Determination of Trace Amount of Unsym-Dimethylhydrazine in Water by Cyclic Voltammetry with MWNTs Modified Glassy Carbon Electrode
摘 要
采用滴涂法制备多壁碳纳米管修饰玻碳电极,用循环伏安法测定水中微量偏二甲肼。多壁碳纳米管修饰玻碳电极对偏二甲肼有良好的富集特性和电催化活性。优化的试验条件如下:①支持电解质为pH 7.0的磷酸盐缓冲溶液;②富集电位为0.8 V;③富集时间为120 s。偏二甲肼的浓度在6.6×10-6~1.45×10-4mol·L-1内与其对应的氧化峰电流呈线性关系,方法的检出限(3S/N)为7.3×10-7mol·L-1。对5.0×10-5mol·L-1偏二甲肼标准溶液连续测定5次,测定值的相对标准偏差为1.5%。方法用于模拟水样的分析,加标回收率为99.3%~112%。
Abstract
Multi-walled carbon nanotubes modified glassy carbon electrode was prepared by dropping method. Cyclic voltammetry was applied to the determination of trace amount of unsym-dimethylhydrazine in water. It was found that multi-walled carbon nanotubes modified glassy carbon electrode had good enrichment and electrocatalytic activity for unsym-dimethylhydrazine. The optimized conditions found were as follows:① supporting electrolyte was PBS of pH 7.0; ② enrichment potential was 0.8 V; ③ enrichment time was 120 s. Linear relationship between values of oxidation peak current and concentration of unsym-dimethylhydrazine was kept in the range of 6.6×10-6-1.45×10-4mol·L-1, with detection limit (3S/N) of 7.3×10-7mol·L-1. Precision of the method was tested at the concentration level of 5.0×10-5mol·L-1 unsym-dimethylhydrazine standard solution for 5 determinations, and value of RSD found was 1.5%. The proposed method was applied to the analysis of simulated water sample, giving values of recovery in the range of 99.3%-112%.
中图分类号 O657.1 DOI 10.11973/lhjy-hx201802011
所属栏目 工作简报
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收稿日期 2017/3/18
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备注胡黎明(1992-),男,山东青州人,硕士研究生,主要从事微量偏二甲肼检测工作
引用该论文: HU Liming,LIU Xiangxuan,ZHANG Langlang. Determination of Trace Amount of Unsym-Dimethylhydrazine in Water by Cyclic Voltammetry with MWNTs Modified Glassy Carbon Electrode[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(2): 177~181
胡黎明,刘祥萱,张浪浪. 多壁碳纳米管修饰玻碳电极的循环伏安法测定水中微量偏二甲肼[J]. 理化检验-化学分册, 2018, 54(2): 177~181
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参考文献
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【3】GB 18063-2000水源水中偏二甲基肼卫生标准[S].
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【6】WANG J, LU Z L. Electrocatalysis and determination of hydrazine compounds at glassy carbon electrodes coated with mixed-valent ruthenium(Ⅲ, Ⅱ) cyanide films[J]. Electroanalysis, 2005,1(6):517-521.
【7】PIROGOV A V, CHERNOVA M V, NEMTSEVA D S, et al. Sulfonated and sulfoacylated poly(styrene-divinylbenzene) copolymers as packing materials for cation chromatography[J]. Analytical and Bioanalytical Chemistry, 2003,376(5):745-747.
【8】张有智,李正莉,王煊军,等.微量偏二甲肼检测技术研究进展[J].化学推进剂与高分子材料, 2008,6(3):20-23.
【9】JIANG L, WANG R, LI X, et al. Electrochemical oxidation behavior of nitrite on a chitosan-carboxylated multiwall carbon nanotube modified electrode[J]. Electrochemistry Communications, 2005,7(6):597-601.
【10】JEYKUMARI D R S, RAMAPRABHU S, NARAYANAN S S. A thionine functionalized multiwalled carbon nanotube modified electrode for the determination of hydrogen peroxide[J]. Carbon, 2007,45(6):1340-1353.
【11】SANTHOSH P, MANESH K M, GOPALAN A, et al. Fabrication of a new polyaniline grafted multi-wall carbon nanotube modified electrode and its application for electrochemical detection of hydrogen peroxide[J]. Analytica Chimica Acta, 2006,575(1):32-38.
【12】赵冬梅,李振伟,刘领弟,等.石墨烯/碳纳米管复合材料的制备及应用进展[J].化学学报, 2014,72(2):185-200.
【13】ZHAO W, ZHAO B. Carbon nanotube-hydrogen peroxide hybrid based optical sensing method for assessment of antioxidant potency:US8796625[P]. 2014-08-05.
【14】赵振廷.纳米材料电化学传感器制备及其在肼检测中的应用研究[D].太原:太原理工大学, 2016.
【15】MALLAKPOUR S, ZADEHNAZARI A. The production of functionalized multiwall carbon nanotube/amino acid-based poly(amide-imide) composites containing a pendant dopamine moiety[J]. Carbon, 2013,56(6):27-37.
【16】孙唯.碳纳米管修饰邻苯二酚传感器的研究[D].无锡:江南大学, 2008.
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