Determination of rhodium by resonance light-scattering technique coupled with solid phase extraction using Rh(III) ion-imprinted polymers as sorbent.
Determination of rhodium by resonance light-scattering technique coupled with solid phase extraction using Rh(III) ion-imprinted polymers as sorbent.
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DOI：
10.1016/j.talanta.2012.11.076
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发表时间：
2013-02
期刊：
影响因子：
6.1
通讯作者：
Bing Yang;Tingying Zhang;Wenxian Tan;Peng Liu;Z. Ding;Qiue Cao
中科院分区：
文献类型：
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作者：
Bing Yang;Tingying Zhang;Wenxian Tan;Peng Liu;Z. Ding;Qiue Cao
基于Rh(III)与WO42-−和乙基罗丹明B的反应，初步建立了测定Rh(III)的共振光散射法。该方法灵敏度高，但缺乏选择性。为此，以2-烯丙基硫代烟酸(ANA)为功能单体，采用沉淀聚合法制备了Rh(III)离子印迹聚合物(IIP)，建立了离子印迹固相萃取(IIP-SPE)法分离复杂基质中的Rh(III)，然后进行RLS测定。详细研究了影响IIP-SPE萃取效率和选择性的实验参数。在最佳条件下，浓缩因子(EF)为10的IIP-SPE柱可重复使用20次以上，萃取率不会显著降低(90%以上)。RLS-IIP-SPE联用测定Rh的线性范围为0.06~1.5ngmLRH(−)，检出限为0.024ngmLRH(III)。在10ngmLRH(III)浓度以下，无金属离子干扰测定0.8ngmLH1RH(III)。−-1RH(III)浓度低于10ngmL时，−-1RH(III)的测定无干扰。IIP-SPE-RLS方法成功地用于催化剂、水和化探样品中痕量Rh的萃取和测定，相对标准偏差(RSD)小于4.0%(n=4)。
A resonance light-scattering method (RLS) for the determination of Rh(III) was initially developed, based on the reaction among Rh(III), WO42−and ethylrhodamine B. The method possesses high sensitivity, but lacks selectivity. Therefore, a Rh(III) ion-imprinted polymer (IIP), prepared by precipitation polymerization using 2-(allylthio)nicotinic acid (ANA) as functional monomer, was used as sorbent to construct a ion-imprint based solid-phase extraction (IIP-SPE) method for separation of rhodium from complicated matrices prior to its determination by RLS. The experimental parameters affecting the extraction efficiency and selectivity of IIP-SPE were studied carefully. Under the optimal conditions, the IIP-SPE column with the enrichment factor (EF) of 10 could be used at least 20 times without decreasing its extraction recovery (above 90%) significantly. The calibration graph for the determination of rhodium by RLS coupled with IIP-SPE procedure was linear in the range of 0.06–1.5ngmL−1with the detection limit of 0.024ngmL−1. There is no metal ions tested at the concentration below 10ngmL−1interfered in the determination of 0.8ngmL−1Rh(III). The proposed IIP-SPE–RLS method was successfully applied to the extraction and measurement of trace rhodium in catalyst, water and geochemical samples with the relative standard deviation (RSD) of less than 4.0% (n=4).