Abstract
A simple and selective method for rapid extraction and determination of Pd(II) ions was developed based on sorption on octadecyl-bonded silica membrane disks of an ion associate of PdBr42− anion with 1-hexadecylpyridinium cation. The sample containing Pd(II) in the presence of 0.15 M of NaBr and 10 mg 1-hexadecylpyridinium bromide was passed through the membrane disk by applying a slight vacuum. Elution was accomplished using 6 ml of acetonitrile. Extraction efficiency and the influence of flow rates of sample solution and eluent, pH, amount of 1-hexadecylpyridinium bromide, type and least amount of eluent for elution of Pd(II) from disks, break through volume and limit of detection were evaluated. Also the effect of various ions on percent recovery of Pd(II) was studied. Extraction efficiencies > 99% were obtained by elution of the disks with minimal amount of solvent. The extraction efficiencies do not depend on the pH (1–10) of solutions nor on the sample solution flow rate in the range of 1–25 ml/min. Hence, with a typical preconcentration factor of 200 the limit of detection of the proposed method is 0.6 µg (for 1000 ml of sample solution). The method was applied to the recovery and determination of Pd(II) in Al–Si–Pd catalysts.
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