Analytical Sciences

Abstract − Analytical Sciences, 21(11), 1337 (2005).

Thermospray Flame Furnace-AAS Determination of Copper after On-line Sorbent Preconcentration Using a System Optimized by Experimental Designs
César Ricardo Teixeira TARLEY,* Eduardo da Costa FIGUEIREDO,** and Geraldo Domingues MATOS**
*Departamento de Ciências Exatas, Universidade Federal de Alfenas (Unifal-MG), Rua Gabriel Monteiro da Silva, 714, 3713-000, Alfenas, Minas Gerais, Brazil
**Departamento de Química Analítica, Universidade Estadual de Campinas (Unicamp), Campus Universitário Zeferino Vaz, 13083-970, Campinas, São Paulo, Brazil
The present paper describes the on-line coupling of a flow-injection system to a new technique, thermospray flame furnace-AAS (TS-FF-AAS), for the preconcentration and determination of copper in water samples. Copper was preconcentrated onto polyurethane foam (PUF) complexed with ammonium O,O-diethyldithiophosphate (DDTP), while elution was performed using 80% (v/v) ethanol. An experimental design for optimizing the copper preconcentration system was established using a full factorial (24) design without replicates for screening and a Doehlert design for optimization, studying four variables: sample pH, ammonium O,O-diethyldithiophosphate (DDTP) concentration, presence of a coil and the sampling flow rate. The results obtained from the full factorial and based on a Pareto chart indicate that only the pH and the DDTP concentration, as well as their interaction, exert influence on the system within a 95% confidence level. The proposed method provided a preconcentration factor of 65 fold, thus notably improving the detectability of TS-FF-AAS. The detection limit was 0.22 µg/dm3 and the precision, expressed as the relative standard deviation (RSD) for eight independent determinations, was 2.7 and 1.1 for copper solutions containing 5 and 30 µg/dm3, respectively. The procedure was successfully applied for copper determination in water samples.