Application of factorial designs and Doehlert matrix in optimization of experimentalvariabl es associated with the preconcentration and determination of vanadium and copper in seawater by inductively coupled plasma optical emission spectrometry

Abstract

In the present paper a procedure for preconcentration and determination of vanadium and copper in seawater using inductively coupled plasma optical emission spectrometry (ICP OES) is proposed, which is based on solid-phase extraction of vanadium (IV), vanadium (V) and copper (II) ions as 1-(2-pyridylazo)-2-naphthol (PAN) complexes by active carbon. The optimization process was carried out using two-level full factorials and Doehlert matrix designs. Four variables (PAN mass, pH, active carbon mass and shaking time) were regarded as factors in the optimization. Results of the two-level full factorial design 24 with 16 runs for vanadium extraction, based on the variance analysis (ANOVA), demonstrated that the factors pH and active carbon mass, besides the interaction (pH=active carbon mass), are statistically significant. For copper, the ANOVA revealed that the factors PAN mass, pH and active carbon mass and the interactions (PAN mass=pH) and (pH=active carbon mass) are statistically significant. Doehlert designs were applied in order to determine the optimum conditions for extraction. The procedure proposed allowed the determination of vanadium and copper with detection limits (3syS) of 73 and 94 ng ly, 1 respectively. The precision, calculated as relative standard deviation (R.S.D.), was 1.22 and 1.37% for 12.50 mg lyof1 vanadium and copper, respectively. The preconcentration factor was 80. The recovery achieved for determination of vanadium and copper in the presence of severalcations demonstrated that this procedure improved the selectivity required for seawater analysis. The procedure was applied to the determination of vanadium and copper in seawater samples collected in Salvador City, Brazil. Results showed good agreement with other data reported in the literature.