Optimization of cloud point extraction procedure with response surface methodology for quantification of iron by means of flame atomic absorption spectrometry

Abstract

A simple micelle-mediated phase separation method has been developed for the pre-concentration of trace levels of iron as a prior step to determination by flame atomic absorption spectrometry (FAAS). The method is based on the cloud point extraction (CPE) of iron using non-ionic surfactant polyethyleneglycolmono-p-nonylphenylether (PONPE 7.5) without adding any chelating agent. Several variables affecting the extraction efficiency were studied and optimized utilizing central composite design (CCD) and three levels full factorial design. Under the optimum conditions, the limit of detection (LOD), limit of quantification (LOQ) and pre-concentration factor were 1.5 μg L-1, 5.0 μg L-1 and 100, respectively. The relative standard deviation (RSD) for six replicate determinations at 50 μg L−1 Fe(III) level was 1.97%. The calibration graph was linear in the rage of 5-100 μg L-1, with a correlation coefficient of 0.9921. The developed method was validated by the analysis of two certified reference materials and applied successfully to the determination of trace amounts of Fe(III) in water and rice samples.

Keywords

• iron
• ligand-less cloud point extraction
• central composite design
• full factorial design
• flame atomic absorption spectrometry
• rice samples