Abstract.
2,3-Dihydroxypyridine loaded (via –N=N–linker) Amberlite XAD-2 (AXAD-2-DHP) was prepared and characterized by elemental analyses, TGA and FT-IR spectra. It (1 g packed in a column of 1 cm diameter; surface area 135.5 m2 g−1) was found to be an effective solid phase sorbent for enriching Zn2+, Mn2+, Ni2+, Pb2+, Cd2+, Cu2+, Fe3+ and Co2+ at pH 3.5 to 7.0 using flow rates between 1.0–5.0 mL min−1. For desorption (recovery 97.0–99.8%) of the metal ions, 8 to 10 mL of 2.0 mol L−1 HCl or 1.5 mol L−1 HNO3 at a flow rate of between 2.0 and 4.0 mL min−1 were found most suitable. The t1/2 (time for 50% sorption) is between 2 and 10 min when a 50 mL solution (containing a total amount of metal of 2 mg) was equilibrated with 0.5 g of resin. Sorption of all metal ions except Pb2+ follows the Langmuir model, whereas for Pb the data fits with the Freundlich model. The sorption capacity is between 60.7 (for Cd) and 406.7 (for Cu) µmol g−1. The resin can withstand an acid concentration of ≤6 mol L−1 and can be reused for thirty cycles of sorption–desorption. The preconcentration factor varies between 100 and 300. For Cd, Ni and Cu the sorption capacity of 2,3-dihydroxypyridine loaded cellulose is lower than that of the present resin. The tolerance limits of electrolytes, humic acid, complexing agents, Ca2+ and Mg2+ in the enrichment of all metal ions are reported. The limits of detection are 3.88, 5.37, 8.72, 13.88, 4.71, 1.24, 0.59 and 0.30 µg L−1 for Zn2+, Mn2+, Ni2+, Pb2+, Cd2+, Cu2+, Fe3+ and Co2+, respectively. The calibration curves for flame AAS determination were linear in the ranges 0.018–1.0, 0.067–5.0, 0.2–5.0, 0.9–20, 0.028–2.0, 0.077–5.0, 0.19–10 and 0.1–3.5 µg mL−1, respectively. All the eight metal ions in river and synthetic water samples, Co in vitamin tablets and Zn in milk samples have been quantitatively enriched with Amberlite XAD-2-DHP and determined by flame atomic absorption spectrometry.
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Venkatesh, G., Jain, A. & Singh, A. 2,3-Dihydroxypyridine Loaded Amberlite XAD-2 (AXAD-2-DHP): Preparation, Sorption–Desorption Equilibria with Metal Ions, and Applications in Quantitative Metal Ion Enrichment from Water, Milk and Vitamin Samples. Microchim Acta 149, 213–221 (2005). https://doi.org/10.1007/s00604-005-0320-0
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DOI: https://doi.org/10.1007/s00604-005-0320-0