应用化学 ›› 2010, Vol. 27 ›› Issue (10): 1225-1229.DOI: 10.3724/SP.J.1095.2010.90845

• 研究论文 • 上一篇    下一篇

纳米TiO2微柱分离富集测定环境样品中的微量碲

张蕾*,张敏,康平利,李娜   

  1. (辽宁大学化学院 沈阳 110036)
  • 收稿日期:2009-12-16 修回日期:2010-02-04 出版日期:2010-10-10 发布日期:2010-10-10
  • 通讯作者: 张蕾,女,博士,教授; E-mail:zhanglei63@126.com; 研究方向:稀散元素分离富集
  • 基金资助:
    辽宁省自然科学基金(20082051)资助项目;辽宁省高等学校优秀人才支持计划(2009R30)

Preconcentration and Separation of Trace Tellurium in Environmental Samples by Nanometer TiO2 Microcolumn

ZHANG Lei*, ZHANG Min, KANG Ping-Li, LI Na   

  1. (College of Chemistry,Liaoning University,Shenyang 110036)
  • Received:2009-12-16 Revised:2010-02-04 Published:2010-10-10 Online:2010-10-10

摘要:

以处理过的纳米TiO2为微柱吸附材料,采用流动注射技术进行微量碲的分离富集,探讨了溶液的pH值、试样流速、试样体积、洗脱液浓度和用量以及干扰离子等因素的影响。 实验结果表明,pH值在8~9.5范围内,纳米TiO2对Te(Ⅳ)具有良好的吸附性能,吸附率接近99%,动态饱和吸附容量为37.02 mg/g;选用2 mL 0.5 mol/L NaOH溶液可将吸附的Te(Ⅳ)完全洗脱,富集倍数为30。 本法的检出限(3σ)为0.013 mg/L,相对标准偏差为RSD=1.99%。 将本法应用于水样的分析,碲的回收率在98%~103%之间,结果令人满意。

关键词: 流动注射, 微柱分离, 纳米二氧化钛,

Abstract:

A new method using a microcolumn packed with nanometer TiO2 as solidphase extractant was developed for the preconcentration and separation of trace amounts of Te(Ⅳ) prior to its measurement by ultraviolet spectrophotometry. Effects of pH, sample flow rate and volume, elution solution and coexisted ions on the recovery of the analytes were investigated. The sorption was optimized with respect to the pH, the maximum sorption was achieved from the solution of pH 8~9.5, and the adsorption percentage was 99%. Sorbed Te(Ⅳ) was desorbed in 2.0 mL of 0.5 mol/L NaOH, with an enrichment factor of 30. The detection limit(3σ) of the method for Te(Ⅳ) was 0.013 mg/L(n=13); and the relative standard deviation was 1.99%(n=13, c=30 mg/L). At room temperature, the dynamic saturated adsorption capacity was 37.02 mg/g. The proposed method was applied to the determination of trace amounts of Te(Ⅳ) in water samples, the determined values were in good agreement with the certified values.

Key words: flow injection, microcolumn preconcentration, titanium dioxide, tellurim

中图分类号: