亚甲基蓝与纳米金复合修饰电极的制备及对汞离子的检测
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摘要
以亚甲基蓝及纳米金复合修饰玻碳电极为基础电极,自组装修饰DL-1,4-二硫苏糖醇,用以检测汞离子.同时,利用扫描电镜观察了电极表面形貌,并对元素组成进行了分析;采用交流阻抗法研究了电极的电化学特性,分析了制备过程对电极的影响;采用差分脉冲伏安法检测汞离子,考察了吸附时间、缓冲液种类以及pH值等因素对汞离子检测过程的影响.结果表明:吸附时间为35min,pH=6,以Tris溶液为缓冲液时,测试条件最佳;检测汞离子的线性范围为1.0×10~(-9)～1.0×10~(-3) mol/L,检测限为5.4×10~(-10) mol/L.最后考察了地表水中常见离子的干扰作用,显示所制备电极对汞离子检测具有良好的选择性.
A composite electrode was prepared to detect mercury ions.The electrode was first modified with methylene blue and gold nanoparticles,and then self-assembled with DL-1,4-dithiothreitol.The morphologies and elements of the electrode surface were analyzed by a scanning electron microscope with an energy dispersive spectrometer.The electrochemical properties of the electrode were studied by electrochemical impedance spectroscopy.In this work,differential pulse voltammetry was used to detect mercury,and the effects of adsorption time,pH and buffer types on the detection of mercury ions were investigated.The experimental results indicated that mercury ions could be effectively detected in the Tris solution(pH=6),and the optimal adsorption time was 35 min.The linear range was 1.0×10~(-9)～1.0×10~(-3) mol/L,and the detection limit was 5.4×10~(-10) mol/L.The results of interference experiments revealed that the electrode prepared here had good selectivity for the detection of mercury ions.
A composite electrode was prepared to detect mercury ions.The electrode was first modified with methylene blue and gold nanoparticles,and then self-assembled with DL-1,4-dithiothreitol.The morphologies and elements of the electrode surface were analyzed by a scanning electron microscope with an energy dispersive spectrometer.The electrochemical properties of the electrode were studied by electrochemical impedance spectroscopy.In this work,differential pulse voltammetry was used to detect mercury,and the effects of adsorption time,pH and buffer types on the detection of mercury ions were investigated.The experimental results indicated that mercury ions could be effectively detected in the Tris solution(pH=6),and the optimal adsorption time was 35 min.The linear range was 1.0×10~(-9)～1.0×10~(-3) mol/L,and the detection limit was 5.4×10~(-10) mol/L.The results of interference experiments revealed that the electrode prepared here had good selectivity for the detection of mercury ions.
引文
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[4]王玉兰.原子荧光光谱法检测土壤样品中砷、汞形态的研究[D].吉林:吉林大学,2012.
[5]SILVA.Development of spectrophotometric method for iron determination in fortified wheat and maize flours[J].Food Chem,2017,242:205-210.
[6]雷兆静,张存政,胡秋辉,等.核酸适体识别荧光法检测汞离子[J].分析化学,2012,40(12):1827-1831.
[7]WU X H,LI M,LIN H,et al.Determination of five heavy metal ions in environmental samples by a rapid high performance liquid chromatography[J].Asian J Chem,2007,19(1):79-86.
[8]杨希春.探讨离子选择电极在化工分析检测中的应用[J].化工管理,2019(1):36-41.
[9]NAMOR A,GAMOUZ A,ALHARTHI S,et al.A ditopic calix pyrrole amide derivative:highlighting the importance of fundamental studies and the use of NaPh4B as additive in the design and applications of mercury(II)ion selective electrodes[J].J Mater Chem A,2015,3(24):13016-13030.
[10]ZHANG W,ROZNIECKA E,MALINOWSKA E,et al.Optical chloride sensor based on dimer-monomer equilibrium of indium(III)octaethylporphyrin in polymeric film[J].Anal Chem,2002,74(17):4548-4557.
[11]DALKIRAN B,?ZEL A D,PARLAYAN S,et al.A novel lariat crown compound as ionophore for construction of a mercury(II)-selective electrode[J].Monatsh Chem,2010,141(8):829-839.
[12]李仙清.硫醇自组装膜金电极对汞离子的快速灵敏检测与机理探讨[D].长沙:长沙理工大学,2016.
[13]曹婷婷.一种简单快速检测汞离子的1-4-二硫苏糖醇膜修饰金平板电极[J].高等学校化学学报,2014,35:1388-1395.