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    基于纳米TiO2和TiN为工作电极的循环伏安法测定过氧化氢的含量

    Determination of Hydrogen Peroxide by Cyclic Voltammetry Based on Nano TiO2 and TiN as Working Electrode

      摘要
    • 摘要: 制备了纳米TiO2、TiN材料，将其作为工作电极，建立了循环伏安法测定过氧化氢含量的方法。将钛片置于含10.0 g氟化铵、0.6 g脲、24 mL 30%（质量分数）过氧化氢溶液、24 mL硝酸组成的抛光液中进行下表面抛光处理，再加入15 mL丙酮、15 mL无水乙醇、15 mL水，超声处理15 min后，得到光亮钛片。以光亮钛片为阳极，普通钛片为阴极，在不同电解质TiO2粗糙膜对应的电解质为1.0 mol·L-1硫酸溶液；TiO2纳米管为50 mL丙三醇、50 mL水、0.2 mol·L-1硫酸溶液、0.5%（质量分数）氟化钠溶液；TiO2纳米孔为100 mL乙二醇、1 mL水、0.38%（质量分数）氟化铵溶液中，采用阳极氧化法，得到不同形貌大小的TiO2粗糙膜、TiO2纳米管、TiO2纳米孔；再通过氨气热还原，得到TiN粗糙膜、TiN纳米管、TiN纳米孔。以TiO2和TiN材料为工作电极，铂片为辅助电极，Ag/AgCl为参比电极，将三电极体系置于磷酸盐缓冲溶液（pH 7.0）中，采用循环伏安法法测定过氧化氢含量。结果显示：TiN粗糙膜、TiN纳米管、TiN纳米孔电极的速率常数分别为2.39×10-6，3.03×10-6，6.40×10-6cm·s-1；以TiO2粗糙膜、TiN粗糙膜、TiO2纳米管、TiN纳米管、TiO2纳米孔、TiN纳米孔为工作电极，过氧化氢的浓度在一定范围内与其对应的还原峰电流呈线性关系，检出限（3s/k）分别为23.30，14.29，19.9，10.6，16.9，5.02 μmol·L-1；在磷酸盐缓冲溶液（pH 7.0）中滴加50 μmol·L-1 H2O2溶液，采用计时电流法在-0.4 V外加电压下进行测定，计算得TiN粗糙膜、TiN纳米管、TiN纳米孔响应电流的相对标准偏差（RSD，n=5）分别为4.7%，3.2%和7.3%。

       

      Abstract: A method for determination of H2O2 by cyclic voltammetry using nano TiO2 and TiN materials as working electrode was established. The lower surface of Ti sheet was polished in polishing solution including 10.0 g of ammonium fluoride, 0.6 g of urea, 24 mL of 30% (mass fraction) hydrogen peroxide solution and 24 mL of nitric acid, and treated with ultrasonic for 15 min in a mixture of 15 mL of acetone, 15 mL of anhydrous ethanol and 15 mL of water. Then bright Ti sheet obtained was used as anode, and ordinary Ti sheet was used as cathode. TiO2 rough film, TiO2 nanotube and TiO2 nanopore with different morphologies were prepared in different electrolytes1.0 mol·L-1 sulfuric acid solution for TiO2 rough film; a mixture of 50 mL of glycerin, 50 mL of water, 0.2 mol·L-1 sulfuric acid solution and 0.5% (mass fraction) sodium fluoride solution for TiO2 nanotube; a mixture of 100 mL of glycol, 1 mL of water and 0.38% (mass fraction) ammonium fluoride solution for TiO2 nanopore by anodic oxidation method, and TiN rough film, TiN nanotube and TiN nanopore were obtained by ammonia thermal reduction reaction. TiO2 and TiN materials were used as working electrode, platinum sheet as auxiliary electrode, and Ag/AgCl as reference electrode, and H2O2 was determined by cyclic voltammetry with three electrodes system in phosphate buffer solution (pH 7.0). It was showed that the rate constants of TiN rough film, TiN nanotube and TiN nanopore electrode were 2.39×10-6, 3.03×10-6cm·s-1 and 6.40×10-6 cm·s-1, respectively. Using TiO2 rough film, TiN rough film, TiO2 nanotube, TiN nanotube, TiO2 nanopore and TiN nanopore as working electrodes, linear relationships between concentrations of hydrogen peroxide and their reduction peak currents were kept in definite ranges, with detection limits (3s/k) of 23.30, 14.29, 19.9, 10.60, 16.90, 5.02 μmol·L-1. 50 μmol·L-1 H2O2 solution dropped in phosphate buffer solution (pH 7.0) was determined by chronoamperometry at -0.4 V of externaly applied voltage, and RSDs (n=5) of response currents of TiN rough film, TiN nanotube and TiN nanopore were 4.7%, 3.2% and 7.3%, respectively.

       

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