交联壳聚糖富集分离-石墨炉原子吸收光谱法测定痕量钯的研究

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摘要：将环氧氯丙烷与壳聚糖进行交联反应制备了不溶于酸、碱的交联壳聚糖(CCTS)，研究了不同pH条件下CCTS对于Pd(Ⅱ)的吸附特性，结果表明：在pH 1～4时，吸附20 min，CCTS对Pd(Ⅱ)的吸附率达98%以上;考察了吸附时间、试样体积、CCTS用量、共存元素等对CCTS吸附Pd(Ⅱ)的影响、吸附容量以及Pd(Ⅱ)的脱附;探讨了吸附机理;建立了CCTS预富集分离, 石墨炉原子吸收光谱(GFAAS)测定痕量钯的新方法。该法检出限(3σ, n=8 )为0.143 μg·L^-1,相对标准偏差(RSD)小于5.47%, 用于湖水和海水中痕量钯的检测, 回收率在92%～96%之间。该法还可用于钯的回收利用。

关键词：交联壳聚糖;预富集;分离;钯;石墨炉原子吸收光谱法

Abstract：A novel crosslinked chitosan(CCTS) not dissolved in acidic or alkaline solutions was synthesized by the crosslinking reaction of chitosan (CTS) with crosslinking agent (3-chloro-1,2-epoxypropane). The adsorption capability of Pd(Ⅱ) by CCTS was studied at different pH value. The results showed that the adsorption efficiency was above 98% after preconcentration for 20 minutes when pH values were 1-4. The effects of preconcentration time, dosage of CCTS, adsorption capacity of CCTS, sample volume, coexistent elements, and elution of Pd(Ⅱ) were investigated. The mechanism of adsorption of CCTS for Pd(Ⅱ) was discussed. A novel method for the preconcentration and separation of trace Pd(Ⅱ) with crosslinked chitosan(CCTS) and its determination in water by graphite furnace atomic absorption spectrometry has been developed. The detection limit(3σ, n=8) was 0.143 μg·L^-1,the relative standard deviation(RSD) was less than 5.47%, and this preconcentration method was used to detect Pd(Ⅱ) in lake water and sea water with recoveries of 92%-96%. It also can be used to recycle Pd(Ⅱ).

Key words：Crosslinked chitosan;Preconcentration;Separation;Palladium;GFAAS

收稿日期: 2005-12-06 修订日期: 2006-03-30

中图分类号:

O657.3

通讯作者: 向罗京 E-mail: roking2008@hotmail.com

引用本文:

钱沙华,向罗京^*,邓红兵，肖玫，林翰，黎雪琴 . 交联壳聚糖富集分离-石墨炉原子吸收光谱法测定痕量钯的研究[J]. 光谱学与光谱分析, 2007, 27(03): 592-594.
QIAN Sha-hua, XIANG Luo-jing^*,DENG Hong-bing, XIAO Mei, LIN Han, LI Xue-qin. Preconcentration of Trace Pd(Ⅱ) on Crosslinked Chitosan and Determination by Graphite Furnace Atomic Absorption Spectrometry . SPECTROSCOPY AND SPECTRAL ANALYSIS, 2007, 27(03): 592-594.

链接本文:

https://www.gpxygpfx.com/CN/Y2007/V27/I03/592