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    Phenanthroline derivatives electrochemically grafted to glassy carbon for Cu(II) ion detection
    (ELSEVIER SCIENCE SA, 2012) Oztekin, Yasemin; Yazicigil, Zafer; Solak, Ali Osman; Ustundag, Zafer; Okumus, Aytug; Kilic, Zeynel; Ramanaviciene, Almira
    New sensing platform based on modified glassy carbon (GC) suitable for design of heavy metal-ion sensor is reported in this study. GC-based electrodes were electrochemically modified by poly-5-nitro-1,10-phenanthroline (poly-5NP) and poly-5-amino, 6-nitro-1,10-phenanthroline (poly-5A6NP) layers. Grafting of electrochemically formed poly-5NP and poly-5A6NP layers at the GC electrode surface was confirmed by electrochemical reduction of nitro groups into amine groups. Presence of grafted poly-5NP and poly-5A6NP layers and formation of their reduced forms on the GC electrode surface were verified by cyclic voltammetry, electrochemical impedance spectroscopy, contact angle measurements, ellipsometry and X-ray photoelectron spectroscopy. The applicability of poly-5NP- and poly-5A6NP-functionalized carbon surfaces for the determination of Cu(II) ions was demonstrated by formation of complexes between GC-grafted poly-5NP and poly-5A6NP layers and Cu(II) ions. (C) 2012 Elsevier B.V. All rights reserved.
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    Surface modification and characterization of phenanthroline nanofilms on carbon substrate
    (WILEY, 2011) Oztekin, Yasemin; Yazicigil, Zafer; Solak, Ali Osman; Ustundag, Zafer; Kilic, Zeynel; Bilge, Selen
    Modification of glassy carbon (GC) surfaces with phenanthroline derivatives (PDs) such as 5-amino-1,10-phenanthroline (5AP) and 5,6-diamino-1,10-phenanthroline (56DAP) is described in this study. Surface modification experiments were performed by cyclic voltammetry (CV) scanning from +1.2 to +2.7 V at scan rate of 100 mV/s applying 30 potential scans in acetonitrile (CH3CN) containing 1 mMPDs and 100 mM tetrabutylammoniumtetrafluoroborate (TBATFB). The presence of PDs on GC electrode was confirmed using CV, electrochemical impedance spectroscopy (EIS), contact angle measurements and ellipsometry and comparing with the results of bare GC electrode. A mechanism was proposed for the electrochemical modification of the GC electrode surface with PDs. The structure of the 5AP and 56DAP films was also discussed in the light of electrochemical and spectroscopic data. The complex-forming ability of the modified surfaces against metal cations was investigated by square-wave voltammetry (SWV). It was shown that surfaces having 1,10-phenanthroline ligands with different functional groups were quite useful for the determination of transition metal ions. Copyright (C) 2010 John Wiley & Sons, Ltd.
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    Synthesis and structural and electrochemical characterization of novel macrocyclic vic-dioxime ligand and its mononuclear transition and nontransition metal complexes
    (SCIENTIFIC TECHNICAL RESEARCH COUNCIL TURKEY-TUBITAK, 2012) Deveci, Pervin; Taner, Bilge; Kilic, Zeynel; Solak, Ali Osman; Ozcan, Emine
    The reaction of N-(4-aminophenyl)aza-15-crown-5 (1) with anti-chlorophenylglyoxime (2) produces a novel azacrown ether containing vic-dioxime, N-(4-aminophenyl)aza-15-crown-5-phenylglyoxime (LH2). LH2 reacts with Ni(II), Cu(II), Co(II), Cd(II), and Zn(II) ions to yield the mononuclear transition and nontransition metal complexes [M(LH)(2)] (M = Ni and Cu), [M(LH)(2) (H2O)(2)] (M = Co), and [M(LH)(H2O) (Cl)] (M = Cd and Zn). The structural features of LH2 were studied using several techniques including elemental analysis. Fourier transform infrared spectroscopy (FT-IR,), ultraviolet visible (UV-Vis), mass spectrometry (MS), 1-dimensional (1D) H-1-NMR and (CNMR)-C-13, distortionless enhancement by polarization transfer (DEPT) 2-dimensional (2D) heteronuclear single-quantum coherence (HSQC), and heteronuclear multiple-bond correlation (HMBC) techniques. The structures of the complexes were confirmed by elemental analyses and with the use of magnetic susceptibility measurements, MS, UV-Vis, FT-IR, H-1-NMR and C-13-NMR techniques. The redox behaviors of the ligand and its Complexes were verified with cyclic voltammetry (CV) at a. glassy carbon (GC) electrode in 0.1 M tetrabutylammoniumtetrafluoroborate (TBATFB) in dimethyl sulfoxide (DMSO).
