Optimization of experimental parameters in the determination of zinc in sea water by adsorptive stripping voltammetry

• Autor(a) principal: Arancibia,V.
• Data de Publicação: 2010
• Outros Autores: Zúñiga,M., Zúñiga,M. C., Segura,R., Esteban,M.
• Tipo de documento: Artigo
• Idioma: eng
• Título da fonte: Journal of the Brazilian Chemical Society (Online)
• Texto Completo: http://old.scielo.br/scielo.php?script=sci_arttext&pid=S0103-50532010000200010
• topic: zinc; adsorptive voltammetry; sea water samples; multivariate experimental design

A procedure for the determination of zinc in sea water by square wave adsorptive stripping voltammetry (SWAdSV) using 8-hydroxyquinoline (oxine) as an adsorbing and complexing agent has been optimized. First, a univariate study of the Zn-Ox complex peak current as a function of pH was carried out choosing values at which adequate currents were obtained. Then, selection of the experimental conditions was made using a multivariate experimental design. Variables like pH, oxine concentration (Cox), adsorption time (t ads) and adsorption potential (Eads) were optimized. The first optimization step was a 2(4) factorial design with 16 measurements made choosing high and low levels, and three measurements at the central point (Zn(II) 10.0 μg L-1). Analysis of variance showed that pH and Cox were the most significant factors, while t ads and Eads were not significant and were kept constant in later measurements. Next, to find the optimum values for pH and Cox a 2² + star factorial design was used. The best experimental parameters were pH = 6.0; Cox = 25 μmol L-1; t ads = 10 s and Eads = -0.70 V. Under these conditions the peak current was proportional to the concentration of zinc over the 0.1-48.0 μg L-1 range, with a detection limit of 0.05 μg L-1. Reproducibility for 5.0 μg mL-1 Zn(II) solution was 1.9 % (n = 16). The method was validated using spiked synthetic sea water (ASTM D665), sea water reference material (CRM-SW. Zn 5 μg kg-1) and fortified water reference material (GBW08607. Zn 5 mg kg-1) with satisfactory results. Finally, the method was successfully applied to the determination of Zn(II) in sea water samples without prior treatment.