Application of simplex optimization in the development of an automated online preconcentration system for manganese determination

Abstract

An automated procedure was developed to determine trace amounts of manganese from vegetal leaves and river waters using flame atomic absorption spectrometry (FAAS) after online preconcentration of this metal using an Amberlite XAD-4 minicolumn modified with 2-aminothiophenol. The preconcentration system is based on the solid-phase extraction of the metal into the minicolumn and elution with 0.30 mol L-1 hydrochloric acid, followed by its determination. Variables associated with the preconcentration system performance, such as pH, sampling flow rate and eluent concentration were optimized using a basic simplex as multivariate technique. The developed method provides an improvement factor of 14 along with limit of detection (3σB) of 2.0 μg L-1, and precision expressed as a 2.2% relative standard deviation (RSD%, n = 10, 30.0 μg L-1). The procedure was applied to determine manganese in river waters collected from urban area of Jequié/Bahia. The accuracy of the procedure was checked by analysis of two certified reference materials (apple leaves, NIST 1515 and spinach leaves, NIST 1570). The developed procedure has been applied for manganese determination in vegetal leaves (chive, spinach, cauliflower and cabbage). © 2010 Sociedade Brasileira de Química.