2,4-ジヒドロキシベンズアルデヒド-セミカルバゾンによる鉱物中のスカンジウムのけい光定量

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Scandium in several minemls {(O.002〜O.3)% Sc} was determined by the flurometric method. The procedure is as follows : (O.05〜01)g of mineral sample is treated with 30ml of concentrated sulfuric acid for 3 hrs on a sand bath, and the solution is evaporated to dryness. The residue is disslved in (3〜5) ml of concentrated hydrochloric acid, and the solution is diluted to (70〜80) ml with water and filtered. Seventy milligrams of Ca^2^+ as a carrier and oxalic acid solution are added and the pH of the solution is adjusted to 2.0. After the solution has stood for ten minutes, the precipitate is centrifuged and decomposed by evaporating with perchloric acid to dryness. The residue is dissolved in 5ml of 6M HCl. Scandium is separated by extracting at pH 1.6 with 10ml of O.2M TTA-benzene followed by backextracting with 1Oml of 1M HCl.The solution is made up to 25ml, and an aliquot of the solution is taken. Two ml of 0.1% 2,4-dihydroxy-benzaldehyde-gemicarbazone solution, 2ml of 20% ammonium acetate solution are added, and the pH of the solution is adjusted to 6 with hydrochloric acid or ammonia, and the solution was diluted to 25ml with water. The fluorescence intensity of the solution is measured (λexitation 360nm, λemlssion 425nm). In this procedure, the recovery of scandium was found to be about 95%. Several mineral samples (naegite,allanite,yamaguchilite,lepidomelane,hokutolite) were analyzed.
社団法人日本分析化学会の論文
1975-05-10