Department of Chemistry, Shahid Bahonar University of Kerman, PO Box 76175-133, 22th Bahman Blvd, Kerman, Iran.
Talanta. 2010 Mar 15;80(5):1827-31. doi: 10.1016/j.talanta.2009.10.029. Epub 2009 Oct 23.
A 4-(2-pyridylazo)-resorcinol (PAR)-modified carbon ceramic electrode (CCE) prepared by the sol-gel technique has been reported for the first time in this paper. By immersing the CCE in aqueous solution of PAR (0.001molL(-1)), after a short period of time, a thin film of PAR was rapidly formed on the surface of the electrode due to its strong adsorption properties. A differential pulse anodic stripping voltammetric (DPASV) method was developed for determination of Ag(I) at the modified carbon ceramic electrode. The analysis procedure consisted of an open circuit accumulation step in a sample solution which was continuously stirred for 12 min. This was followed by replacing the medium with a clean solution where the accumulated Ag(I) was reduced for 15s in -0.6 V. Then, the potential was scanned from -0.2 to +0.2V to obtain the voltammetric peak. The detection limit of silver(I) was 0.123 microg L(-1), and for seven successive determinations of 10, 100 and 200 microg L(-1) Ag(I), the relative standard deviations were 2.1, 1.4 and 1.03%, respectively. The calibration curve was linear for 0.5-300 microg L(-1) silver(I). The procedure was applied to determine silver(I) in X-ray photographic films and super-alloy samples.
本文首次报道了一种通过溶胶-凝胶技术制备的 4-(2-吡啶偶氮)-间苯二酚(PAR)修饰的碳陶瓷电极(CCE)。将 CCE 浸入 PAR(0.001molL(-1))的水溶液中,由于其强吸附性能,在短时间内,电极表面迅速形成一层 PAR 薄膜。建立了在修饰碳陶瓷电极上测定 Ag(I)的差分脉冲阳极溶出伏安法(DPASV)。分析步骤包括在样品溶液中开路累积 12min,然后用干净的溶液替换介质,在 -0.6V 下还原累积的 Ag(I)15s。然后,将电势从 -0.2 扫描到+0.2V,以获得伏安峰。银(I)的检测限为 0.123μg L(-1),对于 10、100 和 200μg L(-1)Ag(I)的七次连续测定,相对标准偏差分别为 2.1%、1.4%和 1.03%。校准曲线在 0.5-300μg L(-1)银(I)范围内呈线性。该方法应用于 X 射线照相胶片和超合金样品中银(I)的测定。