Metal fractionation in sediments of the Sergipe River, northeast, Brazil

The sequential extraction procedure proposed by the European Community Bureau of Reference (BCR) was applied for the fractionation of Cd, Cr, Cu, Ni, Pb and Zn in sediments from the Sergipe Estuary, Brazil. The method showed satisfactory recoveries, detection limits and standard deviations for trace metals determinations in sediment samples. Cd was the metal with the greatest percentage in the exchangeable fraction. Pb and Ni were present mainly in the reducible and oxidizable fractions. Cr, Cu and Zn were predominantly associated with the residual fraction. The order of mobility of metals extracted was Pb > Cd > Ni > Cu > Cr > Zn. According to the risk assessment code (RAC), the sediments showed low to medium risk for all metals. _________________________________________________________________________________________ RESUMO: O procedimento de extração seqüencial proposto pelo European Community Bureau of Reference (BCR) foi empregado para o fracionamento de Cd, Cr, Cu, Ni, Pb e Zn em sedimentos do estuário do Rio Sergipe, Brasil. O método empregado apresentou-se adequado com limite de detecção e desvio padrão aceitável para a determinação de metais em amostras de sedimentos. Cd foi o metal com maior percentagem na fração extraível. Ni e Pb estão presentes principalmente nas frações oxidável e redutível. Cr, Cu e Zn foram encontrados predominantemente na fração residual. A ordem de mobilidade dos metais extraídos foi Pb > Cd > Ni > Cu > Cr > Zn. De acordo com o código de avaliação de risco (RAC), as amostras de sedimentos mostraram risco baixo a médio para todos os metais analisados

Construção de uma cela de fluxo para medidas por espectrofotometria em fase sólida

A simple and low cost flow cell is proposed for measurements by solid-phase spectrophotometry employing a conventional spectrophotometer. The flow cell geometry allows the employment of a large amount of the solid support without causing both excessive attenuation of the radiation beam and increasing of the back-pressure. The adaptation of the flow cell in the optical path of the spectrophotometer in order to increase the precision is discussed. The flow cell characteristics were demonstrated by measurements of Co(II), employing 1-(2-tiazolylazo)-2-naphthol (TAN) immobilized on C18 bonded silica as solid support. The apparent molar absorptivity and coefficient of variation were estimated as 1.86 x 10(5) L mol-1 cm-1 and 1.4 % (n=15). A sample throughput of 40 determinations per hour and a detection limit of 15 mug L-1 (99.7 % confidence level) were achieved

Preconcentration and Determination of Copper and Zinc in Natural Water Samples by ICP-AES After Complexation and Sorption on Amberlite XAD-2

The present paper describes a procedure for separation, preconcentration and sequential determination of trace amounts of copper and zinc in natural water samples, by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES). The proposed method is based on the complexation of copper(II) and zinc(II) ions by 1-(2-thiazolylazo)-2-naphthol (TAN) and sorption on to Amberlite XAD-2 resin. Parameters such as: TAN amount, pH effect on the complexation and sorption of TAN complexes, agitation time for complete sorption, concentration of metal ion, mass of Amberlite XAD-2, desorption of metal ions from XAD-2 resin and sample volume were studied. The results demonstrated that the copper(II) and zinc(II) ions, in the range of 0.10 to 100.00 mug, contained in a solution sample volume of 400 mL, in the pH range of 5.7 to 8.3, on the form of TAN complexes had been quantitatively retained on to XAD-2 resin. The shaking time required for sorption is 1 h using a resin mass of 1.4 g. The solution for determination of copper and zinc by ICP-AES is obtained, after desorption of the ions from the XAD-2 resin, using 5 mL of 2 mol L-1 hydrochloric acid and shaking the system for 5 min. The procedure was applied to the determination of copper and zinc in several natural water samples. The standard addition technique was applied and the obtained recoveries revealed that the proposed procedure has a good accuracy. A high enrichment factor (80) and simplicity are the main advantages in this analytical protocol

Preconcentration and Determination of Copper and Zinc in Natural Water Samples by ICP-AES After Complexation and Sorption on Amberlite XAD-2

The present paper describes a procedure for separation, preconcentration and sequential determination of trace amounts of copper and zinc in natural water samples, by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES). The proposed method is based on the complexation of copper(II) and zinc(II) ions by 1-(2-thiazolylazo)-2-naphthol (TAN) and sorption on to Amberlite XAD-2 resin. Parameters such as: TAN amount, pH effect on the complexation and sorption of TAN complexes, agitation time for complete sorption, concentration of metal ion, mass of Amberlite XAD-2, desorption of metal ions from XAD-2 resin and sample volume were studied. The results demonstrated that the copper(II) and zinc(II) ions, in the range of 0.10 to 100.00 mug, contained in a solution sample volume of 400 mL, in the pH range of 5.7 to 8.3, on the form of TAN complexes had been quantitatively retained on to XAD-2 resin. The shaking time required for sorption is 1 h using a resin mass of 1.4 g. The solution for determination of copper and zinc by ICP-AES is obtained, after desorption of the ions from the XAD-2 resin, using 5 mL of 2 mol L-1 hydrochloric acid and shaking the system for 5 min. The procedure was applied to the determination of copper and zinc in several natural water samples. The standard addition technique was applied and the obtained recoveries revealed that the proposed procedure has a good accuracy. A high enrichment factor (80) and simplicity are the main advantages in this analytical protocol