This present study describes a pencil graphite electrode surface covered with Cu(II) and Fe(III) complexes based on Salophen derivative Schiff bases in acetonitrile solution containing LiClO4 as a supporting electrolyte. Cyclic voltammetry method was used for the surface modification procedure with 25 cycle at a sweep rate of 50 mV s−1. Some characterization methods were used to identify of the prepared modified surfaces including cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), Ultraviolet‐visible Spectroscopy (UV‐Vis), and Scanning Electron Microscopy/Energy Dispersive X‐ray Spectroscopy (SEM/SEM‐EDX). The catalytic activity of these modified surfaces on the electrochemical oxidation of catechol (CC) was investigated and they compared with each other. The results demonstrated that these modified electrodes showed perfect electrocatalytic activity on the catechol determination, however the modified electrode prepared with the Cu(II) complex has higher catalytic activity than this prepared with the Fe(III) complex thanks to its the lower detection limit.
In this study, poly (pyrrole‐co‐o‐anisidine)/chitosan composite (Cs) films were prepared by cyclic voltammetry technique on platinum electrode using different pyrrole and o‐anisidine mole ratios. Immobilization process was accomplished in CoII‐(N,N′‐bis(salicylidene)‐2‐aminobenzylamine)(CoL) dissolved 0.15 M acetonitrile‐LiClO4 solution by cyclic voltammetry technique at 0.2–2.0 V potential range. Three electrode methods were applied in all electrochemical studies. After immobilization process, the characterizations of the electro catalytic surfaces (Cs−CoL−Pt) were carried out by cyclic voltammetry and SEM images. The SEM images clearly indicated that the [CoL] complex is immobilized onto composite films. The electrocatalytic activity of the modified electrodes on the catechol was investigated using buffer solutions of different pH values. The results of catalytic studies revealed that, pH=10 buffer solution was the optimal solution and 1 : 1 Cs−CoL−Pt electrode was the best electrode for catechol oxidation. In square wave voltammetry measurements using this electrode, two linear working ranges were determined. The linear response ranges for catechol determination were found as 3.0 μM–6.0 μM and 16 μM–80 μM for the first and the second linear working ranges, respectively, with 1.1 μM detection limit.
ÖZBu çalışmada, poli(pirol-ko-o-anisidin)kitosan kompozit filmleri pirol ve o-anisidinin farklı monomer mol oranlarındaki çözeltilerinde (pirol : o-anisidin; 7:3, 1:1 ve 3:7) elektrokimyasal olarak sentezlendiler. Kompozit filmlerin sentezi dönüşümlü voltameri tekniği ile gerçekleştirildi. Kompozit filmleri FT-IR, dönüşümlü voltametri ve SEM teknikleri ile karakterize edildi. SEM analiz sonuçları o-anisidin oranı arttıkça kompozit filmlerin parçacık büyüklüklerinin giderek azaldığını ve oran daha da arttıkça düz bir yüzey halini aldığını göstermiştir. Ayrıca elektrokimyasal çalışmalar 3:7 oranındaki kompozit filminin elektrokimyasal olarak iyi bir kararlılığa sahip olduğunu ortaya koymuştur. N,Nʹ-bis(salisiliden)-2aminobenzilaminonikel(II) [NiL] kompleksinin kompozit film yüzeylerine immobilizasyon işlemi 0.15 M asetonitril-LiClO4 çözeltisinde 0.2-2.0 V potansiyel aralığında dönüşümlü voltametri tekniği ile gerçekleştirilmiştir. Schiff bazı metal kompleksinin kompozit filmlerinin yüzeyine immobilizasyonunun gerçekleştiği SEM görüntülerinden belirlenmiştir. SEM görüntüleri Schiff bazı metal kompleksinin kompozit film yüzeylerine immobilizasyonunun açık bir şekilde gerçekleştiğini göstermiştir. Metal kompleksi immobilizayonu gerçekleştirilmiş poli(pirol-ko-o-anisidin)/kitosan kompozit filmlerinin elektrokatalitik aktivite çalışmaları NO2iyonu için denenmiştir. Elektrokatalitik çalışmalar 3:7 oranındaki modifiye kompozit filminin NO2iyonunun katalizlenmesinde oldukça yüksek bir aktiviteye sahip olduğunu göstermiştir.
Anahtar Kelimeler: Pirol, o-anisidin, Kitosan, Kompozit, Elektrokimyasal Sentez
Immobilization of N,N'-bis(salicylidene)-2-aminobenzylaminonickel(II) complex on surfaces of poly(pyrrole-co-o-anisidine)/chitosan composite films and determination of NO2ion ABSTRACTIn this study, poly(pyrrole-co-o-anisidine)/chitosan composite films were electrochemically synthesized in various monomers feed ratio (pyrrole : o-anisidine; 7:3, 1:1 and 3:7) of pyrrole and o-anisidine on the platinum electrode. Electrochemical synthesis of the composite films was carried out via cyclic voltammetry technique. They were characterized by FT-IR, cyclic voltammetry, SEM. The SEM results indicated that the particle size of the composite decreases with increasing o-anisidine ratio and the films became more likely to be smooth morphology. Also, electrochemical studies exhibited that the 3:7 composite film has good electrochemical stability. Immobilization process of N,Nʹ-bis(salicylidene)-2aminobenzylaminonickel(II) [NiL] complex on the composite films was achieved in 0.15 M acetonitrile-LiClO4 via cyclic voltammetry technique at 0.2-2.0 V potential range. The immobilization of the Schiff
In this study; poly (o-amino benzyl alcohol) and poly (o-amino benzyl alcoholco-o-anisidine) copolymer films were electrochemically synthesized by cyclic voltammetry technique on the platinum electrode. The synthesis of copolymer films was achieved in various monomers feed ratio (o-amino benzyl alcohol: o-anisidine; 8:2, 1:1, 2:8) of o-amino benzyl alcohol and o-anisidine. Different solution types were tested in aqueous and non-aqueous media, especially during the synthesis process, as the electrolyte medium. As a result of the experiments, it was determined that sulfuric acid solution was the most suitable solution for both homopolymer and copolymer film growth. Homopolymer and copolymer samples were characterized by FT-IR, cyclic voltammetry (CV), SEM, digital images and TGA/DTA techniques. The CV, SEM and digital images results indicated that the solution which has high ratio of monomer is more effective in copolymer film synthesis mechanism. TGA results showed that the 1:1 copolymer film had higher thermal stability than the films at other monomer ratios. Also, electrochemical studies exhibited that the copolymer film in 1:1 ratio is partially more electrochemically stable than other copolymer films.
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