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无液池紫外-可见微分光光度法测定水中碘酸盐的液-液微萃取法。

Determination of iodate in waters by cuvetteless UV-vis micro-spectrophotometry after liquid-phase microextraction.

机构信息

Departamento de Química Analítica y Alimentaria, Area de Química Analítica, Facultad de Química, Universidad de Vigo, Campus As Lagoas-Marcosende s/n, 36310 Vigo, Spain.

出版信息

Talanta. 2010 Apr 15;81(1-2):625-9. doi: 10.1016/j.talanta.2009.12.053. Epub 2010 Jan 11.

DOI:10.1016/j.talanta.2009.12.053
PMID:20188973
Abstract

The combination of liquid-phase microextraction and microvolume UV-vis spectrophotometry has been applied to the determination of iodate in natural water samples. The method is based on the reduction of iodate into vapor iodine and extraction of this volatile onto a single drop of N,N'-dimethylformamide. The following derivatization reaction was employed: Optimum conditions employed for iodate determination were as follows: 2.5 microL N,N'-dimethylformamide exposed to the headspace of a 10 mL acidic (HCl 0.2 mol L(-1)) aqueous solution stirred at 1400 rpm for 7 min after addition of 1 mL of KI 10(-3)mol L(-1) for in situ iodine generation. The limit of detection was determined as 1.1 microg L(-1). The repeatability, expressed as relative standard deviation, was 4.2% (n=6). A large preconcentration factor (i.e. 396) was obtained in only 7 min.

摘要

液相微萃取和微量紫外可见分光光度法的组合已应用于天然水样中碘酸盐的测定。该方法基于将碘酸盐还原成气态碘,并将这种挥发性物质萃取到一滴 N,N'-二甲基甲酰胺上。采用以下衍生化反应:

对于碘酸盐的测定,采用了最佳条件:在加入 1 毫升 10-3mol/L 的 KI 后,将 2.5 微升 N,N'-二甲基甲酰胺暴露于 10 毫升酸性(HCl 0.2 mol/L)水溶液的顶空,在 1400 rpm 下搅拌 7 分钟,用于原位生成碘。检测限定为 1.1 微克/升。重复性,以相对标准偏差表示,为 4.2%(n=6)。仅在 7 分钟内即可获得大的浓缩因子(即 396)。

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