高純度テルル中のアンチモンの定量

概要

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A method for the determination of antimony in high purity tellurium has been investigated. Antimony is separated as bromide by distillation from sulfuric acid solution of the specimen, and is extracted from the distillate by a chloroform solution of diethylammonium diethyldithiocarbamate. The organic layer containing antimony is treated with HNO3, HClO4 and H2SO4 to destroy organic matters and to oxidize antimony. Then, antimony is extracted by isopropyl ether from a solution which is 14N in H2SO4 and 6N in HCl. The extraction from such a strong sulfuric acid solution is more effective than that from a solution containing hydrochloric acid only. As the separation of the organic and the aqueous layers is wrong, an addition of small amount of water is necessary to separate two layers after the extraction by shaking. By adding Rhodamine B to the organic layer, antimony is determined spectrophotometrically. A micro-amount of antimony as low as 0.5 ppm in tellurium can be estimated by the proposed method.
社団法人日本分析化学会の論文