摘要
制备了聚二-（1,10-邻菲啰啉）（1,10-邻菲啰啉-5,6-二酮）合钌修饰玻碳电极,研究了在非水介质中与水反应后的电极反应,成功构建了一种检测微量水的电化学传感器,建立了在非水介质中检测有机物中微量水的电化学分析法。在含有0.05 mol/L六氟磷酸四丁基胺的乙腈溶液中,采用差分脉冲伏安法,在电位!0.12 V处测得的阳极峰电流与水含量在0.02%＂5.66%范围内成正比,检出限为0.005%（S/N=3）。将传感器分别应用于乙腈、丙酮、93号汽油、柴油4种有机物中微量水的测定,相对标准偏差小于3.6%,加标回收率为94.1%~105.0%,测定结果与卡尔费休法相符。
A glassy-carbon electrode modified with electropolymerized [ Ru （1,10-phenanthroline） 2 （ 1,10- phenanthroline-5,6-dione） 2＋] （pF6 ）2 was prepared and the electrode reaction of the ruthenium complex on the electrode surface with water in non-aqueous media was investigated. The electrode was employed as working electrode of electrochemical sensor to develop a simple and convenient method for detecting trace water in organic compounds. Based on the selective response of the sensor, the trace water in organic compounds could be monitored by using the differential pulse vohammetry in non-aqueous medium. In acetonitrile solution containing 0.05 molZL tetrabutyl ammonium hexafluorophosphate, the anodic peak currents of the modified electrode at potential of -0.12 V were proportional to water content in the range of 0.02% -5.66% with a linear correlation coefficient of 0.9994, and the detection limit for water was estimated to be 0.005% （ S/N= 3）. The sensor was successfully applied to detect the trace water in acetonitrile, acetone, 93 gasoline and diesel oil. The results were consistent with those of the Karl Fischer method with the relative standard deviation of less than 3.6%, and the recovery was 94.1% -105.0%.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2015年第5期729-733,共5页
Chinese Journal of Analytical Chemistry
基金
国家自然科学基金(No.21475072)
精细化工国家重点实验室开放基金项目(KF0508)资助~~
