Extraction chromatographic method of preconcentration, estimation and concomitant separation of vanadium (IV) with silica gel-versatic 10 composite.

A selective method has been developed for the extraction chromatographic separation of V(IV) with SSG-V-10 composite. V(IV) was quantitatively extracted at pH 5.0-6.0, and its loading has been confirmed by EDAX. XRD studies indicate that the SSG network does not get influenced by impregnation with V-10 or by the sorption of V(IV) on the surface of SSG-V-10 composite. The binding between SSG and V-10 is a hydrophobic interaction only, and it takes place at the surface of the hydrophobic SSG. TGA-DTA analysis indicates its thermal stability up to 45°C. The exchange capacity (1.65 meq of H(+) g(-1)), break-through capacity (34.5 mg g(-1)) and column efficiency (360) of the extractor have been rationalized by Brunauer-Emmett-Teller analysis (SA = 149.46 m(2) g(-1) and PV = 0.2001 mL g(-1) at a relative pressure of 0.9-1.0). The sorption process was endothermic (ΔH = 12.63 kJ mol(-1)), entropy gaining (ΔS = 0.271 kJ mol(-1) K(-1)) and spontaneous (ΔG = -68.241 kJ mol(-1)) in nature. Preconcentration factor has been optimized at 182.3 ± 0.2. Formation constants (Kf) of the metal centers [Zn(II) (0.6 × 10(3)), Cd(II) (0.9 × 10(4)), Pb(II) (0.6 × 10(5)), Cu(II) (0.2 × 10(5)), Al(III) (6.2 × 10(5)), Ga(III) (4.2 × 10(5)), Hg(II) (2.2 × 10(6)), Bi(III) (6.2 × 10(6)), Tl(III) (8.9 × 10(6)), Zr(IV) (6.8 × 10(9)), Fe(III) (0.9 × 10(9)) and V(IV) (0.8 × 10(6))] have been determined. The desorption constants Kdesorption (1.9 × 10(-2)) and [Formula: see text] have been determined. Rf values and selectivity factors for diverse metal ions have been determined. V(IV) has been separated from the synthetic and real samples containing its congeners. A plausible mechanism for the extraction of V(IV) has been suggested.