微量のゲルマニウム分析における珪酸の影響について

概要

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Quantitative determination of about 10ppm Ge in sulfite ore by acid decomposition method gives very low value. In order to find the cause of this result, Ge4+ in HNO3 or H2SO4 is heated on a water bath or sand bath with the addition of Na2SiO3, SiO2 prepared from Na2SiO3 and -250 mesh quartzite and the Ge is distilled in HCl acidity. In this case, 20γ of Ge added to 0.1g. of the SiO2 was found to be absorbed to the extent of 20γ, 17.5γ and 1.513γ, respectively. The absorption of Ge was greater with an increase of the temperature of digestion or by increasing the amount or finess of the SiO2. The effect of SiO2 was examined on sulfite ore with Ge and the decomposition of the SiO2 with HF gave good result; also, an experimental result of separation of Ge from Fe3+ by use of SiO2 as a carrier is shown. Quantitative determination is made on 50cc sample solution containing 5cc of 0.04%-phenylfluorone and 9cc of HCl. After the solution is allowed to stand from 4hours to over night to develop the color and the intencity of the color is measured by use of S 50 light filter plate. The method followed Beer's Law very well within the limit of 140γ.
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