Termal indirgenmiş grafen oksit ile elektrokimyasal olarak askorbik asit tayini

Bu çalışmada termal olarak indirgenmiş grafen oksit (T-rGO) ve Nafion çözeltisi (N117) ile kaplanmış camsı karbon elektrotun (GCE), fosfat tampon çözeltisindeki (PBS) askorbik asitin (AA) varlığına göre elektrokimyasal davranışı dönüşümlü voltametri (CV), diferansiyel puls voltametri (DPV) ve amperometrik tekniklerle incelenmiştir. Bu amaçla T-rGO, başlangıç malzemesi olan sentetik grafitten modifiye Hummers yöntemi ile grafen oksite (GO), ardından da GO’nun inert gaz ortamında termal işlem uygulanarak indirgenmesi ile sentezlenmiştir. Yapının karakterize edilmesi amacıyla SEM, XRD, Raman, FTIR ve elementel analiz gibi çeşitli teknikler kullanılmıştır. XRD analiz verileri kullanılarak yaklaşık 3,32 tabaka sayısına sahip T-rGO elde edildiği tespit edilmiştir. 5,0 mM AA içeren farklı pH değerlerine sahip (6, 7 ve 8) PBS arasından, pH 8 çözeltisindeki GCE/T-rGO elektrotu için en belirgin anodik yükseltgenme piki elektrot üzerinden geçen en yüksek akım miktarıyla elde edilmiştir. GCE/T-rGO elektrotu ile elde edilen sonuçlara göre, AA, derişim ve anodik pik akımı arasındaki geniş doğrusal tayin aralığında (4,0-100,0 mM, R2=0,9978) yüksek hassasiyet (0,3 μA mM-1), tayin limiti (0,61 μM), yeniden üretilebilirlik (RSD=%6,25, n=3) ve tekrarlanabilirlikle (RSD=%2,14, n=3) belirlenebilmektedir. Ayrıca, GCE/T-rGO elektrot ürik asit, NaCl ve CaCl2’e karşı yüksek seçicilik sergilemiştir. Bu nedenlerle, hazırlanan GCE/T-rGO elektrotların AA molekülünün elektrokimyasal tayininde kullanılabileceği düşünülmektedir.

Anahtar Kelimeler:

İndirgenmiş grafen oksit, modifiye hummers yöntemi, askorbik asit, camsı karbon elektrot

Electrochemical determination of ascorbic acid with thermally reduced graphene oxide

In this study, electrochemical behavior of a glassy carbon electrode (GCE), which is covered with thermally reduced graphene oxide (T-rGO) and Nafion solution (N117), is investigated using the cyclic voltammetry (CV), differential pulse voltammetry (DPV) and amperometric techniques in phosphate buffer solution (PBS) contains ascorbic acid (AA). For this purpose, T-rGO is synthesized from synthetic graphite as the starting material to graphene oxide by modified Hummers method, followed by reduction of graphene oxide with flash heat treatment in inert gas environment. In order to characterize the structure, several techniques such as SEM, XRD, Raman, FTIR and elemental analysis are used. Number of layer of T-rGO is determined as about 3.32 with using XRD analysis data. In the PBS with different pH values (6, 7 and 8) containing 5.0 mM AA, the highest current value with a clearly anodic oxidation peak is obtained for the GCE/T-rGO electrode in the pH 8 PBS. According to the results obtained with GCE/T-rGO electrode, AA can be detected over a wide linear detection range between the AA concentration and anodic peak current (4.0-100.0 mM, R2=0.9978) with good sensitivity (0.3 μA mM-1), high detection limit (0.61 μM), good reproducibility (RSD=6.25%, n=3) and repeatability (RSD=2.14%, n=3). In addition, the GCE/T-rGO electrode showed good selectivity against the uric acid, NaCl and CaCl2. For these reasons, it is thought that the GCE/T-rGO electrodes can be used for electrochemical determination of AA molecule.

Keywords:

Reduced graphene oxide, modified hummers method, ascorbic acid, glassy carbon electrode,

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