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出 处:《理化检验(化学分册)》2013年第11期1321-1325,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基 金:湖南省高校"中药制剂工程与质量控制"产学研合作示范基地建设项目(11CY013);湖南省教育厅科研基金(13C712);怀化学院大学生开放性实验项目(2012-17)
摘 要:制备了石墨烯(GP)-Nafion/纳米金(Au)复合膜修饰玻碳电极(GCE),并将其用于阳极溶出伏安测定大米中痕量锌。采用x射线衍射(XRD)、扫描电镜(SEM)、电化学交流阻抗谱(EIS)对修饰电极的结构和性能进行了表征。在pH4.5的乙酸盐缓冲溶液中,-1.5V(VS.SCE)富集150s,以100mV·s-1 扫描速率从-1.3V扫描至-0.6V。锌在修饰电极上于-1.0V处产生-灵敏的阳极溶出伏安峰,峰电流与锌的质量浓度在5.0×10^-4~0.15mg·L^-1 范围内呈线性关系,检出限(3σ)为2.8×10^-4mg·L-1。方法用于测定大米样品中痕量锌的含量,并以此样品为基体做回收试验,测得回收率在98.0%~106%之间。方法的测定结果与石墨炉原子吸收光谱法测定值-致。A graphene, Nation and gold nano-particles composite film modified glassy carbon electrode (GP Nafion/Nano-Au/GCE) was prepared and its structure and property were characterized by XRD, SEM and EIS. In an acetate buffer solution of pH 4.5, Zn( Ⅱ ) ion was accumulated at -1.5 V (vs. SCE) for 150 s and upon scanning from -1.3 V to -0. 6 V at the rate of 100 mV . s-1 , a sensitive anodic stripping voltammetric peak given by Zne+ at the modified electrode at the potential of -1.0 V (vs. SCE) was observed. Linear relationship between values of peak current and mass concentration of Zn was obtained in the range of 5.0× 10^-4-0. 15 mg .L-1, with detection limit (3σ) of 2.8 × 10^-4 mg. L-1. The method was used for the determination of Zn in rice sample, and using the same sample as matrix, recovery was tested by standard addition method, giving results of recovery in the range of 98. 0%--106%. The analytical results found by this method were consistent with those obtained by GF-AAS.
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