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Spherical Au–Pd bimetallic nanoparticles, for the first time, have been elucidated to have a high electrochemical performance toward As(III) by square wave anodic stripping voltammetry. A strong Pd tuned effect on electrochemical performance in the detection of As(III) was found. A high sensitivity of 3.9μA/ppb with a low limit of detection (LOD) of 2.40×10 −2 ppb was obtained for Au 1...