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    朱莹, 李龙, 江成德, 边丽, 杨仕骏, 倪晨杰, 杜一平. 富集-部分洗脱-固相光谱法快速测定水样中痕量汞离子[J]. 华东理工大学学报(自然科学版), 2020, 46(6): 753-757. DOI: 10.14135/j.cnki.1006-3080.20191022001
    引用本文: 朱莹, 李龙, 江成德, 边丽, 杨仕骏, 倪晨杰, 杜一平. 富集-部分洗脱-固相光谱法快速测定水样中痕量汞离子[J]. 华东理工大学学报(自然科学版), 2020, 46(6): 753-757. DOI: 10.14135/j.cnki.1006-3080.20191022001
    ZHU Ying, LI Long, JIANG Chengde, BIAN Li, YANG Shijun, NI Chenjie, DU Yiping. Rapid Determination of Trace Hg2+ in Water with Enrichment-Part Elution-Solid Phase Spectroscopy[J]. Journal of East China University of Science and Technology, 2020, 46(6): 753-757. DOI: 10.14135/j.cnki.1006-3080.20191022001
    Citation: ZHU Ying, LI Long, JIANG Chengde, BIAN Li, YANG Shijun, NI Chenjie, DU Yiping. Rapid Determination of Trace Hg2+ in Water with Enrichment-Part Elution-Solid Phase Spectroscopy[J]. Journal of East China University of Science and Technology, 2020, 46(6): 753-757. DOI: 10.14135/j.cnki.1006-3080.20191022001

    富集-部分洗脱-固相光谱法快速测定水样中痕量汞离子

    Rapid Determination of Trace Hg2+ in Water with Enrichment-Part Elution-Solid Phase Spectroscopy

    • 摘要: 基于实验室研发的固相萃取-固相光谱联用仪测试手段,提出了一种有效解决干扰,快速、灵敏检测河水中Hg2+的方法。以双硫腙为显色剂,将溶液中的Hg2+生成橙色的汞-双硫腙络合物,以混合纤维素膜为富集材料,将该络合物富集到膜上,在膜上进行碱洗去除多余的双硫腙后,直接测定膜的漫反射可见光谱,实现Hg2+的定量分析。采用碱选择性地洗脱过量双硫腙,通过加入乙二胺四乙酸(EDTA)二钠掩蔽剂去除Cu2+、Cd2+对Hg2+的干扰,有效解决了干扰问题。在最佳操作条件下,标准曲线的线性范围为0.5~30 μg/L,相关系数(R2)为0.993,检出限为0.444 μg/L。将该方法用于河水、自来水中Hg2+的检测,加标回收率为91.3%~108.0%,相对标准偏差为2.06%~9.68%。

       

      Abstract: By using a hyphenated solid phase extraction (SPE) and solid phase spectroscopy designed by our group, a rapid, sensitive and selective method for detecting Hg2+ in river water is developed. Hg-dithizone produced with dithizone and Hg2+ can be enriched on a mixed cellulose membrane, and the residual dithizone was removed by washing the membrane with sodium hydroxide solution. Then, visible diffuse reflectance spectroscopy was used for the quantitative analysis of Hg2+ in situ. As such, unwanted interference from other contaminants was minimized by washing the membrane to remove dithizone; EDTA disodium is also added to mask Cu2+ and Cd2+. Under the optimal conditions, the liner range of the method is 0.5−30 μg/L with a squared correlation coefficient of 0.993, and the limit of detection is 0.444 μg/L. The method is applied to the quantification of Hg2+ in tap-water and river water. The recovery rates achieve 91.3%−108.0%, and the relative standard deviations of parallel tests range from 2.06 to 9.68. This work offers a fast method for the determination of Hg2+ in river water with high sensitivity and selectivity.

       

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