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Dispersive liquid-liquid microextraction

  • Speciation and Determination of Trace Amount of Inorganic Arsenic in Water, Environmental and Biological Samples

    Speciation and Determination of Trace Amount of Inorganic Arsenic in Water, Environmental and Biological Samples

    A b s t r a c t

    Anew speciation and preconcentration method based on dispersive liquid-liquid microextraction has been developed for trace amounts of As(III) and As(V) in urine and water samples. At pH 4, As(III) is complexed with ammoniumpyrrolidine dithiocarbamate and extracted into 1-Hexyl-3-methylimidazolium hexafluorophosphate, as an ionic liquid (IL) and As(III) is determined by electrothermal atomic absorption spectrometery (ETAAS). Arsenic(V) in the mixing solution containing As(III) and As(V) was reduced by using KI and ascorbic acid in HCl solution and then the procedure was applied to determination of total arsenic. Arsenic(V) was calculated as the difference between the total arsenic content and As(III) content. The effect of various parameters on the recovery of the arsenic ions has been studied. Under the optimum conditions, the enrichment factor 135 was obtained. The proposed method was successfully applied to the determination of trace amounts of As(III) and As(V) in water and biological samples.

    Authors

    Hamid Shirkhanloo, Hassan Zavvar Mousavi and Ahmad Rouhollah

    ACKNOWLEDGEMENTS

    The financial support of this work by K. N. Toosi University of Technology and Semnan University Research Council are greatly acknowledged.

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  • Ultra-trace Arsenic Determination in Urine and Whole Blood Samples

    Ultra-trace Arsenic Determination in Urine and Whole Blood Samples

    A b s t r a c t

    A noble method for pre-concentration and speciation of ultra trace As (III) and As (V) in urine and whole blood samples based on dispersive liquid-liquid microextraction (DLLME) has been developed. In this method, As (III) was complexed with ammonium pyrrolidine dithiocarbamate at pH = 4 and Then, As (III) was extracted into the ionic liquid (IL). Finally, As (III) was back-extracted from the IL with hydrochloric acid (HCl) and its concentration was determined by flow injection coupled with hydride generation atomic absorption spectrometry (FI-HGAAS). Total amount of arsenic was determined by reducing As (V) to As (III) with potassium iodide (KI) and ascorbic acid in HCl solution and then, As (V) was calculated by the subtracting the total arsenic and As (III) content. Under the optimum conditions, for 5-15 mL of blood and urine samples, the detection limit (3σ) and linear range were achieved 5 ng L−1 and 0.02-10 μg L−1, respectively. The method was applied successfully to the speciation and determination of As (III) and As (V) in biological samples of multiple sclerosis patients with suitable precision results (RSD < 5%). Validation of the methodology was performed by the standard reference material (CRM).

    Authors

    Hamid Shirkhanloo,†,‡ Ahmad Rouhollahi,†,* and Hassan Zavvar Mousavi§

    ACKNOWLEDGEMENT

    The authors thank from Petroleum Industry Health Organization (PIHO), Medical Industrial Laboratory of PIHO and Research Institute of Petroleum Industry (IRPI), Tehran, Iran.

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