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纳米氢氧化钴原位修饰碳糊电极固-液微萃取及电化学检测辛硫磷
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作者单位
王佳,朱永春,那宝双,辛士刚,张洪波 1.沈阳师范大学化学化工学院
2.沈阳师范大学能源与环境催化研究所
3.沈阳师范大学实验中心 
基金项目:国家科技部国际合作重大项目(2004DFA02700);国家自然科学基金项目(20875063);辽宁教育厅项目(2004-c022);国家电分析重点实验室项目(2006-06);沈阳市科技局基金项目(2007-GX-32)
中文摘要:运用纳米氢氧化钴原位修饰碳糊电极微分脉冲伏安(DPV)法检测了辛硫磷。在外加电位下辛硫磷分子被萃取到电极表面,并与纳米氢氧化钴相互作用形成络合物,在-0.489 V处得到1还原峰,且还原峰电流随扫速线性增长,表明电极上的还原过程受吸附控制。吸附过程满足Temkin等温吸附模型。pH与电位的关系表明辛硫磷的还原过程为1电子1个质子反应。运用交流阻抗方法考察了反应过程,并辅以理论计算,表明反应为自发过程,计算结果与循环伏安法一致。采用该体系检测辛硫磷,其还原峰电流与辛硫磷浓度的对数分别在3.333×10-13~3.333×10-8 mol/L和3.333×10-8~3.333×10-6 mol/L范围内呈线性关系,检出限(S/N=3)可达3.333×10-13 mol/L。该方法具有良好的重现性及选择性,用于菠菜中辛硫磷农药的检测,结果满意。
中文关键词:纳米氢氧化钴  碳糊电极  辛硫磷
 
Electrochemistry Determination of Phoxim Based on Solid liquid Microextraction on Nanoparticle Cobalt Hydroxide in situ Modified Carbon Paste Electrode
Abstract:A differential pulse voltammetric(DPV) method was developed for the detection of phoxim based on solid liquid microextraction on nanoparticle cobalt hydroxide in situ modified carbon paste electrode.Phoxim was detected by with nanoparticle cobalt hydroxide in-situ modified carbon paste electrode.Under the applied potential,phoxim molecules were extracted onto the electrode surface,which interacted with cobalt hydroxide to form a complex and result in an irreversible reduction peak at-0489 V.The reduction peak current increased linearly with the increase of scan rate,indicating that the reduction reaction was controlled by surface adsorption.The extraction behavior followed a Temkin isothermal adsorption model.The relationship between pH and potential showed that the reduction process was just a reaction of an electron with a proton.Electrochemical impedance spectroscopy(EIS) and quantum chemical method were used to prove that the reduction reactions could occur spontaneously,while the calculation results were consistent with the experimental results.The system was used to detect phoxim.There existed linear relationships between the reduction peak current and logarithm of phoxim concentration in the ranges of 3.333×10-13-3.333×10-8 mol/L and 3.333×10-8-3.333×10-6 mol/L.The limits of detection(S/N=3) was 3.333×10-13 mol/L.With good reproducibility and selectivity,the method was applied in the determination of phoxim pesticides in spinach with satisfactory results.
Key Words:nanoparticle cobalt hydroxide  carbon paste electrode  phoxim
引用本文:王佳,朱永春,那宝双,辛士刚,张洪波.纳米氢氧化钴原位修饰碳糊电极固-液微萃取及电化学检测辛硫磷[J].分析测试学报,2019,(4):403-410.
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