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Single-crystal Fe3O4 with monodisperse microspheres structure has been used for individual electrochemical detection of heavy metal ions. Morphology and structure of the as-prepared Fe3O4 microspheres were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD). Meanwhile the electrochemical properties of the Fe3O4 microspheres modified glass carbon electrodes (GCE) were characterized by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS), and the enhanced electrochemical response in stripping voltammetry for individual detection of Pb(II), Hg(II), Cu(II), and Cd(II) was evaluated using square wave anodic stripping voltammetry (SWASV). With high specific surface area and excellent catalytic activity toward heavy metal ions, the as-prepared monodisperse and single-crystal Fe3O4 microspheres show a preferable sensing sensitivity (22.2 μA/μM) and limit of detection (0.0699 μM) toward Pb(II). Furthermore, the electrochemical sensor of Fe3O4 microspheres exhibits excellent stability and it also offers potential practical applicability for the determination of heavy metal ions in real water samples. This study provides a potential simple and low cost iron oxide for the construction of sensitive electrochemical sensors applied to monitor and control the pollution of toxic metal ions.  相似文献   
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