ベリリウムの分析化学的研究-12・13-

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The basic principle is composed of precipitating beryllium salt solution with NH4OH as Be(OH)2, dissolving with HNO3, heating for 30 minutes at 280-300°C with Bé 60° H2SO4 (about 80%) and estimating it as BeSO4 with 0.17-0.25% error. For quantitative estimation of Be in the presence of Fe (III), Al, Ca and Mg, the author removed larger parts of Fe and Al by Rothe's ether method, the remainder of Fe is separated by precipitating it as FeS with H2S in the presence of tartaric acid, the Al is separated as Al (C9H6ON)3 by oxin method, then the Be in the filtrate is estimated as BeSO4; the error in this case was ±0.2%. This method could used as one of the method of obtaining BeSO4 from the last extract after treating raw mineral materials with general method of treatment. Havens called attention to the fact that an application of a mixture of hydrochloric acid saturated with hydrogen chloride gas and ether on chlorides of berylium and aluminium gives an insoluble AlCl3.6 H2O, while BeCl2. 4H2O remains in the solution, Accoding to the author's investigation, this statement is not absolutely sure. Therefore, a combined use of tannin or oxin method with the above method is investigated and a method of combined use of oxin is taken in this experiment. A good result is obtained by treating the sample solution containing Be, Al, Fe3+, Ca and Mg with NH4Cl and NH4OH to precipitate Be, Al and Fe as hydroxides, filtered, the precipitate is taken up with HCl, the solution is treated with HCl-ether mixture for separation of AlCl3. 6H2O, the filtrate is treated with tartaric acid, H2S and (NH4)2S to separate FeS, the filtrate containing a small amount of Al is removed by precipitating it with oxin, the filtrate is treated with NH4OH to precipitate Be(OH)2 and it is estimated as BeO by usual method.
社団法人日本分析化学会の論文

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秋山知行
京都薬科大学分析化学教室

ベリリウムの分析化学的研究-12・13-

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