2-ヒドロキシ-5-スルホアニリン-N-サリチリデンによる高純度アルミニウム中の微量ガリウムの蛍光定量

概要

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The procedure was as follows : 0.1〜0.2 g of a sample containing less than 20μg of gallium was dissolved by heating in 5 ml of hydrochloric acid (2 + 1). To the solution obtained, were added 0.1 ml of 20 % titanium trichloride solution and 5 ml of hydrochloric acid (2 + 1). The gallium in the solution was extracted twice with 5 ml each of isopropylether by shaking for 1 min. The organic phase was washed 5 times with 2 ml each of hydrochloric acid (2 + 1) by shaking for 15 s. The organic phase was evaporated to dryness on a water bath, and the residue was dissolved in 2 ml of hydrochloric acid (1 + 100) and diluted to 10ml with water. To an aliquot containing O.OO5〜3.0μg of gallium, were added 0.1 % sodium fluoride solution (Ga<0.1μg : 0.05 ml, Ga>0.1μg : 0.1 ml), 2 ml of 0.05% HSS solution in DMF and 0.5ml of2w/v% ammonium acetate solution. The pH of the solution was adjusted to 3.8±0.1 with hydrochloric acid or ammonia water, and the solution was diluted to 25 ml with water. The solution was heated at 50 ℃ for 10 min in a water bath. After cooling to room temperature, the fluorescence intensity was measured at 500 nm (λ excitation : 410 nm) against the standard uranine solution (0.05μg/ml or 0.2μg/ml). The proposed method could be applied to the determination of gallium above 0.05 ppm in practical samples with satisfactory results.
1984-04-05