Synthesis,characterization and solid‐phase extraction properties of novel bis(diazo‐azomethine) ligands supported on mesoporous silica |
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Authors: | Serhan Uruş Muharrem Karabörk Hüseyin Köksal |
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Institution: | 1. Chemistry Department, Faculty of Science and Letters, Kahramanmara? Süt?ü ?mam University, Kahramanmara?, Turkey;2. Research and Development Centre for University‐Industry‐Public Relations (üSK?M), Kahramanmara? Süt?ü ?mam University, Kahramanmara?, Turkey |
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Abstract: | 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 (1H and 13C) and solid‐phase NMR (CP‐MAS 29Si and 13C), 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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Keywords: | azomethine diazo imine Schiff base silica solid‐phase extraction |
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