Cheng Junqi, Li Qing, Zhao Mingyue, Wang Zheng
Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai, 201899, China; Center of Materials Science and Optoelectronics Engineering, University of Chinese Academy of Sciences, Beijing, 100049, China.
Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai, 201899, China; East China University of Science and Technology, Shanghai, 200237, China.
Anal Chim Acta. 2019 Oct 24;1077:107-115. doi: 10.1016/j.aca.2019.06.003. Epub 2019 Jun 4.
A novel method for the determination of ultratrace Pb in seawater by solution-cathode glow discharge atomic emission spectrometry (SCGD-AES) coupled with hydride generation (HG) has been developed. In the SCGD process, the hollow Ti tube, which can introduce gas instead of a solid tungsten rod is used as a discharge anode and combined with hydride generator. HG technology can not only separate Pb from a seawater matrix and reduce the matrix interference on detection, but can also significantly improve the transfer and atomization efficiencies for SCGD-AES. The optimum working conditions for HG and SCGD-AES for quantitative analysis of Pb were determined as 1% HCO as the masking agent and addition of 3% formic acid to increase Pb volatilization. The limit of detection (LOD) for Pb was decreased by two orders of magnitude in comparison to the SCGD-AES process alone. Under optimal conditions, the LOD for Pb was 0.17 μg L, and the relative standard deviation was 2.1% (n = 11) for 100 μg L Pb in artificial seawater. The proposed quantification method was verified using a seawater reference material (BWQ7001-2016), and the obtained results agreed well with certified values. Finally, the approach was used to quantitatively analyse Pb in seawater, and the results agreed well with those obtained by inductively coupled plasma mass spectrometry. The recoveries of standard addition were between 96.0% and 103.0%.
开发了一种通过溶液阴极辉光放电原子发射光谱法(SCGD-AES)结合氢化物发生(HG)测定海水中超痕量铅的新方法。在SCGD过程中,使用可引入气体而非固体钨棒的空心钛管作为放电阳极,并与氢化物发生器结合。HG技术不仅可以将铅与海水基体分离,减少基体对检测的干扰,还可以显著提高SCGD-AES的传输和雾化效率。HG和SCGD-AES用于铅定量分析的最佳工作条件确定为:以1% HCO作为掩蔽剂,并添加3%甲酸以提高铅的挥发度。与单独的SCGD-AES过程相比,铅的检测限(LOD)降低了两个数量级。在最佳条件下,铅的LOD为0.17 μg L,人工海水中100 μg L铅的相对标准偏差为2.1%(n = 11)。使用海水标准物质(BWQ7001-2016)验证了所提出的定量方法,获得的结果与认定值吻合良好。最后,该方法用于海水中铅的定量分析,结果与电感耦合等离子体质谱法获得的结果吻合良好。标准加入法的回收率在96.0%至103.0%之间。