化学学报 ›› 2013, Vol. 71 ›› Issue (08): 1121-1124.DOI: 10.6023/A13040422 上一篇    下一篇

研究通讯

介质阻挡放电微型化-长光程原子吸收光谱测定汞及甲基汞

于永亮a, 高飞b, 陈明丽b, 王建华b   

  1. a 东北大学化学系 沈阳 110819;
    b 东北大学分析科学研究中心 沈阳 110819
  • 收稿日期:2013-04-18 出版日期:2013-08-14 发布日期:2013-05-16
  • 通讯作者: 王建华, E-mail: jianhuajrz@mail.neu.edu.cn; Tel.: 024-83688944; Fax: 024-83676698 E-mail:jianhuajrz@mail.neu.edu.cn
  • 基金资助:

    项目受国家自然科学基金(Nos. 21005013, 21005011)、国家科技支撑计划(No. 2012BAF14B09)和中央高校基本科研业务费(Nos. N120505004, N110805001, N110705002)资助.

A Miniaturized Long-Optical Path Atomic Absorption Spectrometer with Dielectric Barrier Discharge as Atomizer for Mercury and Methylmercury

Yu Yonglianga, Gao Feib, Chen Minglib, Wang Jianhuab   

  1. a Department of Chemistry, Northeastern University, Shenyang 110819;
    b Research Center for Analytical Sciences, Northeastern University, Shenyang 110819
  • Received:2013-04-18 Online:2013-08-14 Published:2013-05-16
  • Supported by:

    Project supported by the National Natural Science Foundation of China (Nos. 21005013, 21005011), the National Science & Technology Pillar Program (No. 2012BAF14B09) and the Fundamental Research Funds for the Central Universities (Nos. N120505004, N110805001, N110705002).

以介质阻挡放电(DBD)为低温原子化器并引入长光程吸收检测池, 建立了微型化原子吸收光谱系统. 在顺序注射系统中产生的汞及甲基汞蒸气依次经过气液分离器、玻璃棉除水微柱和原子化器然后进入长光程吸收检测池, 进行原子吸收光谱测定. 当DBD原子化器关闭时, 通过冷原子吸收测得无机汞的吸光度, 而当DBD原子化器开启时, 得到无机汞和甲基汞的总吸光度. 在本体系中两种汞形态的吸光度具有很好的加合性, 从而有利于实现无机汞和甲基汞的分别测定. 当进样体积为1.0 mL时, 无机汞与甲基汞的检出限分别为0.3和0.4 μg·L-1, 相对标准偏差均小于4%. 用本微型化原子吸收光谱系统测定了实际样品中的汞及其形态, 证明了该系统的可靠性.

关键词: 介质阻挡放电, 长光程, 原子吸收光谱, 汞, 形态分析

The development of miniaturized instrumentations for specific analytical purposes has been one of the most important momentum in the field of instrumental innovation. Sequential injection system as a miniaturized analytical platform provides an alternative for field of analysis of heavy metal contaminants. It will exhibit more powerful capability with the introduction of atomization function and improvement of detection sensitivity. In this work, a miniature long-optical path atomic absorption spectrometric system is developed with dielectric barrier discharge (DBD) low temperature micro-plasma as atomizer. Mercury and methylmercury vapor is generated in a sequential injection system. It is directed to flow through a gas-liquid separator, a glass wool moisture-removal microcolumn and the DBD atomizer, and finally transported into the long optical-path detection cell for quantitative analysis by atomic absorption spectrometry. A 10 mA lamp current is used with a mercury hollow cathode lamp, and a 260 V negative high voltage for the photomultiplier is set. The detection sensitivity of the present system is highly improved by the increase of absorption optical path (1.1 mm i.d., 400 mm length), and the atomization of hydride is completely achieved by the DBD micro-plasma atomizer. Meanwhile, a glass wool moisture-removal microcolumn integrated in the flow system effectively eliminates the influence of concomitant moisture during the vapor generation process, which avoids the drift of absorbance baseline. The absorbance arising from mercury is recorded by turning off the DBD atomizer, while the total absorbance from both mercury and methylmercury is measured by turning on the DBD atomizer. Further experiments demonstrated satisfactory additivity for the absorbance arising from inorganic and methyl mercury, which provides basis for the determination of mercury and methylmercury. With a sampling volume of 1.0 mL, detection limits of 0.3 and 0.4 μg·L-1 are achieved respectively for inorganic and methylmercury, along with RSD values of <4%. The reliability of the present system is demonstrated by analyzing certified reference materials and real samples for mercury speciation.

Key words: dielectric barrier discharge, long optical-path, atomic absorption spectrometry, mercury, speciation