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使用巯基葡聚糖凝胶预富集后,用分光光度法测定水中痕量铅。

Spectrophotometric determination of trace lead in water after preconcentration using mercaptosephadex.

作者信息

Zaijun Li, Yuling Yang, Jian Tang, Jiaomai Pan

机构信息

College of Chemical and Material Engineering, Southern Yangtze University, Wuxi 214036, China(1).

出版信息

Talanta. 2003 May 28;60(1):123-30. doi: 10.1016/S0039-9140(03)00115-2.

Abstract

A highly sensitive and selective spectrophotometric method for determination of trace lead in water after pre-concentration using mercaptosephadex (MS-50) has been developed, the method based on the color reaction of lead(II) with dibromohydroxylphenylporphyrin. Under optimal condition, lead(II) reacts with the reagent to form a 1:2 yellow complex in presence of TritonX-100, which has a maximum absorption peak at 479 nm. The color reaction can complete rapidly and remain stable for 24 h in room temperature. The molar absorption coefficient of the lead complex, the limit of quantification, the limit of detection and relative standard deviations were found to be 2.35x10(5) l mol(-1) cm(-1), 4.3, 1.4 ng ml(-1) and 1.0%, respectively. The absorbance of the lead complex at 479 nm is linear up to 0.48 mug ml(-1) of lead(II). The effect of various co-existing ions in water were examined seriously. No interference was observed. Moreover, a simple pre-concentration method for trace lead in water was also studied using MS-50. It was found that trace lead in water can be adsorbed in 1.0 mol l(-1) HCl and dissociated from MS-50 with 4.0 mol l(-1) HCl quantitatively, that improves the selectivity and the sensitivity of method (its detection limit (3 s) changed into 0.2 ng ml(-1) of lead) obviously. The proposed method has been applied to determine trace lead in water samples with satisfactory results.

摘要

建立了一种高灵敏度和选择性的分光光度法,用于在使用巯基葡聚糖(MS - 50)预富集后测定水中的痕量铅。该方法基于铅(II)与二溴羟基苯基卟啉的显色反应。在最佳条件下,铅(II)与试剂在TritonX - 100存在下反应形成1:2的黄色络合物,其在479 nm处有最大吸收峰。显色反应能迅速完成,在室温下可稳定24小时。铅络合物的摩尔吸收系数、定量限、检测限和相对标准偏差分别为2.35×10⁵ l·mol⁻¹·cm⁻¹、4.3、1.4 ng·ml⁻¹和1.0%。铅络合物在479 nm处的吸光度在铅(II)浓度高达0.48 μg·ml⁻¹时呈线性关系。认真研究了水中各种共存离子的影响,未观察到干扰。此外,还研究了使用MS - 50对水中痕量铅的一种简单预富集方法。发现水中的痕量铅能在1.0 mol·l⁻¹ HCl中被吸附,并能用4.0 mol·l⁻¹ HCl从MS - 50中定量解离,这明显提高了方法的选择性和灵敏度(其检测限(3s)变为0.2 ng·ml⁻¹的铅)。所提出的方法已应用于测定水样中的痕量铅,结果令人满意。

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