166/wst.2012.524 · 1.11 Impact Factor
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ABSTRACT: A new magnetic solid sorbent was synthesized using 3-mercaptopropionic acid grafted silica modified Fe3O4 magnetic nanoparticles. The sorbent was characterized by SEM, XRD, and FT-IR and used for solid phase extraction of Al3+ and Cr3+ ions. Al3+ and Cr3+ ions were measured by graphite furnace and flame atomic absorption spectrometry, respectively. The optimal extraction/preconcentration conditions including pH of sample solution, desorption conditions (type, concentration, and volume of the eluent), sonication time, sample volume, adsorbent amount, and interfering ions were studied. Under optimal conditions, the detection limits of 0.09 and 0.19 ng mL−1 were obtained with a relative standard deviation (RSD%) of 2.1–5.2% for Al3+ and Cr3+ ions, respectively. The enrichment factors were found to be 99 and 92 for Al3+ and Cr3+ ions, respectively. The effects of various cationic interferences on percent recovery of Al3+ and Cr3+ ions were studied. The developed method was successfully applied for selective extraction and preconcentration of trace amounts of Al3+ and Cr3+ in biological and environmental samples.Journal of Analytical Atomic Spectrometry 01/2013; 28(2):251-258. DOI:10.1039/C2JA30286A · 3.47 Impact Factor