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作 者:武江艳 何亚萍[2] 韩权[1,2] 杨晓慧[2] 霍燕燕[2] WU Jiang-yan;HE Ya-ping;HAN Quan;YANG Xiao-hui;HUO Yan-yan(School of Chemistry and Chemical Engineering,Yan'an University,Yan'an716000,China;School of Chemistry and Chemical Engineering,Xi'an University,Xi'an710065,China)
机构地区:[1]延安大学化学与化工学院,陕西延安716000 [2]西安文理学院化学工程学院,陕西西安710065
出 处:《分析测试学报》2018年第12期1469-1474,共6页Journal of Instrumental Analysis
基 金:国家自然科学基金(21445004;21545014;21275116);陕西省创新能力支撑计划(2018KJXX-090);西安市科技计划项目(CXY1531WL22;2016CXWL09;2016CXWL18);陕西省教育厅重点实验室访问学者项目(14JS095);西安文理学院博士启动基金(06005017);大学生创新创业训练计划项目(201611080008;201613);陕西省分析化学重点学科项目(09009001)
摘 要:以钴离子(Co2+)与5-(5-碘-2-吡啶偶氮)-2,4-二氨基甲苯(5-I-PADAT)形成的配合物(Co2+-5-IPADAT)为支持电解质,采用循环伏安法,扫描电位范围-1. 5~0. 5 V,沉积50圈,制备获得Co NPs-5-I-PADAT修饰电极。采用扫描电子显微镜成像、X射线晶体衍射对其形貌及组成进行分析,并研究其对肼的电催化氧化行为。结果表明:在p H 7. 0的磷酸缓冲溶液中,电压位于0. 55 V处呈现显著的肼氧化峰。据此,建立了肼的定量分析方法,其线性范围为0. 64~2 150μmol/L,相关系数为0. 998 0,检出限(S/N=3)为0. 28μmol/L,回收率为95. 3%~102%。Co NPs-5-I-PADAT/GCE修饰电极具有良好的稳定性和选择性,可满足环境样品中肼的检测需求。A cobaltion-5-(5-iodide-2-pyridylazo)-2,4-diamino toluene(5-I-PADAT)(Co^2+-5-I-PADAT)modified electrode was prepared via cyclic voltammetric electrodeposition with Co^2+-5-I-PADAT,a coordination compound as supporting electrolyte in the scanning potential range of-1.5-0.5 V by 50 deposition circles.The morphology and composition of the modified electrode were characterized by scanning electron microscopy and X-ray crystalline diffraction.The electrocatalytic oxidation behavior of hydrazine on the modified electrode was also investigated.Results indicated that a significant hydrazine oxidation peak appeared at a potential of 0.55 V in a pH 7.0 phosphate buffer solution.Based on that,a novel method for the quantitative analysis of hydrazine was established.There was linear relationship for the oxidation peak current with hydrazine in the concentration range of 0.64-2 150μmolL with a correlation coefficient of 0.998 0.The detection limit(SN=3)was 0.28μmolL,and the recoveries were in the range of 95.3%-102%.With the advantages of good reproducibility and selectivity,the sensor could satisfy the requirements for detection of hydrazine in environmental samples.
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