高等学校化学学报

高等学校化学学报 ›› 2010, Vol. 31 ›› Issue (10): 1949.

• 研究论文 • 上一篇    下一篇

在线固相氧化物吸附-火焰原子吸收法测定痕量银

于洪梅1,2, 朱秀慧2 , 陈明丽1, 田永1, 王建华1   

  1. 1. 东北大学分析科学研究中心, 沈阳 110819;
    2. 辽宁科技大学化工学院, 鞍山 114051
  • 收稿日期:2010-04-07 出版日期:2010-10-10 发布日期:2010-10-10
  • 通讯作者: 王建华, 男, 博士, 教授, 博士生导师, 主要从事流动注射分析技术及样品预处理研究. E-mail: jianhuajrz@mail.neu.edu.cn
  • 基金资助:

    国家杰出青年科学基金(批准号: 20725517), 国家自然科学基金重大国际合作项目(批准号: 20821120292), 国家自然科学基金(批准号: 20805004)及中央高校基本科研业务费资助项目(批准号: N090105001, N090605001, N090405004)资助.

Determination of Trace Silver in Water Samples by On-line Solid Phase Oxide Collection-Flame Atomic Adsorption Spectrometry

YU Hong-Mei1,2, ZHU Xiu-Hui2, CHEN Ming-Li1, TIAN Yong1, WANG Jian-Hua1*   

  1. 1. Research Center for Analytical Sciences, Northeastern University, Shenyang 110819, China;
    2. School of Chemical Engineering, Liaoning University of Science and Technology, Anshan 114051, China
  • Received:2010-04-07 Online:2010-10-10 Published:2010-10-10
  • Contact: WANG Jian-Hua. E-mail: jianhuajrz@mail.neu.edu.cn
  • Supported by:

    国家杰出青年科学基金(批准号: 20725517), 国家自然科学基金重大国际合作项目(批准号: 20821120292), 国家自然科学基金(批准号: 20805004)及中央高校基本科研业务费资助项目(批准号: N090105001, N090605001, N090405004)资助.

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被引次数

8

摘要： 基于硅胶表面对碱性体系中新生成的氧化银(Ag2O)的有效吸附, 建立了流动注射-固相氧化物分离富集-火焰原子吸收法测定痕量银的方法. 当银以氧化物的形式被滞留在硅胶固相表面时, 硅胶表面的硅醇基和表面电荷有利于反应体系中新生成的Ag2O胶状沉淀的吸附, 将收集的沉淀用HNO3(10%, 体积分数)洗脱后用火焰原子吸收测定. 当进样体积为5.4 mL时, 测得的富集系数为25.5, 检出限为0.6 μg/L, 采样频率为50次/h, 线性范围为2~150 μg/L, 相对标准偏差(RSD)为2.0%(40 μg/L, n=11). 将该法用于自来水、河水、井水、雪水和山泉水中银含量的测定, 加标回收率分别为93.3%, 89.5%, 96.6%, 108.4%和102.8%.

关键词: 流动注射, 固相氧化物吸附, 氧化银, 火焰原子吸收法

Abstract: A novel flow injection-solid phase oxide collection-flame atomic adsorption spectrometry(FAAS) was developed for the determination of trace silver in water samples using sodium hydroxide as precipitating reagent and silica beads as adsorbent. Silver was precipitated in form of oxide and then collected on solid phase surface of silica beads packed micro-column as oxide collector. The silanol groups and surface charges on the surface of silica beads contribute to precipitation adsorption of Ag2O. The precipitate was afterwards quantitatively eluted by 10%(volume fraction) nitric acid with the detection by FAAS. By loading 5.4 mL sample solution, an enrichment factor of 25.5, a detection limit(3σ) of 0.6 μg/L and a sampling frequency of 50 times/h were achieved, along with a linear range within 2—150 μg/L and a precision of 2.0% RSD at the 40 μg/L level(n=11). The present procedure was applied for the determination of silver by spiking recoveries in tap water, river water, well water, snow water and spring water, and the spiking recoveries were 93.3%, 89.5%, 96.6%, 108.4% and 102.8%, respectively.

Key words: Flow injection, Solid phase oxide adsorption/collection, Silver oxide, Flame atomic adsorption spectrometry

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