Diazonyum Tuzu Kullanılarak Elektrokimyasal Olarak ModifiyeEdilmiş Karbon Kompozit Elektrot

Karbon kompozit termoplastik elektrotlar (TPE'ler), grafit, termoplastik bağlayıcı ve çözücü kullanılarak üretilmiştir. TPE'ler, yüksekiletkenlik, iyi elektron transfer kinetiği, düşük maliyetli olma, kolay şekil verilebilme ve tekrar kullanılabilirlik gibi üstün özelliklerinedeniyle kullanılmıştır. TPE'ler, ilk kez p-nitroanilin kullanılarak aril diazonyum tuzları ile modifiye edilmiştir. Termoplastikelektrotlar için diazonyum iyon sentezine dayanan bir modifikasyon yöntemi geliştirilmiştir. Sulu fazda bir aril amin, p-tolüensülfonikasit ve sodyum nitrit karışımı hazırlanmış ve diazonyum tuzunun sentezlenmesi için birlikte öğütülmüştür. Reaksiyon sonucundadiazonyum iyonu oluşumunun göstergesi olarak pastanın rengi yeşil renkten sarı renge dönüşmüştür. Diazonyum iyonununsentezlenmesi ve graf edilmesi için 4-nitroanilin kullanılmıştır. Termoplastik elektrot yüzeyinde üretilen nitrofenil monodiazonyumkatyonları elektrokimyasal olarak aminofenil gruplarına indirgenmiştir. Elektrotun yüzeyindeki aminofenil gruplarının varlığı elektrokimyasal yolla doğrulanmıştır. Sulu asidik ortamdaki elektrokimyasal indirgeme işleminden sonra, 4-aminofenil ile modifiyeedilen termoplastik elektrotun elektrokimyasal davranışı ferrisiyanür varlığında araştırılmıştır. Dönüşümlü voltametri ile elektrotyüzeyinde graf edilen grupların oluşması nedeniyle karakteristik pikler elde edilmiştir. Ag/AgCl referans elektrota karşı yaklaşık -0,4V'de 4-aminofenilin indirgenerek amino grupları oluşmuştur. Modifiye edilen TPE'ler ile tarama hızı testi yapılarak anodik pik akımın100 mV/s'ye kadar lineer bir davranış gösterdiği gözlemlenmiştir. Bu da elektroaktif türlerin TPE yüzeyine graf edildiğinigöstermiştir. Ayrıca, sentezlenmiş diazonyum tuzunun elektrot yüzeyi üzerindeki inkübasyon süresi optimize edilmiştir ve optimuminkübasyon süresi 5 dakika olarak bulunmuştur.

Electrochemically Modified Carbon Composite Electrode Using Diazonium Salt

Carbon composite thermoplastic electrodes (TPEs) were fabricated using graphite, thermoplastic binder and solvent. TPEs were useddue to their outstanding properties such as high conductivity, good electron transfer kinetics, inexpensive, easy patterning andreusability. TPEs were modified with aryl diazonium salts using p-nitroaniline for the first time. An in-situ modification methodbased on diazonium ion synthesis was developed for thermoplastic electrodes. A mixture of aryl amine, p-toluenesulfonic acid, andsodium nitrite in aquous phase was prepared and grinded together in order to synthesize diazonium salts. A color change (from greento yellow) of the synthesized paste occurred upon reaction, which indicated diazonium ion formation. 4-nitroaniline was used tosynthesize and graft diazonium ion. In-situ generated nitrophenyl monodiazonium cations were electrochemically reduced toaminophenyl groups on the surface of the thermoplastic electrode. The presence of aminophenyl groups on the surface of theelectrode was confirmed via electrochemistry. After electrochemical reduction in aqueous acidic media, the electrochemical behaviorof a 4-aminophenyl modified thermoplastic electrode was investigated in the presence of ferricyanide. Characteristic peaks wereobtained due to the formation of grafted groups on the electrode surface by cyclic voltammetry. The reduction of the 4-aminophenyl resulted in the product of amino groups at about -0.4 V versus Ag/AgCl reference electrode. A scan rate study was performed bymodified TPEs and a linear dependence of the anodic peak current was observed up to 100 mV/s indicating that the electroactivespecies were grafted at the TPE surface. Furthermore, incubation time of synthesized diazonium salt on the electrode surface wasoptimized and found as 5 min.

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