A Pre-Concentration Procedure Using Cloud Point Extraction for the Determination of Manganese in Saline Effluents of a Petroleum Refinery by Flame Atomic Absorption Spectrometry

Abstract

This paper describes the development of a cloud point extraction procedure for the determination of manganese in saline effluents by flame atomic absorption spectrometry (FAAS). The optimization step was performed using the Doehlert matrix involving the following variables: buffer concentration, pH and centrifugation time. The validation process was assessed as: parameters of the analytical curve, precision, effect of other ions in the proposed procedure, robustness test and accuracy. The proposed procedure allows the determination of manganese with a detection limit (3δ/S) of 0.60 µg L−1, and a precision expressed as relative standard deviation (RSD) of 2.2 (n = 8) and 1.5% (n = 8) for a manganese concentration of 1 and 5 µg L−1, respectively. The pre-concentration factor obtained was 84. The recovery achieved for the determination of manganese in the presence of several other metal ions demonstrated that this procedure could be satisfactorily applied to the analysis of environmental samples. The accuracy was confirmed by the analysis of CRM trace elements in water (NIST 1643d). This procedure was applied to the determination of manganese in saline effluents of a petroleum refinery. For three analyzed samples the manganese content varied between 44.9 and 67.9 µg L−1.