Abstract
A novel vortex-assisted liquid–liquid microextraction (VA-LLME) for determination of iodide was developed. The method includes the oxidation of iodide with iodate in the presence of hydrochloric acid followed by VA-LLME of the ion-pair formed between ICl2− and Astra Phloxine reagent (AP) and subsequent absorbance measurement at 555nm. The appropriate experimental conditions were investigated and found to be: 5mL of sample, 0.27molL−1 HCl, 0.027mmolL–1 KIO3 as the oxidation agent, 250μL of extraction mixture containing amyl acetate as the extraction solvent and carbon tetrachloride as the auxiliary solvent (1:1, v/v), 0.04mmolL−1 AP reagent, vortex time: 20s at 3000rpm, centrifugation: 4min at 3000rpm. The calibration plot was linear in the range 16.9–169μg L−1 of iodide, with a correlation coefficient (R2) of 0.996, and the relative standard deviation ranged from 1.9 to 5.7%. The limit of detection (LOD) and limit of quantification (LOQ) were 1.75 and 6.01μgL−1 of iodide, respectively. The suggested procedure was applied for determination of iodide in real mineral water samples.
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