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Fabrication of Calix[4]pyrrole Nanofilms at the Glassy Carbon Surface and Their Characterization by Spectroscopic, Optic and Electrochemical Methods
(Elsevier Science Sa, 2010) Taner, Bilge; Özcan, Emine; Üstündağ, Zafer; Keskin, Selda; Solak, Ali Osman; Ekşi, Haslet
meso-Octamethylcalix[4]pyrrole (CP) and meso-heptaethylcalix[4]pyrrole-meso-4-aminophenyl (4APCP) modified glassy carbon (GC) electrodes were prepared by the electrochemical oxidation in acetonitrile solution. Binding of the calix[4]pyrroles with the glassy carbon surface was investigated that it is through the etheric linkage revealed from the reflection absorption infrared spectroscopy (RAIRS). Surface films of CP and 4APCP were investigated by cyclic voltammetry (CV), ellipsometry, X-ray photoelectron spectroscopy. RAIRS and the contact angle measurements. The thicknesses of the films were determined by ellipsometry which confirmed that the film was multilayer and homogeneous over the surface. Ellipsometric measurements also provided that the CP and 4APCP film thicknesses were 2.49 nm and 4.58 nm for 6 CV cycle modification, corresponding to 66 mu F/cm(2) and 106 mu F/cm(2) capacitances obtained by CV. The wetting behavior was examined by contact angle measurements and found that the hydrophobicity of the GC-4APCP surface was higher than that of GC-CP, probably due to the aromatic meso substituent present in the former.
Kiral Sensör Olarak Ferrosen Türevli YeniSchiff Bazının Sentezi
(2015) Uçar, Asuman; Fındık, Mükerrem; Bingöl, Haluk; Güler, Ersin; Özcan, Emine
Ferrosen ve ferrosenil bileşikleri enerji ve elektron transferi gerçekleştirebilmesinden dolayı floresans çalışmalarında yaygın olarak kullanılmıştır (1). Yüksek seçiciliğin yanında analitik, biyolojik, klinik ve biyokimya alanlarında potansiyel uygulamaları nedeniyle enantiyoseçici floresans sensör çalışmaları literatürlerde yer almaktadır (2). Aminoasitler hem doğal kiral moleküller olduğu için hem de amid bağları mükemmel hidrojen bağı yaptıkları için kiral reseptor eldesinde önem taşımaktadırlar (3). Bu çalışmada kiral yapıda olan 3 bileşiği sentezlenmiş ve floresans özellikleri çalışılmıştır. Bu bileşiğin çeşitli kiral aminoasitlerle (D- Metiyonine, L- Metiyonine, DAlanin, L-Alanin, D-Valin, L-Valin, L-Serin, D-Serin, D-Histidin, L-Histidin, D-Sistein, LSistein D- Treonin, L- Treonin) etkileşimi sonucu floresans değişimleri incelendiğinde D-metiyonine karşı gözle görülür bir değişim söz konusuyken incelenen diğer amino asitlere karşı bu artışın mevcut olmadığı görülmüştür. Bu sonuçlar sentezlenen bileşiğin D-metiyonin enantioselektif tanıması için kullanışlı bir sensor olduğunu göstermektedir.
Modification of glassy carbon electrode by the electrochemical oxidation of 3-aminophenylcalix[4]pyrrole in nonaqueous media
(Wiley, 2012) Taner, Bilge; Deveci, Pervin; Üstündağ, Zafer; Keskin, Selda; Özcan, Emine; Solak, Ali Osman
3-Aminophenylcalix[4]pyrrole (3APCP) was grafted to a glassy carbon (GC) surface during the electrochemical oxidation process in 0.1 M tetrabutylammoniumtetra-fluoroborate (TBATFB) containing acetonitrile solution. The presence of a surface film was confirmed electrochemically by comparing voltammograms of dopamine and ferricyanide redox probes at the bare and modified electrodes. Reflection-absorption infrared spectroscopy (RAIRS), XPS, atomic force microscopy (AFM), ellipsometry and the contact angle measurements were also employed to characterize 3APCP film on GC electrode. RAIRS analysis revealed that calix[4]pyrrole was bonded to the glassy carbon surface via the etheric linkage. The stability of the modified GC electrode was also studied. Copyright (C) 2011 John Wiley & Sons, Ltd.
