CN102621203B - 一种席夫碱修饰铜电极的制备方法 - Google Patents

一种席夫碱修饰铜电极的制备方法 Download PDF

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CN102621203B
CN102621203B CN201210080994.3A CN201210080994A CN102621203B CN 102621203 B CN102621203 B CN 102621203B CN 201210080994 A CN201210080994 A CN 201210080994A CN 102621203 B CN102621203 B CN 102621203B
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CN102621203A (zh
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刘峥
张小鸽
王苗苗
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Guilin University of Technology
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Abstract

本发明公开了一种席夫碱修饰铜电极的制备方法。截取铜棒，用砂纸打磨，在6mol/LHNO3中浸泡10s，然后快速用蒸馏水冲洗，电极周围用石蜡密封，仅有底端和顶端，顶端用于固定电极，底端接触溶液.然后在50mL含0.0135g配体的1mo l/LNaOH中于-1.2～0.6V电位区间以50mV·s-1扫速扫描14圈，即制得邻氧乙酸苯甲醛缩牛磺酸席夫碱修饰铜电极。本发明的修饰电极制作方法简单，制备的电极对过氧化氢有较高的电催化还原活性，可应用于环境样品中过氧化氢的分析测定。

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一种席夫碱修饰铜电极的制备方法
技术领域
本发明属电化学技术领域，特别涉及一种席夫碱修饰铜电极的制备方法。
背景技术
目前，席夫碱及其配合物种类繁多，结构多样，有许多独特的性能，在分析化学、医药领域、催化领域、腐蚀领域、光致变色等许多方面应用非常广泛。在分析化学领域，含硫Schiff碱作为良好配体，可以用来鉴别、鉴定金属离子并可借助色谱分析、荧光分析、光度分析等手段达到对某些有机小分子和金属离子的定量分析，且效果十分理想，但席夫碱修饰铜电极对过氧化氢电催化氧化的研究则少有报道。过氧化氢(H2O2)作为一种强氧化剂，具有消毒杀菌和漂白等作用，是工业生产、临床医学和环境科学等方面的重要物质。随着工业农业的发展，各种工农业产品越来越多，但其残余物(其中就有过氧化氢)对水源和土壤存在污染，因此，过氧化氢的快速、准确、定量的检测具有重要意义。化学修饰电极因其测试速度快、准确度高、便于携带等特点越来越得到人们的重视，因此，研究新型化学修饰剂的制备及相关电极的制作方法至关重要。
发明内容
本发明的目的是提供一种能分析检测过氧化氢的席夫碱修饰铜电极的制备方法。
具体步骤为：
截取铜棒，用砂纸打磨，在6mol/LHNO3中浸泡10秒，然后用蒸馏水冲洗，电极除底端和顶端外周围用石蜡密封，顶端用于固定电极，底端接触溶液；然后在50mL含0.0135g邻氧乙酸苯甲醛缩牛磺酸席夫碱配体的1mol/LNaOH中于-1.2～0.6V电位区间以扫50mV·s-1扫描14圈，即制得邻氧乙酸苯甲醛缩牛磺酸席夫碱修饰铜电极。
本发明制备了1种邻氧乙酸苯甲醛缩牛磺酸席夫碱铜电极的修饰剂。以邻氧乙酸苯甲醛为原料，制备了新的邻氧乙酸苯甲醛缩牛磺酸席夫碱，并以此作为化学修饰剂，研制了邻氧乙酸苯甲醛缩牛磺酸席夫碱修饰铜电极，发现该电极对过氧化氢有较好的电催化还原活性。在过氧化氢浓度为2.576×10-3-1.288×10-2mol/L范围内，过氧化氢的浓度与还原峰电流成线性关系。
本发明的修饰电极制作方法简单，制备的电极对过氧化氢有较高的电催化还原活性，可应用于环境样品中过氧化氢的分析测定。
具体实施方式
实施例：
截取约6.5cm长的铜棒(φ＝2.0mm)，用砂纸打磨，在6mol/LHNO3中浸泡10秒，然后快速用蒸馏水冲洗，电极除底端和顶端外周围用石蜡密封，顶端用于固定电极，底端接触溶液.然后在50mL含0.0135g邻氧乙酸苯甲醛缩牛磺酸席夫碱配体的1mol/LNaOH中于-1.2～0.6V电位区间以50mV·s-1扫速扫描14圈，即制得邻氧乙酸苯甲醛缩牛磺酸席夫碱修饰铜电极。
准确量取水样5mL，用pH＝6.5PBS缓冲溶液定容至50mL，用上述修饰电极测定此溶液的还原峰电流值，代入线性回归方程，计算H2O2的浓度，并计算水样中H2O2的含量。
准确量取水样5mL，用pH＝6.5PBS缓冲溶液定容至50mL，准确加入一定体积的20％H2O2溶液，定容至50mL，进行加标回收实验，结果见表1。
从表1可知，用此方法测定H2O2的回收率为98.7％～104.9％，这说明这种方法有很高的准确性。
表1：加标回收实验结果
Figure BSA00000690252600021

Claims (1)

1. 一种席夫碱修饰铜电极的制备方法，其特征在于具体步骤为：
截取铜棒，用砂纸打磨，在6mol/LHNO3中浸泡10秒，然后用蒸馏水冲洗，电极除底端和顶端外周围用石蜡密封,顶端用于固定电极，底端接触50mL含0.0135g邻氧乙酸苯甲醛缩牛磺酸席夫碱配体的1mol/LNaOH溶液，在该溶液中于-1.2～ 0.6 V电位区间以扫速50 mV·s-1扫描14圈，即制得邻氧乙酸苯甲醛缩牛磺酸席夫碱修饰铜电极。
CN201210080994.3A 2012-03-22 2012-03-22 一种席夫碱修饰铜电极的制备方法 Expired - Fee Related CN102621203B (zh)

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