Abstract
A few decomposition methods were examined in order to determine impurities in sintered magnesia and spinel samples. Pulverized samples were severely contaminated by a grinding vessel. A lump (about 0.3 g) of sintered magnesia sample was decomposed with a mixture of 0.1 mL of hydrofluoric acid and 9.9 mL of hydrochloric acid in a Teflon pressure vessel at 170°C for 4 h. Similarly, about 0.3 g of a sintered spinel sample was decomposed with 10 mL of sulfuric acid(1+1) at 230°C for 5 d, or with a mixture of 0.2 mL of hydrofluoric acid and 9.8 mL of sulfuric acid(1+1) at 230°C for 24 h. It was necessary to match the matrix components (acids, magnesium and aluminum) in standard solutions to those in sample solutions. The proposed methods were applied to several commercial samples, and the impurities were determined by ICP-OES. The detection limits of most elements (21 elements in magnesia, 20 elements in spinel) were below several μg g−1.
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