Novel Bioactive Vic-Dioxime Ligand Containing Piperazine Moiety: Synthesis, X-ray Crystallographic Studies, 2D NMR Applications and Complexation With Ni(II)
(Pergamon-Elsevier Science Ltd, 2010) Yılmaz, Aytek; Taner, Bilge; Deveci, Pervin; Yılmaz Obalı, Aslıhan; Arslan, Uğur; Şahin, Ertan; Uçan, H. İsmet; Özcan, Emine
A new vic-dioxime ligand bearing an important pharmacophore substituent, anti-1-(4-benzylpiperazine-1-yl) phenylglyoxime (LH2) (Scheme 1), has been synthesized and its nickel(II) complex was obtained by the reaction of NiCl2 center dot 6H(2)O and the ligand. The characterization of the newly formed compounds was performed by elemental analysis, FT-IR, 1D NMR (H-1, C-13, DEPT), 2D NMR (HMBC), ESI mass-spectrometry, TG/DTA, X-ray crystallography. The antibacterial activity was also studied against Staphylococcus aureus ATCC 25923, Streptococcus mutans RSHM 676, Enterococcus faecalis ATCC 29212, Lactobacillus acidophilus RSHM 06029, Escherichia coli ATCC 25922, E. coli ATCC 35218, Pseudomonas aeruginosa ATCC 27853. The antimicrobial test results indicated that all the compounds have mild antibacterial activity against both Gram negative and Gram positive bacterial species.
Radyo frekans tanımlama sistemi ve bir uygulaması
(Selçuk Üniversitesi Fen Bilimleri Enstitüsü, 2013-06-07) Özcan, Emine; Ülker, Erkan
Kimlik ve otomatik tanımlama işlemleri son yıllarda birçok endüstri alanında kullanılmaya başlanmıştır. Bu sistemlerden biriside RFID sistemleridir. RFID teknolojisi günümüzde elektronik pasaport uygulamalarında, lojistik uygulamalarda, askeri uygulamalarda, sağlık uygulamalarında, kimlik tanımlama sistemlerinde kullanılmaktadır. Gelişen yapısıyla birlikte geleceğin teknolojisi de olacaktır. RFID teknolojisinin otomasyonda kullanılması ile işlem maliyetleri büyük ölçüde düşmüştür. Bu konuda geniş bir araştırma yapılarak, RFID teknolojisi kriterleri belirlenmiş ve bir uygulaması yapılmıştır. Bu tez çalışmasında ?elektronik para ve kimlik kartı ? uygulaması yapılmıştır. Çalışma iki ana bölümden oluşmaktadır. İlk bölümde RFID sistemi ve teknolojisi anlatılmış, ikinci bölümde yapılan uygulama tanıtılmıştır. İkinci bölüm içerisinde kullanılmış olan demo kitin tanıtımı ve geliştirilen yazılım sunulmuştur. Çalışmada 13,56 MHz, yüksek frekansta çalışan pasif mifare kartlar ve SMX1300 demo kiti kullanılmıştır. Visual Studio 2010 NET. platformunda C# yazılım dilinde RFID teknolojisi kullanılarak kimlik kartı ve bu kart ile ürün satın alımı yapılabilen bir elektronik para yazılımı geliştirilmiştir.
Synthesis and Complex-Formation of New Unsymmetrical Vic-Dioximes
(MARCEL DEKKER INC, 1995) Pekacar, Ah İhsan; Özcan, Emine
anti-p-Chlorophenylchloroglyoxime (C8H6 Cl-2 N2O2) has been synthesized by chlorination of anti-p-chlorophenylglyoxime. The reaction of C8H6Cl2N2O2 with aryl- or arylalkylamines in ethanol between -10 degrees C and -15 degrees C gives unsymmetrical vic-dioximes, namely, anilino-p-chlorophenylglyoxime (L(1)H(2)), benzylamino-p-chlorophenylglyoxime (L(2)H(2)), p-toluidino-p-chlorophenylglyoxime (L(3)H(2)), p-anisidino-p-chlorophenylglyoxime (L(4)H(2)). The Ni(II) and Cu(II) complexes of these ligands are square-planar while the Co(II) complexes are octahedral with water molecules as axial ligands. H-1 NMR, IR and UV-vis data are given.
Synthesis and Complex-Formation of Substituted Aminoglyoximes of Unsymmetrical Vic-Dioximes
(TAYLOR & FRANCIS INC, 1994) Sevindir, Cahit H.; Mirzaoğlu, Ramazan; Özcan, Emine; Ertul, Şeref; Güler, Ersin
Three new substituted aminoglyoximes, p-chloroanilinoglyoxime (p-CAGH2), o-chloroanilinoglyoxime (o-CAGH2), M-chloroanilinoglyoxime (M-CAGH2) have been synthesized from anti-chloroglyoxime (CPGH2) and the corresponding substituted amines. The Ni(II) and Cu(II) complexes of these ligands are square-planer while the Co(II) complexes are octahedral with water molecules as axial ligands. H-1-NMR, mass, IR spectra and elemental analyses data of the new compounds are given.
