铋系超导体组成分析

本文首次提出了一种离子交换柱分离——滴定法测定Bi系超导体中Bi、Pb、Cu、Ca和Sr含量的方法。研究了进样条件和淋洗方法,特别是Bi~(3+)在微酸性溶液中的亚稳态进样。测定合成样品时,Bi、Pb、Cu、Ca和Sr的相对标准偏差分别为0.7％、1.6％、0.5％、0.4％和0.2％。分析了超导体样品,并测定了其中Cu~(3+)。

Determination of Components in Bismuth-system Superconductor

A method for the determination of Bi ,Cu, Ca and Sr in Bi-system superconductor was presented by titrimetry after sample was separated by the ion-exchange. The condition of introduction and elution of samples was studied, especially the introduction of Bi ions was solved at the metastable state in weak nitric acid solution. Bi, Pb, Cu , Ca and Sr were separated completely by fractional elution of 0. 2 mol/L HBr, 0. 6 mol/L HBr ,0. 5 mol/L NH4Ac-HAc,1. 5 mol/L NH4Ac,2 mol/L HNO3. Bi, Pb, Ca and Sr in eluate were titrated by EDTA.and Cu by Na2S2O3 with the relative standard deviation of 0. 7%, 1.6%, 0. 5% , 0. 4% and 0. 2% , respectively, when synthetic samples were determined. The superconductor samples were analyzed and the valency of Cu3+ was also determined.