ベリリウムの分析化学的研究-15-

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The beryllium in beryllium salt solution is precipitated as BeNH4PO4·41/2H2O, this is dissolved in nitric acid, the phosphoric acid thus liberated is precipitated as ammonium phosphomolybdate, the precipitate is dissolved in a standard alkali solution and the excess alkali is titrated back with a standard sulfuric acid solution, and the amount of beryllium equivalent to the consumed alkali is calculated. Also, the sample precipitated as BeNH4PO4·41/2H2O is taken up in hydrochloric acid, it is converted into oxine phosphomolybdate, it is dissolved in acid and the liberated oxine is estimated by bromatometry for indirect quantitative estimation of beryllium. The sample solution containing Ti, Al, Fe+++ and Mn is treated with ammonium nitrate solution and methanol, and the hydroxides of Al, Fe+++, Be and Ti are separated while hot, the precipitate is taken up in hydrochloric acid, adjusted to pH 4.2, boiled with potassium sulfate and potassium bromate for separation and deposition of titanium oxidehydrate, the iron in the filtrate is separated as sulfide, the filtrate from iron precipitate is utilized for estimation of aluminium by oxine method, then the filtrate is used for estimation of beryllium by usual method. There was some error in this method, but it was better than Moser's method (Monat. 43, 663, 1922). In case of using sodium sulfide method, the sample solution containing Fe, Al, Mn, Ca and Mg is heated with sodium carbonate, caustic soda and sodium sulfide, the precipitates of FeS, MnS, CaCO3 and MgCO3 are filtered off, the filtrate containing beryllate and aluminate are hydrolyzed with NH4Cl for deposition of Be(OH)2 and Al(OH)3, these are taken up in hydrochloric acid, combined with the filtrate, the iron is removed by Rothe's method, the aluminum is separated by oxine method, then the beryllium is determined by usual method. However, this is not very promissing method.
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ベリリウムの分析化学的研究-15-

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