The Synthesis and Ni(II), Co(II), Cu(II), Cd(II), and Zn(II) Complexes of Two New Unsymmetrical vic-Dioximes
(MARCEL DEKKER INC, 2001) Özcan, Emine; Karapınar, Emin; Karapınar, Nazan
Two new substituted aminoglyoximes, N-(4-ethylphenyl)amino-amphi-glyoxime [(LH2)-H-1] and N-(4-ethylphenyl)amino-anti-glyoxime [(LH2)-H-2], have been synthesized from amphi-chloroglyoxime and anti-chloroglyoxime and 4-ethylanilin. The preparation of nickel(II), cobalt(II), copper(H), zinc(II) and cadmium(II) complexes of the amphi- and anti-isomers of these ligands are described. All of these complexes are insoluble in common solvents. IR spectra and elemental analyses data of these complexes are given. Also, mass and H-1 NMR spectra of these ligands are presented.
The Synthesis and Ni(Ii), Co(Ii), Cu(Ii), Zn(Ii), Cd(Ii) and Uo2(Vi) Complexes of N,N'-Bis(2-tolyl)Diaminoglyoxime and N,N'-Bis(4-tolyl)Diaminoglyoxime
(MARCEL DEKKER INC, 1995) Mercimek, Bedrettin; Özcan, Emine; Pekacar, All İhsan
N,N'-Bis(2-toyl)diaminoglyoxime (L(1)H(2)) and N,N'-bis(4-tolyl)diaminoglyoxime (L(2)H(2)) have been prepared from anti-dichloroglyoxime with o-toluidine and p-toluidine in ethanol. The complexes of these vic-dioximes with Ni(II), Co(II), Cu(II), Zn(II), Cd(II) and UO2(VI) metal ions have been investigated. The nickel(II), cobalt(ll) and copper(ll) complexes of the ligands have a metal-ligand ratio of 1:2 and the ligand oo-ordinates through the N atoms, as do most of the vic-dioximes. [Zn(LH)Cl(O-2)] and [Cd(LH)CI(H2O)] (LH(2) = L(1)H(2) or L(2)H(2)) form six-membered chelate rings and co-ordinate through N and O atoms. LH(2) reacts with UO2(CH3COO)(2) . 2H(2)O to give binuclear complexes with a metal-ligand ratio of 1:1. Their structures were identified by elemental analyses and H-1 NMR, IR, UV-visible spectroscopy, respectively.
Synthesis of 4 New Substituted Arylaminoglyoximes and Their Complexes With Copper(Ii), Nickel(Ii), Cobalt(Ii), and Palladium(Ii)
(MARCEL DEKKER INC, 1988) Özcan, Emine; Mirzaoğlu, Ramazan
Four new substituted aminoglyoximes, N-(4-sulfamido- phenyl) glyoxime (SAGH?), N-(4-nitrophenyl) aminoglyoxime (NGH), N-(4-tolyl) aminoglyoxime (PTGH?) and N-(2-tolyl) aminoglyoxime (OTGH2) have been synthesized from anti- chloroglyoxime and the corresponding substituted amines. All these dioximes are in the trans-anti-form according to IR and NMR data. The complexes of these four ligands with Cu(II), Ni(II), Co(II) and Pd(II) are square planar H-bridged structures with a metal-ligand ratio of 1:2, except the Cu(II) complex of SAGH, where the metal-ligand ratio is 1:1. In the case of NGH?, the 4-nitrophenylamino group is replaced by the -NH2 group when Pdcl? dissolved in conc. ammonium hydroxide was used to prepare the palladium (II) complex. 1H-NMR, IR and UV-visible data of the new compounds are given.
The Synthesis of Five New bis(Amino-p tolylglyoximes) and Their Polymeric Metal Complexes
(MARCEL DEKKER INC, 1992) Sevindir, Cahit H.; Özcan, Emine; Mirzaoğlu, Ramazan
In this study, five new bis(amino-p-tolylglyoximes), 1,1'-diphenylethylene-4,4'-bis(amino-p-tolylglyoxime) (LH2)-H-1, 1,1'-diphenylmethylene-4,4'-bis(amino-p-tolylglyoxime) (LH2)-H-2, 1,1'-diphenyloxy-4-4'-bis(amino-p-tolylglyoxime) (LH2)-H-3, 1,1'-biphenyl-4,4'-bis(amino-p-tolylglyoxime) (LH2)-H-4 and 1,4-phenylene-bis(amino-p-tolylglyoxime) (LH2)-H-5, have been synthesized from anti-p-tolylchloroglyoxime (PTCGH2) and the corresponding aromatic diamines. Their polymeric complexes with Ni(II), Cu(II) and Co(II) have been obtained. The Ni(II) and Cu(II) complexes of these ligands are square-planar while the Co(II) complexes are octahedral with water molecules as axial ligands. H-1-NMR, IR spectra and elemental analyses data are given.
