新型杂多酸[Bu4N][Ni(pph3)2]PW11O39硅溶胶修饰电极电化学性质及电催化研究

The electrochemical property and electrocatalytic study of a novel polyoxometalates [Bu_4N][Ni(pph_3)_2]PW_(11)O_(39) silicon sol modified electrode

采用溶胶-凝胶技术制备了新多金属氧酸盐[Bu4N][Ni（pph3）2]PW11O39（Bu为四丁基，pph为苯基磷）有机．无机杂化材料修饰电极，该修饰电极不仅保持了本体溶液的电化学和电催化性质，而且还具有很好的稳定性与灵敏度．研究表明，优选条件下修饰电极在pH=4．5的缓冲溶液中，其催化电流与NO2^-浓度在6．0×10^-6～1×10^-3mol／L范围内呈良好的线性关系，对不同基质环境水样的加标回收率为97％-102％，方法的检出限为1．0×10^-7mol／L，对1．0×10^-4mol／L NO2^-平行测定10次的相对标准偏差（RSD）为1．96％．

A novel polyoxometalates [Bu4N][Ni（pph3）2]PW11O39 was prepared as organic-inorganic hybrid material for modified electrode by the sol-gel technique. The modified electrode not only maintains its property in solution, but also has high stability and sensitivity. The research results indicate that under selective conditions a catalytic current of the modified electrode shows a favorable linear relation for cNO2^- at range of 6.0 × 10^-6 ～ 1 × 10^-3 mol/L in pH = 4.5 buffered solution. The recoveries of standard addition of nitrite are 97 % - 102%. The detection limit is 1.0 × 10^-7 mol/L （Signal-to-Noise = 3）. The relative standard deviation for 1.0 × 10^-4 mol/L NO2^- is 1.96% （ n = 10）.