Multivariate technique for optimization of digestion procedure by focussed microwave system for determination of Mn, Zn and Fe in food samples using FAAS

This article describes the development by response surface methodology (RSM) of a procedure for iron, zinc and manganese determination by flame atomic absorption spectrometry (FAAS) in food samples after digestion employing a focussed microwave system. A Doehlert matrix was used to find optimal conditions for the procedure through response surface study. Three variables (irradiation power and time and composition of oxidant solution-HNO3 + H2O2) Were regarded as factors in the optimization study. The working conditions were established as a compromise between optimum values found for each analyte taking into consideration the robustness of the procedure. These values were 12 min. 260 W and 42% (v/v) for irradiation time, irradiation power and percent of H2O2 in solution, respectively. The accuracy of the optimized procedure was evaluated by analysis of certified reference materials and by comparison with a well-established closed vessel microwave dissolution methodology. (c) 2005 Elsevier B.V. All rights reserved.