Ion Exchange Separation of Lead from Strontium in Certified Reference Samples and Spectrophotometric Determination of Lead as Extractable Ion-Pair of Eosin2− and the Lead–Cryptand (2.2.2)2+ Complex

R. Al-Merey, O. Al-Shayah
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引用次数: 1

Abstract

Abstract A two-step procedure including anion exchange separation of lead from strontium in geological reference samples and a spectrophotometric determination of the separated lead as lead–cryptate (2.2.2) complex is presented. The exchangeable anion Cl− of the ion exchange resin (Dowex 1 × 4) is changed to Br− in 6 M HBr solution. Lead is quantitatively retained in the column from 0.5 M HBr medium, while Sr2+, Ba2+, Ca2+, Mg2+, Na+, K+, Fe3+, Cr3+, and Al3+ are passed through. Subsequently the retained Pb is eluted from the column with 6 M HBr. The separation efficiency of the resin is controlled using mixed standard solution of (Pb, Sr, Ca, Mg, Ba, Na, K, Fe, Cr and Al), and radioactive tracers of 85Sr and 131Ba. The resin selectivity coefficient (K) of separating Pb from Sr is found to be . The Spectrophotometric method of lead determination is based on the formation of lead–cryptate (2.2.2) complex at pH 8.3 using borate/HCl as a buffer solution. Then the ion-pair of eosin2+ and lead–cryptand (2.2.2) complex is extracted with chloroform, finally the absorbance of the extractable legend is measured at 550 nm. The extraction recovery, accuracy, precision, linearity and detection limit of the spectrophotometric method are 99.58%, 1.7%, 0.080 µg mL−1, 0–9 µg mL−1, and 0.060 µg mL−1, respectively.
标准样品中铅与锶的离子交换分离及铅作为可萃取离子对的Eosin2 -和铅- cryptand(2.2.2)2+络合物的分光光度测定
摘要介绍了一种两步法,包括阴离子交换分离地质参考样品中的铅和锶,以及分光光度法测定分离后的铅作为隐酸铅(2.2.2)配合物。离子交换树脂(Dowex 1 × 4)的可交换阴离子Cl−在6 M HBr溶液中变为Br−。在0.5 M HBr介质中,铅定量地保留在柱中,而Sr2+、Ba2+、Ca2+、Mg2+、Na+、K+、Fe3+、Cr3+、Al3+则通过。随后,用6m HBr从色谱柱中洗脱残留的Pb。采用(Pb、Sr、Ca、Mg、Ba、Na、K、Fe、Cr、Al)混合标准溶液和85Sr、131Ba放射性示踪剂控制树脂的分离效率。树脂对铅和锶的选择性系数K为。分光光度法测定铅的方法是基于硼酸盐/盐酸作为缓冲溶液,在pH 8.3下形成隐酸铅(2.2.2)络合物。然后用氯仿提取伊红2+离子对和铅-隐式(2.2.2)配合物,最后在550 nm处测定可提取的图符的吸光度。该方法的提取回收率为99.58%,准确度为1.7%,精密度为0.080µg mL−1,线性度为0 ~ 9µg mL−1,检出限为0.060µg mL−1。
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