Shamsipur Mojtaba, Fasihi Javad, Ashtari Khadijeh
Department of Chemistry, Razi University, Kermanshah, Iran.
Anal Chem. 2007 Sep 15;79(18):7116-23. doi: 10.1021/ac070968e. Epub 2007 Aug 21.
A new ion imprinted polymer coated silica gel sorbent has been prepared using the radical "grafting from" polymerization method through surface-bound azo initiators for selective uranyl uptake. The introduction of azo initiator onto the silica surface was achieved by the reaction of surface amino groups with 4,4'-azobis(4-cyanopentanoic acid chloride). The grafting step was then carried out in a stirred solution of initiator-modified silica particles in the presence of uranyl ion and functional and cross-linking monomers. The prepared sorbent was characterized using FT-IR spectroscopy, scanning electron microscopy (SEM), elemental analysis (EA), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), and BET adsorption isotherm analysis. The influence of the uranyl concentration, pH, and flow rate of solution on the grafted polymer affinity has been investigated. Maximum uptake of uranyl ion was observed at a pH 3.0. The rebinding behavior of the sorbent has been successfully described by the Langmuir-Freundlich isotherm. The dynamic column capacity of sorbent and enrichment factor for uranyl ion were 52.9 +/- 3.4 micromol g(-1) and 52, respectively. It was found that imprinting results in increased affinity of the sorbent toward uranyl ion over strong competitor metal ions such as Fe(III) and Th(IV). The sorbent was repeatedly used and regenerated for 3 months without any significant decrease in polymer binding affinities. Finally the sorbent was applied to the preconcentration and determination of uranyl ion in real water samples.
通过表面结合的偶氮引发剂,采用自由基“接枝自”聚合法制备了一种新型离子印迹聚合物包覆硅胶吸附剂,用于选择性摄取铀酰离子。通过表面氨基与4,4'-偶氮双(4-氰基戊酰氯)的反应,将偶氮引发剂引入硅胶表面。然后在引发剂改性的硅胶颗粒的搅拌溶液中,在铀酰离子以及功能单体和交联单体存在的情况下进行接枝步骤。使用傅里叶变换红外光谱(FT-IR)、扫描电子显微镜(SEM)、元素分析(EA)、热重分析(TGA)、差示扫描量热法(DSC)和BET吸附等温线分析对制备的吸附剂进行了表征。研究了铀酰浓度、pH值和溶液流速对接枝聚合物亲和力的影响。在pH 3.0时观察到铀酰离子的最大摄取量。吸附剂的再结合行为已成功地用Langmuir-Freundlich等温线描述。吸附剂对铀酰离子的动态柱容量和富集因子分别为52.9±3.4 μmol g(-1)和52。发现印迹导致吸附剂对铀酰离子的亲和力高于强竞争金属离子如Fe(III)和Th(IV)。吸附剂重复使用和再生3个月,聚合物结合亲和力没有任何显著下降。最后,将该吸附剂应用于实际水样中铀酰离子的预富集和测定。