活性炭富集-电热塞曼原子吸收光谱法测定水中痕量的汞

发布时间：2018-05-23 16:34

本文选题：水 + 汞　；参考：《分析化学》2016年08期

【摘要】：建立了一种水中痕量汞的测定方法。通过活性炭定量吸附水中痕量汞,采用电热塞曼原子吸收光谱法测定活性炭富集的汞。与目前水中总汞测定方法相比,本方法避免了消解等步骤,减少了汞污染和汞损失,操作更加简单。考察了活性炭粒度、酸处理方法、酸介质和富集时间对富集效率的影响,以及热解温度和干扰离子对方法测定结果的影响。通过空白活性炭加标、空白溶液加标和环境水样加标3种方法制作标准曲线,三者的相关系数达0.9999,经统计检验,3条标准曲线的斜率无差异,表明了在此实验条件下环境水样中的共存物不干扰汞的测定,同时也表明可直接用空白活性炭加标的方法进行标准曲线的绘制。采用本方法对含5和50 ng/L汞的水样进行测定,其相对标准偏差分别为7.2%和4.2%(n=11)。本方法测定下限达到1.2 ng/L。地表水和自来水样中添加10 ng/L汞的加标回收率在92.0%~103.0%之间。用ICP-MS作对照,二者分析结果相符合,相对误差在2.9%~3.4%之间,表明本方法准确可靠、精密度好。
[Abstract]:A method for the determination of trace mercury in water was established. Trace mercury in water was quantitatively adsorbed by activated carbon and mercury enriched by activated carbon was determined by electrothermal Zeeman atomic absorption spectrometry. Compared with the present method for the determination of total mercury in water, the method avoids the steps of digestion, reduces mercury pollution and mercury loss, and is simpler to operate. The effects of particle size of activated carbon, acid treatment method, acid medium and enrichment time on the enrichment efficiency, as well as the effects of pyrolysis temperature and interference ions on the determination results were investigated. The standard curves were made by three methods: blank activated carbon, blank solution and environmental water. The correlation coefficient of the three curves was 0.9999, and the slope of the three standard curves was not different by statistical test. It is shown that the coexistence in the environmental water sample does not interfere with the determination of mercury under this experimental condition, and that the standard curve can be drawn directly by the method of adding standard activated carbon. Water samples containing 5 and 50 ng/L mercury were determined by this method. The relative standard deviations were 7.2% and 4.2%, respectively. The lower limit of this method is 1.2 ng / L. The recoveries of adding 10 ng/L mercury to surface water and tap water samples were between 92.0% and 103.0%. The results of ICP-MS analysis were in agreement with each other, and the relative error was between 2.9% and 3.4%, which indicated that the method was accurate, reliable and accurate.
【作者单位】：中国广州分析测试中心广东省测试技术公共实验室广东省化学危害应急检测技术重点实验室;
【基金】：国家自然科学基金(21307120) 广东省科技计划项目(2015A020218001)资助~~
【分类号】：O657.31;X832

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