色谱 ›› 2013, Vol. 31 ›› Issue (3): 281-285.DOI: 10.3724/SP.J.1123.2012.10034

• 技术与应用 • 上一篇    

二维离子色谱法同时测定环境水样中的碘离子、硫氰酸根和高氯酸根

林立1,3*, 王海波2, 史亚利2   

  1. 1. 国家食品质量安全监督检验中心, 北京 100094; 2. 中国科学院生态环境研究中心 环境化学与生态毒理学国家重点实验室, 北京 100085; 3. 北京工业大学,北京100022
  • 收稿日期:2012-11-06 修回日期:2012-12-21 出版日期:2013-03-28 发布日期:2013-03-22
  • 通讯作者: 林立
  • 基金资助:

    质检公益性行业科研专项(201110042);国家重大科学仪器设备开发专项(2012YQ090229).

Determination of iodide, thiocyanate and perchlorate ions in environmental water by two-dimensional ion chromatography

LIN Li1,3*, WANG Haibo2, SHI Yali2   

  1. 1. China National Food and Safety Supervision and Inspection Center, Beijing 100094, China; 2. State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China; 3. Beijing University of Technology, Beijing 100022, China
  • Received:2012-11-06 Revised:2012-12-21 Online:2013-03-28 Published:2013-03-22
  • Contact: Li Lin

摘要: 建立了二维离子色谱法同时测定环境水样中的碘离子、硫氰酸根离子和高氯酸根离子的方法。先采用常规阴离子色谱柱(IonPac AS16, 250 mm×4 mm)将水样中的碘离子、硫氰酸根离子和高氯酸根离子与干扰离子进行分离。样品溶液通过抑制器后,将含有碘离子、硫氰酸根离子和高氯酸根离子的淋洗液导入富集柱(MAC-200, 80 mm×0.75 mm),再通过毛细管阴离子色谱柱(IonPac AS20 Capillary, 250 mm×0.4 mm)进行分离和定量分析。方法的线性范围为0.05~100 μg/L,相关系数达到0.9999,检出限为0.02~0.05 μg/L。样品中碘离子、硫氰酸根离子和高氯酸根离子的加标回收率在85.1%~100.1%之间,回收率的相对标准偏差(RSD)(n=6)在1.7%~4.9%之间。该法试剂用量小,灵敏度比常规离子色谱提高30~40倍,同时去除了样液中的高浓度基体杂质,适用于水样中低含量碘离子、硫氰酸根离子和高氯酸根离子的检测。

关键词: 地表水, 碘离子, 二维离子色谱, 高氯酸根离子, 硫氰酸根离子, 毛细管离子色谱

Abstract: A procedure for the determination of iodide, thiocyanate and perchlorate ions in environmental water by two-dimensional ion chromatography has been developed. At first the iodide, thiocyanate and perchlorate ions were separated from interfering ions by a column (IonPac AS16, 250 mm×4 mm). The iodide ion, thiocyanate and perchlorate ions were then enriched with an enrichment column (MAC-200, 80 mm×0.75 mm). In the 2nd-dimensional chromatography, iodide thiocyanate and perchlorate ions were separated and quantified by a capillary column (IonPac AS20 Capillary, 250 mm×0.4 mm). The linear ranges were 0.05-100 μg/L with correlation coefficients of 0.9999, and the detection limits were 0.02-0.05 μg/L. The spiked recoveries of iodide, thiocyanate and perchlorate ions were in the range of 85.1% to 100.1%. The relative standard deviations of the recoveries were 1.7% to 4.9%.

Key words: capillary ion chromatography (CIC), iodide ion, perchlorate ion, surface water, thiocyanate ion, two-dimensional ion chromatography