2011International Journal of Environmental & Analytical ChemistryRequires access

Cloud point extraction for the determination of cadmium and lead employing sequential multi-element flame atomic absorption spectrometry

Walter Nei Lopes dos Santos, Dannuza Dias Cavalcante, Hadla S. Ferreira, Cesário Francisco das Virgens, Aline Rocha Borges, Márcia M. Silva, Maria Goreti R. Vale

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Abstract

A cloud point extraction procedure for pre-concentration and determination of cadmium and lead in drinking water using sequential multi-element flame atomic absorption spectrometry is described. 4-(2-thiazolylazo)-orcinol (TAO) has been used as complexing agent and the micellar phase was obtained using the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114) and centrifugation. The conditions for reaction and extraction (surfactant concentration, reagent concentration, effect of incubation time, etc) were studied and the analytical characteristics of the method were determined. The method allows the determination of cadmium and lead with quantification limits of 0.30 µg L−1 and 2.6 µg L−1, respectively. A precision expressed as relative standard deviation (RSD, n = 10) of 2.3% and 2.6% has been obtained for cadmium concentrations of 10 µg L−1 and 30 µg L−1, respectively, and RSD of 1.3% and 1.7% for lead concentrations of 10 µg L−1 and 30 µg L−1, respectively. The accuracy was confirmed by analysis of a natural water certified reference material. The method has been applied for the determination of cadmium and lead in drinking water samples collected in the cities of Ilhéus and Itabuna, Brazil. Recovery tests have also been performed for some samples, and results varied from 96 to 105% for cadmium and 97 to 106% for lead. The cadmium and lead concentrations found in these samples were always lower than the permissible maximum levels stipulated by World Health Organization and the Brazilian Government.

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What this paper is about

A cloud point extraction procedure for pre-concentration and determination of cadmium and lead in drinking water using sequential multi-element flame atomic absorption spectrometry is described. 4-(2-thiazolylazo)-orcinol (TAO) has been used as complexing agent and the micellar phase was obtained using the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114) and centrifugation. The conditions for reaction and extraction (surfactant concentration, reagent concentration, effect of incubation time, etc) were studied and the analytical characteristics of the method were determined. The method allows the determination of cadmium and lead with quantification limits of 0.30 µg L−1 and 2.6 µg L−1, respectively. A precision expressed as relative standard deviation (RSD, n = 10) of 2.3% and 2.6% has been obtained for cadmium concentrations of 10 µg L−1 and 30 µg L−1, respectively, and RSD of 1.3% and 1.7% for lead concentrations of 10 µg L−1 and 30 µg L−1, respectively. The accuracy was confirmed by analysis of a natural water certified reference material. The method has been applied for the determination of cadmium and lead in drinking water samples collected in the cities of Ilhéus and Itabuna, Brazil. Recovery tests have also been performed for some samples, and results varied from 96 to 105% for cadmium and 97 to 106% for lead. The cadmium and lead concentrations found in these samples were always lower than the permissible maximum levels stipulated by World Health Organization and the Brazilian Government.

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Available abstract

A cloud point extraction procedure for pre-concentration and determination of cadmium and lead in drinking water using sequential multi-element flame atomic absorption spectrometry is described. 4-(2-thiazolylazo)-orcinol (TAO) has been used as complexing agent and the micellar phase was obtained using the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114) and centrifugation. The conditions for reaction and extraction (surfactant concentration, reagent concentration, effect of incubation time, etc) were studied and the analytical characteristics of the method were determined. The method allows the determination of cadmium and lead with quantification limits of 0.30 µg L−1 and 2.6 µg L−1, respectively. A precision expressed as relative standard deviation (RSD, n = 10) of 2.3% and 2.6% has been obtained for cadmium concentrations of 10 µg L−1 and 30 µg L−1, respectively, and RSD of 1.3% and 1.7% for lead concentrations of 10 µg L−1 and 30 µg L−1, respectively. The accuracy was confirmed by analysis of a natural water certified reference material. The method has been applied for the determination of cadmium and lead in drinking water samples collected in the cities of Ilhéus and Itabuna, Brazil. Recovery tests have also been performed for some samples, and results varied from 96 to 105% for cadmium and 97 to 106% for lead. The cadmium and lead concentrations found in these samples were always lower than the permissible maximum levels stipulated by World Health Organization and the Brazilian Government.

Key concepts: Cadmium, Cloud point, Chemistry, Extraction (chemistry), Atomic absorption spectroscopy, Detection limit, Certified reference materials, Chromatography

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