N-シンナモイル-N-(2,3-キシリル)ヒドロキシルアミンによるバナジウムの抽出-吸光光度定量 : 鋼試料への応用

概要

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An extraction-spectrophotometric method for the determination of vanadium with N-cinnamoyl-N-(2,3-xylyl)hydroxylamine(CXA) was studied. The procedure is as follows: Take an aliquot of a sample solution containing less than 50 μg of vanadium in a separatory funnel and add 40μl of 0.3 % (w/v) potassium permanganate solution. Allow to stand for 5 min and then add 5 ml of 0.1 % (w/v) solution of CXA in carbon tetrachloride. Add hydrochloric acid to aqueous phase to give a final concentration of ca. 6 N. Extract vanadium(V)-CXA complex into carbon tetrachloride by shaking the mixture for 3 min. Dehydrate the organic layer with anhydrous sodium sulfate and filter this solution thro.ugh a small was of cotton into a 1 cm cell and measure the absorbance at 525nm against carbon tetrachloride. Vanadium(V)-CXA complex was cxtracted quantitatively into carbon tetrachloride from (4〜9) N hydrochloric acid. The apparent extinction coefficient of the complex at 525nm was estimated to be 6.1 × 10^3 1 mol^<-1> cm^<-1>. Many coexisting elements do not interfere with the determination of vanadium. And perchloric acid up to 3 M does not interfere. The proposed method was applied to the determination of vanadium in high speed and chrome-vanadium steels.
社団法人日本分析化学会の論文
1980-02-05