We combined the ion-imprinting technique and the binding ability of Fe 3+ ions to organosmectite to create the inorgano-organo Fe 3+ ions imprinted polymer-nanocomposite traps with the goal of preparing a solid phase that has high selectivity for Fe 3+ ions. In the first step, the intercalation of quartamine cations was conducted by an ion-exchange process between the smectite host and an aqueous quartamine solution and Fe 3+ ions were complexed with methacryloylamidoantipyrine (MAAP). In the second step, quartamine cations were exchanged with a preorganized metal-chelate complex monomer for the preparation of polymer nanocomposite traps based on the intersurface ion-imprinting. After that, the template ions (i.e., Fe 3+ ) were removed using 4.0 M HNO 3 solution. Fe 3+ -imprinted nanocomposites were characterized by Fourier transform infrared (FTIR), X-ray diffraction (XRD), swelling studies, and elemental analysis. Maximum binding capacity, optimum pH, and equilibrium binding time were found to be 78.5 mg/g, pH 3.0, and 10 min, respectively. The relative selectivity coefficients of the imprinted nanocomposite traps for Fe 3+ /Al 3+ , Fe 3+ /Cu 2+ , Fe 3+ / Co 2+ , and Fe 3+ /Zn 2+ were 5. 28, 11.4, 15.8, and 72.6 times greater than the nonimprinted nanocomposites, respectively. The Fe 3+ -imprinted nanocomposite traps could be used many times without decreasing in their adsorption capacities significantly.
The novel mesoporous silica-supported bis(diazo-azomethine) compounds have been synthesized and characterized successively. In the first step, 1,3-phenylenedimethanamine and 4,4′-diaminodiphenylmethane were diazotized, and the obtained bis(diazonium) cations were coupled with 2,4-dihydroxybenzaldehyde. The synthesized bis(diazo-carbonyl) compounds, 5,5′-((1,3-phenylenebis(methylene))bis(diazene-2,1-diyl))bis(2,4-dihydroxybenzaldehyde) (A1) and 5,5′-((methylenebis(4,1-phenylene)) bis(diazene-2,1-diyl))bis(2,4-dihydroxybenzaldehyde) (A2) were chemically supported on amino-modified silica-gel (as L1 and L2). Elemental analysis, liquid chromatography-mass spectroscopy, liquid-phase NMR ( 1 H and 13 C) and solid-phase NMR (CP-MAS 29 Si and 13 C), FT-IR, TG/DTA, scanning electron microscopy and energy-dispersive X-ray spectroscopy techniques were used for characterizations of all the synthesized compounds. The syringe and batch techniques were applied for the solid-phase extraction properties of Pb(II), Cu(II), Cd(II) and Cr(III) ions using an inductively coupled plasma-atomic emission spectroscopy instrument. The recoveries of Pb(II), Cu(II), Cd(II) and Cr(III) ions have been achieved to 95-99% with the (RSDs) of ± 2-3% in optimum conditions.
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