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用于超声辅助分散微固相萃取汞(II)的磁性石墨相氮化碳纳米复合材料,随后通过原子荧光光谱法定量分析。

Magnetic graphitic carbon nitride nano-composite for ultrasound-assisted dispersive micro-solid-phase extraction of Hg(II) prior to quantitation by atomic fluorescence spectroscopy.

作者信息

Shi Meng-Ting, Yang Xin-An, Zhang Wang-Bing

机构信息

Department of Applied Chemistry, Anhui University of Technology, Maanshan, Anhui 243002, PR China.

Department of Applied Chemistry, Anhui University of Technology, Maanshan, Anhui 243002, PR China.

出版信息

Anal Chim Acta. 2019 Oct 3;1074:33-42. doi: 10.1016/j.aca.2019.04.062. Epub 2019 Apr 29.

DOI:10.1016/j.aca.2019.04.062
PMID:31159937
Abstract

A nanosheet structure of FeO/g-CN magnetic composite has been prepared and utilized as adsorbent for the ultrasound-assisted dispersive magnetic micro-solid-phase extraction of the ultra-trace inorganic mercury [Hg(II)]. Scanning electron microscopy, transmission electron microscopy, X-ray diffraction and Fouries transform infrared spectroscopy images manifested that the hydrothermal systhesis promoted the binding of FeO particles with g-CN. The enrichment performance of composites depended on their compositions, and the recovery of Hg(II) on C-m30 (with FeO/g-CN mass ratio 2:3) was higher than that on other ratios. Recorded data showed that ultrasound wave was an effective method for reducing the agglomeration of magnetic materials and enhancing their adsorption properties. The Hg signal obtained by 80% power input is 3.2 times stronger than the signal by strring mode. X-ray diffraction characterization of the recovered adsorbent showed that g-CN needed to be updated after repeated use for four times. In addition, competitive adsorption may be main factor affecting the inhibitory effect of high concentration methylmercury on inorganic mercury. Under the optimized conditions, the detection limit of the proposed method was 1.4 ng L and relative standard deviation of 4.6% for 0.05 μg L Hg(II) was obtained. The linear calibration range was 0.005-0.4 μg L. The accuracy of the method was verified through analysis of the certificated reference materials. The proposed method has been applied in the determination of inorganic Hg in natural water samples.

摘要

制备了一种FeO/g-CN磁性复合材料的纳米片结构,并将其用作吸附剂,用于超声辅助分散磁性微固相萃取超痕量无机汞[Hg(II)]。扫描电子显微镜、透射电子显微镜、X射线衍射和傅里叶变换红外光谱图像表明,水热合成促进了FeO颗粒与g-CN的结合。复合材料的富集性能取决于其组成,C-m30(FeO/g-CN质量比为2:3)对Hg(II)的回收率高于其他比例。记录的数据表明,超声波是减少磁性材料团聚和增强其吸附性能的有效方法。80%功率输入获得的Hg信号比搅拌模式下的信号强3.2倍。回收吸附剂的X射线衍射表征表明,重复使用四次后需要更新g-CN。此外,竞争吸附可能是影响高浓度甲基汞对无机汞抑制作用的主要因素。在优化条件下,该方法的检测限为1.4 ng L,对于0.05 μg L Hg(II)的相对标准偏差为4.6%。线性校准范围为0.005-0.4 μg L。通过对有证标准物质的分析验证了该方法的准确性。该方法已应用于天然水样中无机汞的测定。

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