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采用结式反应器流动注射在线吸附与氢化物发生原子荧光光谱法间接测定天然水中超痕量硫化物。

Indirect determination of sulfide at ultratrace levels in natural waters by flow injection on-line sorption in a knotted reactor coupled with hydride generation atomic fluorescence spectrometry.

作者信息

Jin Yan, Wu Hong, Tian Ye, Chen Luhong, Cheng Jiongjia, Bi Shuping

机构信息

School of Chemistry and Chemical Engineering, State Key Laboratory of Coordination Chemistry and Key Laboratory of MOE for Life Science, Nanjing University, Nanjing 210093, China.

出版信息

Anal Chem. 2007 Sep 15;79(18):7176-81. doi: 10.1021/ac070699s. Epub 2007 Aug 18.

Abstract

A simple and sensitive nonchromatographic approach for indirect determination of sulfide at ultratrace levels in natural waters based on its selective precipitation with Hg2+ on the inner wall of a knotted reactor (KR) was developed for flow injection on-line sorption coupled with hydride generation atomic fluorescence spectrometry (HG-AFS). With the Hg2+ pH kept at 2.0, the HgS precipitation was formed in the KR after a reaction time of 120 s. A 10% (v/v) HCl was introduced to elute the remnant inorganic mercury and to merge with the KBH4 solution (0.05% m/v) for HG-AFS detection. Under the optimal experimental conditions, the sample throughputs were 20 h(-1). The detection limit was found to be 0.05 microg L(-1), and the relative standard deviation (RSD, n = 11) for determination of 2.0 microg L(-1) sulfide was 3.3%. The developed method was successfully applied to the determination of sulfide in a variety of natural water samples and wastewater samples with the gas-phase separation and sorption apparatus.

摘要

基于硫化物在打结反应器(KR)内壁与Hg2+的选择性沉淀反应,开发了一种简单灵敏的非色谱方法,用于间接测定天然水中超痕量水平的硫化物,该方法用于流动注射在线吸附结合氢化物发生原子荧光光谱法(HG-AFS)。在Hg2+的pH值保持为2.0的情况下,反应120 s后在KR中形成HgS沉淀。引入10%(v/v)的HCl以洗脱残留的无机汞,并与KBH4溶液(0.05% m/v)合并用于HG-AFS检测。在最佳实验条件下,样品通量为20 h-1。检测限为0.05 μg L-1,测定2.0 μg L-1硫化物的相对标准偏差(RSD,n = 11)为3.3%。所开发的方法通过气相分离和吸附装置成功应用于各种天然水样和废水样中硫化物的测定。

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