Svegl Irena Grabec, Bele Marjan, Ogorevc Bozidar
National Institute of Chemistry, P.O. Box 660, SI-1001 Ljubljana, Slovenia.
Anal Chim Acta. 2008 Nov 3;628(2):173-80. doi: 10.1016/j.aca.2008.08.046. Epub 2008 Sep 16.
A new type of carbon film electrode, composed of a thin layer of tightly packed carbon black (CB) nanoparticles deposited onto a gelatin-covered indium tin oxide/glass support using the surface-induced deposition (SID) approach, is presented. Some parameters of the novel SID method were optimized and the surface image and functionalization of the investigated carbon black film electrode (CBFE) was inspected by employing scanning electron microscopy and infrared spectroscopy. A cyclic voltammetry (CV) study was conducted in which the electron-transfer kinetics and CBFE interfacial characteristics were evaluated employing several selected reference redox systems, such as Ru(NH(3))(6), Fe(CN)(6) and Fe(3+/2+) in aqueous, and ferrocene/ferrocenium in acetonitrile media. CV recordings were also performed in order to compare the electrochemical behavior of the CBFE with that of some well-known and established bare carbon-based electrodes. In order to confirm the validity of the CB film preparation method, the electroanalytical performance of the proposed CBFE was examined by carrying out linear sweep voltammetry of ascorbic acid (AA), anodic stripping square-wave voltammetry of Cu(II) in acidic medium, and amperometric measurements of hydrogen peroxide under flow injection conditions. The sensing characteristics of the novel carbon film electrode, demonstrated in this preliminary study, comprise: (i) a wide working potential window ranging from +1.0 to -1.3 V (depending on the solution pH), (ii) a wide applicable pH range (at least from 2 to 12), (iii) low voltammetric background (<5 microA cm(-2)), (iv) a satisfactory linear voltammetric and amperometric response (r(2)>0.99) to various analytes, (v) good reproducibility (for example, r.s.d. of 2% in amperometric detection of H(2)O(2) and r.s.d. of 8.5% for electrode-to-electrode CV runs), and (vi) stable and fast current response (at least 100 CV runs with negligible change in CV response). The main advantages of the proposed CBFE originate from the unique CB film formation procedure that enables fast, simple, inexpensive and non-toxic CBFE preparation, which can find application in advanced electrochemical devices and is suitable for mass production.
本文介绍了一种新型碳膜电极,它是通过表面诱导沉积(SID)方法,将一层紧密堆积的炭黑(CB)纳米颗粒沉积在明胶覆盖的氧化铟锡/玻璃载体上制成的。对这种新型SID方法的一些参数进行了优化,并通过扫描电子显微镜和红外光谱对所研究的炭黑膜电极(CBFE)的表面图像和功能化进行了检测。进行了循环伏安法(CV)研究,采用几种选定的参比氧化还原体系,如水中的Ru(NH(3))(6)、Fe(CN)(6)和Fe(3+/2+),以及乙腈介质中的二茂铁/二茂铁鎓,评估了电子转移动力学和CBFE的界面特性。还进行了CV记录,以比较CBFE与一些知名的裸碳基电极的电化学行为。为了证实CB膜制备方法的有效性,通过对抗坏血酸(AA)进行线性扫描伏安法、在酸性介质中对Cu(II)进行阳极溶出方波伏安法以及在流动注射条件下对过氧化氢进行安培测量,考察了所提出的CBFE的电分析性能。在这项初步研究中展示的新型碳膜电极的传感特性包括:(i)宽工作电位窗口,范围从+1.0到 -1.3 V(取决于溶液pH值);(ii)宽适用pH范围(至少从2到12);(iii)低伏安背景(<5 μA cm(-2));(iv)对各种分析物具有令人满意的线性伏安和安培响应(r(2)>0.99);(v)良好的重现性(例如,在安培检测H(2)O(2)时相对标准偏差为2%,电极间CV运行的相对标准偏差为8.5%);以及(vi)稳定且快速的电流响应(至少100次CV运行,CV响应变化可忽略不计)。所提出的CBFE的主要优点源于独特的CB膜形成过程,该过程能够快速、简单、廉价且无毒地制备CBFE,可应用于先进的电化学装置,适合大规模生产。