【摘要】 以混酸低温加热方式溶解合金，采用电感耦合等离子体质谱法测定复杂高温合金中微量硅。通过实验前准备、动能歧视和完全匹配基体消除二次污染、多原子离子干扰和共存元素干扰。采用5 mL盐酸、0.5 mL硝酸和几滴氢氟酸作溶剂，于80℃加热溶解合金样品，以Sc为内标校正仪器波动产生的影响。以硅的信号强度值为纵坐标，其质量分数为横坐标，绘制标准工作曲线，质量分数在0.002%～0.10%范围内线性良好，相关系数为0.999，检出限为0.000 3%。样品加标平均回收率为90.0%～110.0%，测定结果的相对标准偏差不大于2.0%(n=6)。该方法操作简便，能够满足日常测试要求。更多还原

【Abstract】 The alloy was dissolved by low-temperature heating with mixed acid, and trace silicon in complex superalloys was determined by inductively coupled plasma mass spectrometry(ICP-MS) method. Secondary contamination,polyatomic ion interference and co-existing element interference were eliminated by pre-experiment preparation, kinetic energy discrimination and complete matching of substrates. The alloy was dissolved by heating at 80 ℃ with 5 mL hydrochloric acid, 0.5 mL nitric acid and a few drops of hydrofluoric acid, and the influence of instrument fluctuation was corrected with Sc as internal standard element. The standard working curve was drawn with the signal intensity value of silicon as the ordinate and its mass fraction as the abscissa. The mass fraction had a good linearity in the range of 0.002%-0.10%, the correlation coefficient was 0.999, and the detection limit was 0.000 3%. The recoveries were 90.0%-110.0%,and the relative standard deviations were not more than 2.0%(n=6). This method was simple to use, accurate to analyze, and it can adapt to the requirements of daily testing.更多还原