电化学氢化物发生原子荧光法测定环境样品中的锑  

Determination of Sb in Environment Samples by Atomic Fluorescence Spectrometry Coupled with Electrochemical Hydride Generation

作　　者：张王兵[1] 

机构地区：[1]安徽工业大学化工学院应用化学系,马鞍山243002

出　　处：《应用化学》2009年第6期738-741,共4页Chinese Journal of Applied Chemistry

基　　金：安徽省科技攻关计划(08010304219)资助项目

摘　　要：使用中性磷酸盐缓冲体系作为电解质,研究了锑化氢的电解生成情况。结果发现,Sb(Ⅲ)的原子荧光光谱(AFS)响应信号强度比在酸性介质中提高了1倍,而Sb(Ⅴ)几乎没有响应信号,因此可以在此缓冲体系中进行价态分析,可消除酸性介质对电极的腐蚀,延长了电解池及电极的使用寿命,提高了信号的稳定性。将传统的平板式电解池的螺丝密封改进为螺纹密封,使电解池安装时间从原来的20 min缩短为1 min,提高了电解池的密封性能。Sb(Ⅲ)的检出限为0.038μg/L(3σ),相对标准偏差为3.9%(n=11)。分析了多种环境样品中的锑,结果满意。A novel sample introduction system for the determination of Sb by electrochemical hydride generation in a phosphate buffer solution （PBS） was developed. It was found that using neutral PBS as electrolytic solution could markedly increase the fluorescence intensity of Sb （ Ⅲ ） and suppress totally the signal of Sb （ Ⅴ ）. The valence analysis of Sb could be carried out in buffer solution. Moreover, it has some merits like reducing self-erodible effect of the cathode material, prolonging the lifetime of the cell and increasing the signal stability. The traditional thin-type cell was improved and a new cell with screw-thread was developed. Assembly time of the disk cell was only about 1 min, shortened largely compared with that for the traditional cells of about 20 min. Furthermore, sealing performance of this cell was better than that of the traditional electrolytic. The detection limit（3σ） and the precisions（n = 11 ） for 20 μg/L Sb（ Ⅲ ） were 0. 038 μg/L Sb （ Ⅲ ） and 3.9% , respectively. This system has been applied satisfactorily to the determination of Sb in soil samples.

关 键 词：原子荧光光谱法 电化学氢化物发生 电解质 中性磷酸盐缓冲体系 Sb(Ⅲ) Sb(Ⅴ) 

分 类 号：O657[理学—分析化学]