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    Synthesis of some azacrown derivatives and fabrication of their nanofilms on the glassy carbon surface
    (SPRINGER, 2012) Deveci, Pervin; Taner, Bilge; Ustundag, Zafer; Kilic, Zeynel; Solak, Ali Osman; Ozcan, Emine
    The modification of N-phenyl-aza-15-crown-5 (PA15C5) and N-(4-aminophenyl)-aza-15-crown-5 (4APA15C5) on glassy carbon (GC) electrode was performed by the electrochemical oxidation of the corresponding azacrown derivatives in anhydrous acetonitrile media. The electrochemical behavior of the resulting modified GC electrode was investigated in the presence of electroactive redox probes and these results, together with the X-ray photoelectron spectroscopy (XPS) and reflection-absorption infrared spectroscopy were used to confirm the attachment of these molecules onto the GC surface. The ellipsometric thicknesses of PA15C5 and 4APA15C5 films at the GC surface was obtained around 9.28 +/- 0.40 and 10.50 +/- 1.10 nm, respectively. Azacrown modified nanoscale surfaces serve as alkali metal sensor specific for their cavity in the crown ring.
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    Synthesis, electrochemical and structural characterization of novel azacrown ether containing macrocyclic redox-active vic-dioxime ligand and its mononuclear transition metal complexes: Application of DEPT, HSQC, HMBC-NMR and cyclic voltammetry
    (PERGAMON-ELSEVIER SCIENCE LTD, 2011) Deveci, Pervin; Taner, Bilge; Kilic, Zeynel; Solak, Ali Osman; Arslan, Ugur; Ozcan, Emine
    This paper presents a new azacrown containing vic-dioxime: anti-N-(4-aminophenyl)aza-15-crown-5-glyoxime (LH2), and its mononuclear nickel(II), copper(II), cobalt(II), cadmium(II) and zinc(II) complexes. The azacrown moieties appended at the periphery of the oxime provide solubility for the vic-dioxime ligand and complexes in common organic solvents. The mononuclear M(LH)(2) (M = Ni and Cu), M(LH)(2)(H2O)(2) (M = Co) and [M(LH)(H2O)(Cl)] (M = Cd and Zn) complexes have been obtained with the metal:ligand ratios of 1:2 and 1:1. The structure of the ligand is confirmed by elemental analysis, Fourier transform infrared (FT-IR), ultraviolet-visible (UV-Vis), mass spectrometry (MS), one-dimensional (1D) H-1, C-13 NMR, distortionless enhancement by polarization transfer (DEPT) and two-dimensional (2D) heteronuclear single quantum coherence (HSQC) and heteronuclear multiple bond correlation (HMBC) techniques. The structures of the complexes are confirmed by elemental analyses, MS, UV-Vis, FT-IR and H-1, C-13 NMR techniques. Redox behaviors of the ligand and its complexes have been investigated by cyclic voltammetry at the glassy carbon electrode in 0.1 M TBATFB in DMSO. The antibacterial activity was studied against Staphylococcus aureus ATCC 29213, Streptococcus mutans RSHM 676. Enterococcus faecalis ATCC 29212, Lactobacillus acidophilus RSHM 06029, Escherichia coli ATCC 25922, Pseudomonas aeruginosa ATCC 27853. The antimicrobial test results indicate that all the complexes have low levels of antibacterial activity against both Gram negative and Gram positive bacterial species. (C) 2011 Elsevier Ltd. All rights reserved.