One-Step in-Syringe Dispersive Liquid-Liquid Microextraction and Spectrophotometric Determination of Trace Amounts of Palladium in Aqueous Sample

Document Type : Research Article

Authors

Department os Chemistry, Faculty of Science, University of Sistan and Baluchestan, Zahedan, I.R. IRAN

Abstract

A new and rapid methodology has been developed and applied successfully for the determination of trace levels of palladium in real water samples. This technique is based on the combination of In-Syringe Dispersive Liquid-Liquid microextraction (IS-DLLME) and micro-volume UV–Vis spectrophotometry. All extraction, preconcentration and separation steps were performed in a convenient 10-mL glass syringe. By means of a 1-mL syringe, a mixture of rhodanin (complexing agent), benzyl alcohol (extraction solvent) and ethanol (dispersive solvent) was injected rapidly
into the sample solution through the tip of 10 mL syringe which leads to the complexation of palladium and its extraction into the alcoholic phase. The extractant containing the target analyte was then transferred into UV-Vis spectrophotometer for analysis versus standards which were made in the same manner as the analyte. In order to prevent of precipitation of rhodanin, cetylpyridinum chloride surfactant was added to the aqueous samples before extraction. The factors influencing the extraction efficiency such as type and volume of extracting and disperse solvent, pH and volume of the sample and amount of ligand and surfactant were investigated and optimized. The developed protocol was found to have a linear calibration curve in the concentration range between 120 - 2000 µg/L with a limit of detection of 75 µg/L. Excellent enrichment factor of 44.8 fold was observed for the analyte. The repeatability of the method was satisfactory (RSD≤ 5.81%) and the total analysis time including microextraction was less than 10 min. The method has been successfully applied for the analysis of palladium in three spiked tap, lake and treated water samples.

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References

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