アルセナゾ3による鉄鋼中のスカンジウムの光度定量

概要

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A method for the photometric determination of 0.050.5% scandium in iron and steel with Arsenazo III was studied. In order to remove the interfering elements, the extraction method with 2-thenoyltrifluoroacetone (TTA) was successfully adopted after iron(III) was reduced. The time required for an analysis was about 90 minutes. Two tenths g of sample is decomposed with 10 ml of 6 N hydrochloric acid. One tenth aliquot is taken and the pH of the solution is adjusted to about 1.8 after 10 ml of 1% L-ascorbic acid and 1 ml of 1 N sodium acetate are added. Five ml of the HCl-KCl buffer solution (pH 1.8) is added and the system is shaken with 15 ml of 0.5 M TTA-benzene for about 3 minutes. Scandium in the organic phase is shaken with 6 N hydrochloric acid for 3 minutes and backextracted. The acid layer is shaken with 15 ml of benzene for about 1 minute. After several drops of nitric acid and 3 ml of perchloric acid (60%) are added, the acid layer is heated to white fumes and evaporated to less than 1 ml. Ten ml of water, 10 ml of 1% L-ascorbic acid and 1 ml of 1 N sodium acetate are added. The pH of the solution is adjusted to about 1.8 and then 15 ml of the HCl-KCl buffer solution and 7ml of 0.05% Arsenazo III solution are added. The solution is diluted with water to 50 ml and allowed to stand for 5 minutes. The absorbance of the solution is measured against water at 675 mμ.
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