Sistema em linha para pré-concentração e determinação de cádmio e chumbo por Espectrometria de Absorção Atômica com chama utilizando minicoluna de espuma de poliuretano impregnada com 2-(2-benzotiazolilazo)-p-cresol.

AUTOR(ES)
DATA DE PUBLICAÇÃO

2001

RESUMO

In the present work, an on-line system for preconcentration and determination of cadmium and lead by Flame Atomic Absorption Spectrometry (FAAS) is proposed. It is based on the sorption of cadmium(II) and lead (II) ions onto a minicolumn packed with polyurethane foam loaded with 2-(2-benzothiazolylazo)-2-p-cresol (BTAC) reagent. BTAC was firstly synthesized, purified and characterized. Spectral characteristics of cadmium(II) and lead(II) BTAC complexes were also determined. Analytical parameters were evaluated and the results demonstrated that cadmium can be on-line preconcentrated, with sample pH in the range of 6.5 ? 9.5, preconcentration time of 1 min with a sampling rate of 7.0 ml min-1. The desorption is carried out with 0.10 mol l-1 hydrochloric acid solution at flow rate of 4.0 ml min-1. Afterwards, cadmium is determined by FAAS with detection limit of 0.27 mg l-1 and preconcentration factor of 41. The accuracy of procedure was confirmed by cadmium determination in certified reference materials. Others parameters such as: type and eluent concentration, type of buffer solution used, selectivity and column construction were also studied. In the on-line preconcentration of lead were proposed several modifications for a best performance of system. These modification include the use of system with two columns, two six-port valves and three-way solenoid valves. In the simplest procedure, lead can be on-line preconcentrated with the pH range of 6.7 - 9.3, with a sampling rate of 7.0 ml min-1. The desorption is carried out with 0.10 mol l-1 hydrochloric acid solution at flow rate of 4.0 ml min-1. Afterwards, lead is determined by FAAS with detection limit of 1.0 mg l-1 and preconcentration factor of 26. The accuracy was confirmed by lead determination in certified reference materials. The proposed system was used for lead determination in real samples such as seafoods and wines. Recoveries of spike additions (0.2 or 1.0 mg g-1) to several seafood samples were quantitative (90 - 107 %).

ASSUNTO(S)

espuma de poliuretano cádmio chumbo injeção em fluxo quimica analitica pré-concentração faas

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