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    Liquid-Liquid Extraction of Transition Metal Cations by Glyoximes and Their Macrocyclic Glyoxime Ether Derivatives
    (HINDAWI PUBLISHING CORPORATION, 2013) Karapinar, Nazan; Karapinar, Emin; Ozcan, Emine
    Liquid-liquid extraction of various alkalis (Li+, Na+, K+, and Cs+), transition metals (Co2+, Ni2+, Cu2+, Zn2+, Cd2+, and Hg2+), and Pb2+ cations with phenylglyoxime (L1), p-tolylglyoxime (L2), N'-(4'-Benzo[15-crown-5]) phenylaminoglyoxime (L3), and N'-(4'-Benzo[15-crown-5])-p-tolylaminoglyoxime (L4) from the aqueous phase into the organic phase was carried out. For comparison, the corresponding two glyoximes and theirmacrocyclic glyoxime ether derivatives were also examined. Crown ether groups having ligands (L3, L4) carry especially Na+ cation from aqueous phase to organic phase. The extraction equilibrium constants (K-ex) for complexes of ligands with Cu2+ and Hg2+ metal picrates between dichloromethane and water have been determined at 25 degrees C. The values of the extraction constants (log K-ex) were determined to be 12.27, 13.37, 12.94, and 12.39 for Cu2+ and 10.29, 10.62, 11.53, and 11.97 for Hg2+ with L1-L4, respectively.
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    Synthesis of N-(4 '-benzo[15-crown-5])thiophenoxyphenylaminoglyoxime and its complexes with some transition metals
    (SPRINGER, 2008) Coskun, Ahmet; Karapinar, Emin
    4-(Chloroacetyl)diphenyl thioether (1) was synthesized from chloroacetyl chloride and diphenyl thioether in the presence of AlCl3 as catalyst in a Friedel-Crafts reaction. Subsequently, its keto oxime (2) and glyoxime (3) derivatives were prepared. N-(4'-Benzo[15-crown-5]thiophenoxyphenylaminoglyoxime (H2L) and its sodium chloride complex (H2L center dot NaCl) were prepared from 4-(thiophenoxy)chlorophenylglyoxime (3), 4'-aminobenzo[15-crown-5] and sodium bicarbonate or sodium bicarbonate and sodium chloride. Ni(II), Co(II) and Cu(II) complexes of H2L and H2L center dot NaCl have a metal-ligand ratio of 1:2 and the ligand coordinates through the two N atoms, as do most of the vic-dioximes. The BF2-capped Ni(II) mononuclear complex of the vic-dioxime was prepared. The macrocyclic ligands and their transition metal complexes were characterized on the basis of FT-IR, H-1 NMR, C-13 NMR spectroscopy and elemental analyses data.
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    Synthesis, characterization and extraction properties of four unsymmetrical vic-dioximes and their complexes with nickel(II), cobalt(II) and copper(II)
    (TAYLOR & FRANCIS INC, 2007) Karapinar, Emin; Karapinar, Nazan; Ozcan, Emine; Coskun, Ahmet
    Four new unsymmetrical vic-dioximes: [(LH2)-H-1] N-(4-acetanilidyl) amino-amphi-glyoxime, [(LH2)-H-2] N-(4-acetanilidyl) amino-anti-glyoxime, [(LH2)-H-3] N-(2-thiazolyl) amino-amphi-glyoxime and [(LH2)-H-4] N-(2-thiazolyl) amino-anti-glyoxime were prepared by the reaction of amphi-chloroglyoxime and anti-chloroglyoxime with 4-aminoacetanilide and 2-aminothiazol in absolute ethanol. The preparation Ni(II), Co(II), and Cu(II) complexes of the amphi-and anti-isomers of these ligands are described. The ligands and their complexes were characterized by elemental analyses, IR, mass, H-1 and C-13 NMR spectra and magnetic susceptibility measurements. Ligands complexing properties were studied by the liquid-liquid extraction of selected alkali (Li+, Na+, K+, Cs+) and transition metals (Co2+, Ni2+, Cu2+, Zn2+, Cd2+, Hg2+, Pb2+). It has been observed that all ligands show a high affinity to Cu2+ and Hg2+ ions, where as almost no affinity to alkali metals. The extraction equilibrium constants (Kex) for complexes of ligands with Cu2+ and Hg2+ metal picrates between dichloromethane and water have been determined at 25 degrees C.
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    Thermal Degradation Behaviour of Ni(II) Complex of 3,4-Methylenedioxaphenylaminoglyoxime
    (HINDAWI PUBLISHING CORPORATION, 2013) Karapinar, Emin; Gubbuk, Ilkay Hilal; Taner, Bilge; Deveci, Pervin; Ozcan, Emine
    Thermal degradation behaviour of the Ni(II) complex of 3,4-methylenedioxaphenylaminoglyoxime was investigated by TG, DTA, and DTG at a heating rate of 10 degrees C min(-1) under dinitrogen. The acquired experimental data shows that the complex is thermally stable up to 541 K. The pyrolytic decomposition process occurs by melting metal complex and metal oxide remains as final product. The energies of the reactions involved and the mechanism of decomposition at each stage have been examined. The values of kinetic parameters such as activation energy (E), preexponential factor (A) and thermodynamic parameters such as enthalpy (Delta H), entropy (Delta S), and Gibbs free energy (Delta G) are also evaluated.