Co-microprecipitation/flotation of trace amounts of cadmium from environmental samples through its complexation with iodide and neutralization with cetyltrimethylammonium bromide in the presence of perchlorate ions

Abstract

ABSTRACTA fast, cost-effective and reliable method is presented for separation and preconcentration of trace amounts of cadmium based on co-precipitation and flotation prior to its flame atomic absorption (AAS) spectrometric determination. Cadmium (II) was complexed with iodide and neutralized with cetyltrimethylammonium bromide (CTAB) in the presence of perchlorate ions. This resulted in the formation of a bulky precipitate containing the ternary complex of CdI4(CTA)2, floating on the top of the solution. The aqueous layer was then simply drained out, the floated layer was dissolved in 1.0 mL of acetonitrile, and its Cd content was determined by flame atomic absorption spectrometry. The parameters affecting the designed separation method such as KI, CTAB, and ClO4− concentration, pH, ionic strength, volumes of sample and dissolving solvent, and extraction time were studied and optimized. For preconcentration of 200 mL of the sample, the calibration graph was linear in the range of 1–30 μg L−1 of cadmium with a correlation coefficient of 0.9997, enhancement factor of 194 and a limit of detection of 0.18 μg L−1. The relative standard deviation for seven replicate determinations at 20 μg L−1 levels of cadmium was found to be 2.1%. The effect of the presence of different common cations and anions on the separation and determination of Cd(II) by the developed method was studied. The method was successfully applied to the determination of trace amounts of Cd(II) ions in different types of real samples including tap water, polluted industrial wastewater, dust, and soil with the recoveries in the range of 95.3 to 103.4.