Abstract：The content of impurity silicon in beryllium-aluminium alloy with high content of beryllium had great influence on its properties such as hot isostatic pressure, precision casting and corrosion resistance. Therefore, the content of silicon should be strictly controlled and it was necessary to determine the content of silicon in beryllium-aluminium alloy with high content of beryllium. The sample was dissolved by sulfuric acid (1+1), nitric acid and hydrofluoric acid in water bath. The residual fluoride ions were masked by boric acid. In the medium of 0.10-0.15mol/L sulfur acid-nitric acid mixture, the ammonium molybdate could react with silicon to form silicon molybdenum yellow heteropolyacid. After stabilizing for 20min, iron ions were masked with oxalic acid. Meanwhile, ascorbic acid was added to reduce silicon molybdenum yellow to silicon molybdenum blue. After placing for 10min, the solution was determined by spectrophotometry at wavelength of 820nm. A determination method of silicon in beryllium-aluminium alloy with high content of beryllium (the mass fraction of beryllium was 60%-70%) was established by spectrophotometry. Under the optimized experimental conditions, the mass of silicon in sample solution in range of 10-60μg had good linear relationship to its corresponding absorbance. The correlation coefficient was 1.000. The detection limit and low limit of determination for silicon was 0.0021% and 0.0071% (mass fraction), respectively. The contents of silicon in two beryllium-aluminium alloy samples (60BeAl and 70BeAl) with high content of beryllium were determined according to the experimental method. The relative standard deviations (RSDs, n=8) of the results were between 2.9% and 3.4%. The results were consistent with those obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES).
白英丽, 王佳丽, 孙洪涛, 张健康. 硅钼蓝分光光度法测定高铍铍铝合金中硅[J]. 冶金分析, 2019, 39(9): 81-85.
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