针对分光光度法测定游离总硅含量受干扰因素多、测试数据不稳定的缺点，探讨了采用ICP-AES法测定碳化硅中游离总硅含量。采用行星球磨仪对碳化硅样品进行研磨，以硝酸钠、硝酸、氢氟酸作溶剂，采用微波消解法处理样品。选择212.412 nm特征谱线并以其强度(I )与对应的硅浓度(c)建立校准曲线，硅的质量浓度在10～100μg/mL范围内与特征谱线强度呈良好的线性关系，线性方程为I=233.76c+86.94，线性相关系数r=0.997，检出限为0.027μg/mL。测定结果的相对标准偏差为1.35%～2.79%(n=6)，加标回收率为97.6%～108.0%。该法测定碳化硅中游离总硅含量是可行的。%For characteristics of more interference factors and the unstable test data in the spectrophotometric determination of the free total silicon content,inductively coupled plasma-atomic emission spectroscopy was used to determine the free total silicon content of silicon carbide. Planetary ball milling apparatus was used to ground the sample of silicon carbide. Sample was prepared by using sodium nitrate,nitric acid,hydrofluoric acid solvent in microwave digestion system. The appropriate elements of the 212.412 nm characteristic line was selected. The linear regression equation was I=233.76c+86.94 with correlation coefficient of 0.997 in the rang of 10-100μg/mL. The relative standard deviation of this method was 1.35%-2.79%(n=6) and the average recovery was 97.6%-108.0%. The method is feasible in the determination of total free silicon content in silicon carbide.
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