高純度チタンスラック中のMgO,CaOの同時定量法
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概要
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The sample was fused in alkali, and the fusion product was disintegrated in water. The acidity was regulated with dil HCl, and the mixture was boiled with Na<SUB>2</SUB>S<SUB>2</SUB>O<SUB>3</SUB> solution for complete precipitation of Ti and separation from Ca and Mg. Two portions of this solution were measured out. One was used as follows: first impurities such as Mn and Fe were separated out by the use of Br<SUB>2</SUB>-NH<SUB>4</SUB>OH, and then the solution was treated with KCN and 10 cc buffer solution to pH 10, and titrated with 0.01<I>M</I> EDTA standard solution, using EBT as an indicator, to give the sum of Ca and Mg. The other portion of the sample solution, after removal of impurities as above was treated with 15 cc 20% NaOH for decomposition of NH<SUB>4</SUB>Cl, and neutralized with HCl; then 10 cc 20% Na<SUB>2</SUB>S<SUB>2</SUB>O<SUB>3</SUB> and 7<I>N</I> NaOH to pH 13 were added and the Ca was determined by titration with 0.01<I>M</I> EDTA using Dotite NN as an indicator. The amount of Mg was calculated by subtracting the amount required for titration of of Ca from that required for the titration of Ca and Mg.<BR>The standard deviation of error was ± 0.054% for MgO, and ± 0.032% for CaO, and the time required for these procedures was 230 min/sample.
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