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FAAS determination of palladium after its selective recovery by silica modified with hydrazone derivative

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Abstract

Amino propyl silica (APS) gel reacts immediately with benzyl monopyridyl hydrazone (BMPH) to produce a new effective and selective derivative (BMPH-APS) for the separation and preconcentration of traces of Pd(II) in aqueous solution. Factors affecting the sorption and desorption of Pd ions have been investigated. Acidic aqueous solution of 0.5% thiourea in 0.5 mol L−1 HCl has been used as eluent for the desorption of Pd(II). The stripped metal ion was determined by flame AAS. The modified silica quantitatively sorbed Pd(II) at pH 2–4 with a sorption capacity of 0.65 mmol g−1 and preconcentration factor of 250 fold in less than one minute (t1/2). Common other ions did not interfere except Co(II) which was eliminated by EDTA . The limit of detection (LOD) is 0.1 ng mL−1 and the relative standard deviation (R. S. D.) for 10 replicate measurements at 20 ng mL−1 Pd level was 1.51%. The method was successfully applied for Pd preconcentration in highly concentrated salt solutions and in spiked clay, road dust, scrap and water samples.

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Authors and Affiliations

  1. Department of Chemistry, Industrial Education College, Beni-Suef University, Beni-Suef, 269, Egypt

    Mohamed Mahmoud Hassanien

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  1. Mohamed Mahmoud Hassanien
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Correspondence to Mohamed Mahmoud Hassanien.

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Table S1

Effect of potentially interfering ions (0.01–0.5 mol L−1) on the determination of 100 mL solution of 0.1 µg/mL Pd(II) in presence of 50 mg BMPH-APS (DOC 33 kb)

Table S2

FAAS determination of Pd(II) in spiked water (500 mL), clay, road dust (10 g) and scrap (0.5 g) samples after separation and preconcentration using BMPH-APS (DOC 34 kb)

Fig. S1

Effect of pH on the extraction of palladium. 20 mL of 0.5 µg mL−1 Pd (II) solution, 50.0 mg solid support and stirring time 15 min. (DOC 34 kb)

Fig. S2

The effect of initial Pd(II) concentration (batch mode: 50.0 mg BMPH-APS at pH 2 with shaking time 2 h for 50 ml volume) at room temperature. (DOC 84 kb)

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Hassanien, M.M. FAAS determination of palladium after its selective recovery by silica modified with hydrazone derivative. Microchim Acta 167, 81 (2009). https://doi.org/10.1007/s00604-009-0219-2

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  • DOI: https://doi.org/10.1007/s00604-009-0219-2

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