The Synthesis of Four New Bis(Amino-P-Chlorophenylglyoximes) and Their Polymeric Complexes
(MARCEL DEKKER INC, 1997) Pekacar, Ali İhsan; Mercimek, Bedrettin; Özcan, Emine
In this study, four new bis(amino-p-chlorophenylglyoximes), 1,2-phenylenebis(amino-p-chlorophenylglyoxime) L(1)H(2), 1,5-naphthylenebis(amino-p-chlorophenylglyoxime) L(2)H(2), 3,4-tolylenebis(amino-p-chlorophenylglyoxime) L(3)H(2), and 2,6-pyridylbis(amino-p-chlorophlenylglyoxime) L(4)H(2), have been synthesized from anti-p-chlorophenylchloroglyoxime and the corresponding aromatic diamines. Their polymeric complexes with Ni(II), Co(II) and Cu(II) have been prepered. The Ni(II) and Cu(II) complexes of these ligands have been found to be square-planar, while the Co(II) complexes are octahedral with water molecules as axial ligands. H-1 NMR, AAS, IR, magnetic susceptibility and elemental analytical data of the complexes and ligands are discussed.
Synthesis of N '-(4 '-benzo[15-crown-5]phenylaminoglyoxime and Its Complexes With Copper(Ii), Nickel(Ii), and Cobalt(Ii)
(Marcel Dekker Inc, 2003) Karapınar, Emin; Karapınar, Nazan; Özcan, Emine
N'-(4'-Benzo[15-crown-5]phenylaminoglyoxime (H2L) and the sodium chloride adduct of N'-(4'-benzo[15-crown-5]phenylaminoglyoxime ((H2LNaCl)-Na-.) have been prepared from chlorophenylglyoxime, 4'-aminobenzo[15-crown-5] and sodium bicarbonate or sodium bicarbonate and sodium chloride. Nickel(II), cobalt(II) and copper(II) complexes of H2L and H2L-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. Their IR spectra and elemental analyses are given, together with H-1 NMR spectra of the ligands.
Synthesis of N '-[4 '-Benzo(15-crown-5)]-4-Tolylaminoglyoxime and N '-[4 '-Benzo(15-crown-5)]-4-Chlorophenylaminoglyoxime and Their Complexes With Copper (Ii), Nickel (Ii) and Cobalt (Ii)
(Springer, 2003) Karapınar, Emin; Özcan, Emine
N'-[4'-benzo(15-crown-5)]-4-tolylaminoglyoxime (H2L1), the sodium chloride salt of H2L1 (H2L1.NaCl), N'-[4'-benzo(15-crown-5)]-4-chlorophenylaminoglyoxime (H2L2) and the sodium chloride salt of H2L2 (H2L2.NaCl) have been prepared from p-chlorophenylchloroglyoxime, p-tolylchloroglyoxime, 4'-aminobenzo[15-crown-5] and sodium bicarbonate or sodium bicarbonate and sodium chloride. Nickel (II), cobalt (II) and copper (II) complexes of H2L and H2L.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. Their IR spectra and elemental analyses are given, together with H-1 NMR spectra of the ligands.
Synthesis of Novel Homo and Heterobimetallic Complexes of Ferrocenyl Formazans
(TAYLOR & FRANCIS INC, 1993) Gök, Yaşar; Tüfekçi, Mehmet; Özcan, Emine
l-(~-Carboxyphenyl~-5-~p-hydroxy-~-carboxyphenyl~-3-ferrocenylformazan (HFF) and l-~~-carboxyphenyl~-5-~~-nitro-~-carboxyphenyl~-3- ferrocenylformazan (NFF) have been synthesized by the addition reaction of the diazonium salts of 2-amino-5-hydroxybenzoic acid, 2-amino-5-nitrobenzoic acid and ferrocenaldehyde-2-carboxyphenylhydrazone. The Ni(II), Pd(II), and Fe(I1) complexes of HFF and NFF have also been obtained. The structures of formazans and their transition metal complexes were confirmed by elemental analyses, 'H and 13C-NMR, IR and UV-VIS. spectral data.
