应用化学 ›› 2009, Vol. 26 ›› Issue (6): 738-741.

• 研究论文 • 上一篇    下一篇

磷酸盐缓冲介质电化学氢化物发生原子荧光法测定环境样品中的锑

张王兵   

  1. 安徽工业大学
  • 收稿日期:2008-05-12 修回日期:2008-09-17 出版日期:2009-06-10 发布日期:2009-06-10
  • 通讯作者: 张王兵

Determination of Sb in environment samples by atomic fluorescence spectrometry and electrochemical hydride generation in phosphate buffer solution

  • Received:2008-05-12 Revised:2008-09-17 Published:2009-06-10 Online:2009-06-10

摘要:

本文通过对传统的电化学氢化物发生技术进行改进,使用中性磷酸盐缓冲体系作为电解质,研究锑化氢的电解生成情况。实验发现在磷酸盐缓冲体系中, Sb(III)的响应信号比酸性介质中提高了一倍,同时Sb(V)几乎没有响应信号,因此可以在缓冲体系中进行价态分析;同时使用中性缓冲体系消除了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;对传统的平板式电解池进行了改进,利用螺纹密封的方式代替螺丝密封,电解池安装时间从原来的20分钟缩短为1分钟,并且提高了密封性能,同时有效地解决了电解池渗漏问题。对各种实验参数进行了详细的研究,检出限为0.038μg/L (3σ),相对标准偏差为3.9%(,n=11)。利用该体系分析了多种环境样品中的锑,结果满意。

关键词: 电化学氢化物发生, 电解质, 磷酸盐缓冲体系, 锑, 电化学氢化物发生, 电解质, 磷酸盐缓冲体系,

Abstract:

A novel system for determination Sb by electrochemical hydride generation in phosphate buffer solution was studied. It was found that the use of neutral phosphate buffer solution could markedly increase the fluorescence intensity of Sb (III) and suppress totally signal of Sb (V). The analysis of Sb valence could be carried out in buffer solution. Moreover, it has some merits like reducing self-erodible effect of cathode materials, prolonging the lifetime of cell and increseing stability of signal. The traditional thin-type cell was improved and a new cell with screw-thread for easy dismounting, named disk type cell, was developed. Assembly time of the disk cell is only about 1 min, and the time of analytical process is shortened largely compared with the other cells because the time of assembling eight or ten screws is about 20 minutes. Secondly, sealing performance of this cell is better than the traditional electrolytic cell, which is held together with several screws or epoxy resin. The effects of the electrolytic conditions and interferences ion on the EcHG have been studied. The detection limits (3? of 0.038 礸/L Sb (III) in aqueous solutions were obtained, respectively. The precisions (n=11) for 20 礸/L Sb(III) was 3.9%,. This system has been applied satisfactorily to the determination of Sb in environment samples.

Key words: Electrochemical hydride generation, electrolyte, phosphate buffer solution, antimony