在含有1 mmol/L H2PtCl6的0.1 mol/L H2SO4中,通过恒电位还原在铂盘电极表面原位沉积出球形、菱形、花状等不同形貌的Pt纳米颗粒.改变还原电位和时间实现了纳米铂的形貌及催化活性调控.实验表明,COD的电流响应信号与纳米Pt的形貌密切相关,-03 V还原2 min制备的花状纳米铂对COD的信号增强效应最强,显著提高了COD的响应电流.考察了pH值及安培检测电位的影响,构建了一种新型COD电化学传感器,检出限为1.8 mg/L,将其用于不同湖水COD浓度的测定,结果与国标法一致.
Platinum nanoparticles with different shapes such as spheres, rhombs and flowerlike sheets were in situ deposited on the surface of Pt disk electrode via reduction of 1 mmol/L H2PtC16 in 0.1 mol/L H2SO4. By variation of reduction potential and time, the morphology and catalytic activities of Pt nanoparticles were readily tuned. The electrochemical tests revealed that the response of chemical oxygen demand (COD) on nano-Pt surface was shape-dependent. Compared with nanospheres and nanorhombs, flowerlike Pt nanosheets that deposited at -0.3 V for 2 min greatly increased the response current of COD, displaying strong signal enhancement for COD. The influences of pH value and detection potential were discussed. As a result, a novel electrochemical sensor using flowerlike Pt nanosheets as sensing film was constructed for COD, and the detection limit was 1.8 mg/L. The sensor has been used for the determination of COD in different lake water samples. The obtained results were consisted with those values by the national standard method.