Dissolution of molybdenum-silicon (-boron) alloys using a mixture of sulfuric, nitric and hydrofluoric acids and a sequential correction method for ICP-AES analysis

For the major component analysis of Mo-Si (-B) alloys by ICP-AES, an appropriate dissolution method is necessary. The general procedure using a HNO₃-HF mixture cannot be applied for Mo-Si (-B) alloys due to Si volatilization followed by violent reaction and due to MoO₂ precipitation in the preparation of a Mo standard solution from metallic Mo. Good results were obtained with a mixture of 10 mL H₂SO₄, 1 mL HNO₃, 2 mL HF and 12 mL H₂O for Mo-Si (-B) alloys. The samples were completely dissolved at room temperature without any losses. A sequential correction method is also suggested to correct several errors in ICP-AES analysis such as fluctuation in the emission intensities, spectral interferences, non-spectral interferences and blank values.