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制备了磷钼杂多酸-L-半胱氨酸自组装超分子膜电极(P2Mo18-L-Cys/Au)。采用水平衰减全反射(ATR-FTIR)光谱表征了膜的组成。研究了该膜电极的电化学性质,发现它在1.0 mol/L H2SO4溶液中,于0.0~0.7V(vs.SCE)间CV扫描出现两对稳定、可逆的氧化还原峰,其中峰电位分别为Em1=0.334 V,Em2=0.188V,对应着P2Mo18O_(62)~(6-)的两步2电子-2质子反应;计时库仑法计算了薄膜内的电子传递系数D为5.01 × 10~(-8)cm2·s~(-1)。该膜电极对酸性溶液中的NO_2~-有明显的电催化还原作用,初步探讨了电催化机理。用差分脉冲伏安法(DPV)测定其还原峰电流与NO_2~-的浓度在2.0 ×10~(-6)~2.0 × 10~(-4)mol/L范围内呈良好的线性关系,相关系数为0.9953,检测限5.0×10~(-7)mol/L。该电极用于模拟水样中NO_2~-的测定,结果满意。
A phosphomolybdic heteropoly-L-cysteine self-assembled supramolecular membrane electrode (P2Mo18-L-Cys / Au) was prepared. The composition of the membrane was characterized by ATR-FTIR spectroscopy. The electrochemical properties of the membrane electrode were investigated and it was found that there were two pairs of stable and reversible redox peaks in CV scan between 0.0 and 0.7 V (vs.SCE) in 1.0 mol / L H2SO4 solution. The peak potentials were Em1 = 0.334 V and Em2 = 0.188 V, corresponding to the two-step2electron-2 proton reaction of P2Mo18O_ (62) ~ (6-) .The chronocoulometry method was used to calculate the electron transfer coefficient D is 5.01 × 10 ~ (-8) cm2 · s ~ (-1). The membrane electrode has obvious electrocatalytic reduction effect on NO 2 - in acidic solution, and the electrocatalytic mechanism was discussed preliminarily. The peak current and the concentration of NO_ (2) were measured by differential pulse voltammetry (DPV) in the range of 2.0 × 10 -6 -6.0 × 10 -4 mol / L The correlation coefficient was 0.9953 and the detection limit was 5.0 × 10 ~ (-7) mol / L. The electrode was used to simulate the determination of NO 2 - in water samples with satisfactory results.