2-ニトロソ-5-ジメチルアミノフェノールを用いる抽出吸光光度法による耐熱合金中のコバルトの定量

概要

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A method using 2-nitroso-5-dimethylaminophenol(nitroso-DMAP) was developed for the determination of micro-amounts of cobalt in nickel-based alloy and zirconium alloy which are used as nuclear industry materials. A required amount of sample (ca. 1g) was dissolved in a mixed solution of 2 ml of hydrofluoric acid, 10 ml of nitric acid and 20 ml of(1+1) hydrochloric acid solution. Heat the solution so as to expel excess hydrogen fluoride and nitric acid. Cool and dilute the solution to 100 ml with water. Transfer 5 ml of the sample solution into a 30-ml glass-stoppered test tube, and add 3 ml of buffer solution (citric acid and sodium hydroxide, pH 5.3) and 3 ml of nitroso-DMAP. Mix thoroughly and allow to stand for 30 minutes. Into this tube, transfer 10 ml of 1,2-dichloroethane and shake vigorously for 30 seconds. Back-extract the excess of the reagent and other metal chelates with 10 ml of (1+1) hydrochloric acid solution. Filter the organic phase through a dry filter paper and measure the absorbance at 456 nm. The procedure was checked by two different JAERI Standard Samples with excellent agreement. Percentage recoveries ranged from 96-106 with a mean 101 and a coefficient of variation of 2.7% The proposed method was applied to the determination of cobalt in nickel metals and nickel-based weldings.
社団法人日本分析化学会の論文
1977-05-05