A new method for extraction and pre-concentration of the heavy metals using a microemulsion system in winsor II equilibrium and determination by HR-CS AAS

Abstract

For the very first time, a microemulsion system in the Winsor II (WII) equilibrium was applied in a sample preparation method for extraction and pre-concentration in the determination of Pb, Cd, Co, Tl, Cu and Ni, in natural waters by high resolution continuum source atomic absorption spectrometry (HR-CS AAS). The method was optimized using the graphite furnace atomization. A simplex-centroid design for determine optimum extraction condition (77.5% aqueous phase, 5% of the oil phase, and 17.5% cosurfactant/surfactant ratio - C/S = 4) was applied. The optimized time for the sample preparations was around 30 min. The analytical performance of the optimized method using HR-CS GF AAS showed that the detection limits were: 0.09, 0.01, 0.06, and 0.05 μg L^-1 for determination of Pb, Cd, Tl, and Co, respectively and the enrichment factors were between 6 and 19, considered excellent for all analytes. The RSD values were lower than 5%, demonstrating the good precision of the proposed method. When the optimized method was applied using the HR-CS F AAS, the sensibility increased 9 to 12 times for Cu and Ni, respectively. The analytical method was successfully applied for the determination of analytes in Certified Reference Material and real samples for natural waters such as Brackish water (recovery between 107 and 112%), Saline water (recovery between 83 and 94%), Produced water from oil industry (recovery between 98 and 110%) and Fresh water (recovery 80 and 87% to Cu and Ni respectively). All the results confirming the accuracy of the analytical method proposed. The repeatability of the measurements has been better 5% (n = 3), for all elements.

Keywords: Atomic absorption spectrometry; Extraction; Metals; Microemulsion; Pre-concentration; Waters analysis.