Shanghai Key Laboratory of Functional Materials Chemistry, and Research Center of Analysis and Test, East China University of Science and Technology, Shanghai, China.
J Hazard Mater. 2012 Sep 30;233-234:207-12. doi: 10.1016/j.jhazmat.2012.07.016. Epub 2012 Jul 13.
A simple, sensitive and selective solid phase reflectometry method is proposed for the determination of trace mercury in aqueous samples. The complexation reagent dithizone was firstly injected into the properly buffered solution with vigorous stirring, which started a simultaneous formation of nanoparticles suspension of dithizone and its complexation reaction with the mercury(II) ions to make Hg-dithizone nanoparticles. After a definite time, the mixture was filtered with membrane, and then quantified directly on the surface of the membrane by using integrating sphere accessory of the UV-visible spectrophotometer. The quantitative analysis was carried out at a wavelength of 485 nm since it yielded the largest difference in diffuse reflectance spectra before and after reaction with mercury(II).A good linear correlation in the range of 0.2-4.0 μg/L with a squared correlation coefficient (R(2)) of 0.9944 and a detection limit of 0.12 μg/L were obtained. The accuracy of the method was evaluated by the analysis of spiked mercury(II) concentrations determined using this method along with those determined by the atomic fluorescence mercury vapourmeter and the results obtained were in good agreement. The proposed method was applied to the determination of mercury in tap water and river water samples with the recovery in an acceptable range (95.7-105.3%).
本文提出了一种简单、灵敏和选择性的固相反射光度法，用于测定水样中的痕量汞。首先将双硫腙络合剂注入适当缓冲的溶液中，剧烈搅拌，开始同时形成双硫腙纳米粒子悬浮液及其与汞(II)离子的络合反应，生成 Hg-双硫腙纳米粒子。经过一定时间后，将混合物用膜过滤，然后直接在膜表面用紫外可见分光光度计的积分球附件进行定量分析。在与汞(II)反应前后漫反射光谱差异最大的 485nm 波长处进行定量分析。在 0.2-4.0μg/L 范围内得到了良好的线性相关，平方相关系数（R²）为 0.9944，检测限为 0.12μg/L。该方法的准确性通过使用该方法和原子荧光汞蒸气计测定的加标汞(II)浓度的分析进行评估，结果吻合良好。该方法应用于自来水中和河水中汞的测定，回收率在可接受范围内（95.7-105.3%）。
