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 Hg^2+in Water with Enrichment-Part Elution-Solid Phase Spectroscopy

作　　者：朱莹 李龙[1] 江成德 边丽 杨仕骏 倪晨杰 杜一平[1] ZHU Ying;LI Long;JIANG Chengde;BIAN Li;YANG Shijun;NI Chenjie;DU Yiping(Shanghai Key Laboratory of Functional Materials Chemistry,East China University of Science and Technology,Shanghai 200237,China;Preekem Scientific Instruments Co.Ltd,Shanghai 201108,China)

机构地区：[1]华东理工大学上海市功能性材料化学重点实验室,上海200237 [2]上海屹尧仪器科技发展有限公司,上海201108

出　　处：《华东理工大学学报（自然科学版）》2020年第6期753-757,共5页Journal of East China University of Science and Technology

基　　金：上海市科委科研计划项目(17142201100)。

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0.5~30μg/L,相关系数(R2)为0.993,检出限为0.444μg/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%。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 0.5−30μg/L with a squared correlation coefficient of 0.993,and the limit of detection is 0.444μg/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.

关 键 词：固相萃取光谱 Hg2+ 可见光谱 掩蔽 污水 

分 类 号：O652[理学—分析化学]