应用化学 ›› 2010, Vol. 27 ›› Issue (03): 323-327.DOI: 10.3724/SP.J.1095.2010.90206

• 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硒

张蕾*,刘娜,康平利,李绮,周新宇   

  1. (辽宁大学化学学院 沈阳 110036)
  • 收稿日期:2009-03-27 修回日期:2009-06-18 出版日期:2010-03-10 发布日期:2010-03-10
  • 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:
    辽宁省教育厅优秀人才支持项目(2009R30),辽宁省自然科学基金(20082049)资助项目

Nanometer TiO2 Microcolumn Preconcentration of Trace Selenium in Environment Samples

ZHANG Lei*, LIU Na, KANG Ping-Li, LI Qi, ZHOU Xin-Yu   

  1. (College of Chemistry,Liaoning University,Shenyang 110036)
  • Received:2009-03-27 Revised:2009-06-18 Published:2010-03-10 Online:2010-03-10

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硒的分离富集,考察了纳米TiO2微柱对Se(IV)的吸附性能,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在1~6范围内,试样流速为0.5 mL/min,纳米TiO2对Se(IV)具有良好的吸附性能,吸附率可达97%,动态饱和吸附容量为7.92 mg/g;选用1 mL 0.1 mol/L NaOH溶液可将吸附的Se(IV)完全洗脱,富集倍数为40。本法的检出限(3σ)为0.13 mg/L,相对标准偏差为1.56 %。将本法应用于国家标准样品GBW07280的分析,测定值与参考值一致。

关键词: 流动注射,微柱分离,纳米二氧化钛,硒

Abstract:

A method using a microcolumn packed with nanometer TiO2 as solid-phase extractant has been developed for the preconcentration of trace amounts of Se(Ⅳ) prior to the measurement by ultraviolet spectrophotometry. Effects of pH, sample flow rate and volume, elution solution and interfering ions on the recovery of the analytes have been investigated. The sorption was optimized with respect to the pH, maximum sorption was achieved from the solutions of pH 1~ 6. The optimum sample flow rate to adsorb Se(Ⅳ) ions was 0.5 mL/min, and the adsorption percentage was 98.3%. Sorbed Se(Ⅳ) was desorbed with 1.0 mL of 0.1 mol/L NaOH, with an enirchment of 40. The detection limit(3σ) of the method for Se(Ⅳ) was 0.13 mg/L(n=13); and the relative standard deviation was 1.56%(n=13, c=10 mg/L). At room temperature, dynamic saturated adsorption capacity was 7.92 mg/g. The proposed method was applied to the determination of trace amounts of Se(Ⅳ) in GBW07280, the determined value was in good agreement with the certified value.

Key words: heterogemini surfactant CmOhpNC8,NaBr,aqueous solution surface tension,premicellization

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