Synthesis, Characterization, Thermal and Redox Properties of a Vic-Dioxime and Its Metal Complexes
(TAYLOR & FRANCIS LTD, 2010) Uçar, Asuman; Deveci, Pervin; Taner, Bilge; Fındık, Mükerrem; Bereket, Soner; Özcan, Emine; Solak, Ali Osman
A new vic-dioxime ligand containing benzophenone hydrazone units, N'-(benzophenone hydrazone)glyoxime [LH2] has been prepared from benzophenone hydrazone and anti-chloroglyoxime in absolute ethanol. Mononuclear nickel(II), cobalt(II), copper(II), zinc(II), and cadmium(II) complexes were also synthesized. Ligand and complexes were characterized by elemental analyses, FT-IR, 1H NMR, and 13C NMR spectroscopy, magnetic moments, and DTA/TG techniques. On the basis of the magnetic and spectral evidences a square-planar geometry for Ni(II) and Cu(II) complexes, tetrahedral for Cd(II) and Zn(II) complexes, and octahedral for Co(II) complex were proposed. Redox behaviors of ligand and its complexes were also investigated by cyclic voltammetry at the glassy carbon electrode.
Synthesis, Enhanced Spectroscopic Characterization and Electrochemical Grafting of N-(4-Aminophenyl)aza-18-Crown-6: Application of Dept, Hetcor, Hmbc-Nmr and X-Ray Photoelectron Spectroscopy
(ELSEVIER, 2010) Deveci, Pervin; Taner, Bilge; Üstündağ, Zafer; Özcan, Emine; Solak, Ali Osman; Kılıç, Zeynel
This work describes the synthesis, characterization and electrochemical grafting of N-(4-Aminophenyl)aza-18-Crown-6 (4APA18C6). The key step in the synthesis is the reaction of N-phenylaza-18-crown-6 (PA18C6) with sodium nitrite. The compound, N-(4-nitrosophenyl)aza-18-crown-6 (NOPA18C6) could not be isolated purely from the reaction mixture, but a reduction of the residue with SnCl2 gave the desired aza-crown ether, N-(4-aminophenyl)aza-18-crown-6 (4APA18C6). To confirm its proposed structure detailed characterization techniques such as elemental analysis, FT-IR, H-1 NMR, C-13 NMR, DEPT, HETCOR, HMBC and ESI mass-spectrometry were used. Due to the importance of azacrown compounds in the field of analytical chemistry, in the derivatization of dyes, chemical sensors and ionic extraction, as molecular receptors, grafting of 4APA18C6 on the glassy carbon (GC) surface has been investigated by amine oxidation to gain new insight into the modification area. The oxidation mechanism has been established, and the results are in accordance with the attachment of amines to a glassy carbon surface by cyclic voltammetry. The modification of 4APA18C6 molecules onto the glassy carbon surface was verified by cyclic voltammetry (CV), X-ray photoelectron spectroscopy (XPS) reflection-absorption infrared spectroscopy (RAIRS) and ellipsometry. The film on the GC surface was formed according to the layer-by-layer mechanism and the ellipsometric thickness was obtained around 11.5 +/- 1.1 nm.
Yeni Bir Ferrosen Türevli Schiff Bazının Sentezi ve Zn2/Cd2 İyonlarının Tayininde Sensör Olarak Kullanımı
(2015) Fındık, Mükerrem; Uçar, Asuman; Bingöl, Haluk; Güler, Ersin; Özcan, Emine
Supramoleküler kimyada ağır metallerin tayini için kimyasal sensörlerin geliştirilmesi büyük öneme sahiptir[1]. Bu doğrultuda enerji ve elektron sağladıkları için ferrosen ve türevleri kemosensör olarak floresans çalışmalarında kullanılmaktadır[2,3]. Ağır metal iyonları olan Zn2 ve Cd2 benzer kimyasal özelliklere sahip oldukları için bu iki iyonu birbirinden ayırt etmek için araştırmacılar yeni sensörler sentezlemektedirler. Bu ayırımı yapmak için florimetrik çalışmalar hem basit hem de yüksek hassasiyete sahiptir[4]. Bu çalışmada, yeni bir ferrosen türevli Schiff bazı sentezlendi. Sentezlenen bileşik elementel analiz, FT-IR, 1H NMR ve 13C NMR ile karakterize edildi. Bu bileşik Florimetri kullanılarak bazı alkali, toprak alkali ve ağır geçiş metal iyonları arasından Zn2 ve Cd2 iyonlarının tayini için sensör olarak kullanıldı. Elde edilen veriler sonucunda sentezlenen sensörün Zn2 ve Cd2 iyonlarına karşı iyi bir seçici olduğu tespit edildi.

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