应用化学 ›› 2010, Vol. 27 ›› Issue (09): 1088-1092.DOI: 10.3724/SP.J.1095.2010.90751

• 研究论文 • 上一篇    下一篇

痕量铜的流动注射-固相萃取-光度法测定

樊静1,2,3*,叶存玲1,秦玉霞1,朱桂芬1,2,3,冯素玲1   

  1. (1.河南师范大学化学与环境科学学院;2.河南省环境污染控制重点实验室;
    3.黄淮水环境与污染防治省部共建教育部重点实验室 新乡 453007)
  • 收稿日期:2009-11-13 修回日期:2010-03-29 出版日期:2010-09-10 发布日期:2010-09-10
  • 通讯作者: 樊静,女,博士,教授; E-mail:fanjing@henannu.edu.cn; 研究方向:环境分析化学
  • 基金资助:
    高等学校博士学科点专项科研基金项目(200804760004);河南省科技攻关计划重点项目(072102320007)

Determination of Trace Amounts of Copper Using a Catalytic Kinetic Spectroscopy Coupled with On-line Flow Injection and Solid-phase Extraction

FAN Jing1,2,3*, YE Cun-Ling1, QIN Yu-Xia1, ZHU Gui-Fen1,2,3, FENG Su-Ling1   

  1. (1.College of Chemistry and Environmental Sciences,Henan Normal University;
    2.Henan Key Laboratory for Environmental Pollution Control;
    3.Key Laboratory for Yellow River and Huaihe River Water Environment
    and Pollution Control,Ministry of Education,Xinxiang 453007)
  • Received:2009-11-13 Revised:2010-03-29 Published:2010-09-10 Online:2010-09-10

摘要:

根据在酸性介质中,Cu2+对溴酸钾氧化藏红T的反应具有催化作用,利用自制的二苯卡巴腙功能键合硅胶做固相萃取固定相,联用流动注射样品处理技术,建立了在线选择性固相萃取催化动力学流动注射光度法测定痕量Cu2+的新方法。 研究了富集时间、反应管长、富集和洗脱流速、反应介质及洗脱液、试剂浓度、反应温度和共存物质的影响。 在最佳实验条件下,对铜测定的线性范围为0.0010~0.60 mg/L,检出限为7.9×10-4 mg/L。 在线分离富集后分析方法的灵敏度提高20多倍,允许干扰物质存在的倍率提高了近10倍。 11次重复测定的相对标准偏差小于2.6%。 一份样品溶液从分离富集处理到测定,仅需6 min和6 mL试剂。 方法已用于中药和茶叶中痕量铜的测定。

关键词: 固相萃取, 催化动力学, 流动注射光度法,

Abstract:

A new flow-injection catalytic kinetic spectroscopy was developed for the determination of Cu2+ based on its catalytic activity on the oxidation of safranine T by potassium bromate in sulfuric acid solution. Cu2+ can be separated and enriched on-line by using a customer designed 1,5-diphenylcarbazone grafted silica gel micro-column coupled with flow injection technology. The determination conditions including the enrichment time, coil length, flow rates of sample, type of eluent, reaction medium, amounts of all reagents, reaction temperature and effects of external ions, were optimized. Under these conditions, the linear range of the concentration determination curve is 0.0010~0.60 mg/L and the detection limit is 7.9×10-4 mg/L. The sensitivity was improved by 20 times and the permitted amounts of some external ions were enhanced at least 10 times than that of a non-preconcentrated step method. The relative standard deviation of eleven replicate measurements is less than 2.6%. One assay cycle only takes 6 min and the total volume of reagents consumed is 6.0 mL. This established method has been applied for the determination of trace amounts of copper in Chinese traditional medicine and tea.

Key words: Solid-phase extraction, catalytic kinetic, flow injection spectrophotometry, copper

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