1-ニトロソ-2-ナフトール抽出光度法による耐熱合金及びウラン中のコバルトの定量

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An extraction-photometric method for the determination of cobalt in zirconium and its alloys with 1-nitroso-2-naphthol{T,Sawada and S.Kato, Sumitomo Light Metal Technical Reports, 5,302 (1964)} was applied to the analysis of nickel- and iron-base alloys which could be used in a high temperature gas cooled reactor. Tne amount of 1-nitroso-2-naphthol added must be increased six times as much as the amount used in the original work because nickel and iron consume the reagent. An oxidized product of the reagent which was sometimes obtained during the extraction, could be removed by shaking the extract with an alkaline solution contaning hydroxylamine. The following method (ε=3.5x10^4) was used for the detemination of more than O.O1% of cobalt in standard samples of high-temperature alloy which are being produced at Japan Atomic Energy Research Institute and for the determination of traces of cobalt in uranium. The method is also usedful for analyzing aluminum, molybdenum, tungsten, niobium and titanium. A nickel-and iron-base alloy(<O.5g) is dissolved in an acid mxture (HCl : HN0_3 : H_20=1:1:1). Metal and oxides of uranium (<3g) are dissolved in nitric acid. To a solution (Co<40μg), are added 25ml of 2M ctric acid and 15ml of 2x10^2 M 1-nitroso-2-naphthol, and the pH of the solution is adjusted to 3 to 4 with 10 M sodium hydroxide. After addition of 10ml of conc. hydrochloric acid, the cobalt complex is extracted in exactly 20 ml of benzene by shaking vigorously for 1 min. The organic phase is successively washed with 20ml each of conc. hydrochloric acid, water, 1 M sodium hydroxide and sodium hydroxide (1 M)-hydroxylamine hydrochloride (O.5%) by shaking to remove other metals and the excess 1-nitroso-2-naphthol. The absorbance of the organic phase is measured at 40 nm.
社団法人日本分析化学会の論文
1975-07-10

1-ニトロソ-2-ナフトール抽出光度法による耐熱合金及びウラン中のコバルトの定量

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