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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。
The determination of free total silicon content by spectrophotometry interference by many factors, the instability of the test data, the use of ICP-AES method to determine the silicon free silicon content. Silicon carbide samples were ground using a planetary ball mill, and samples were treated with microwave digestion using sodium nitrate, nitric acid and hydrofluoric acid as solvents. The characteristic line of 212.412 nm was selected and the calibration curve was established by its intensity (I) and the corresponding silicon concentration (c). The linearity of the linear equation was linear with the concentration of silicon in the range of 10-100 μg / mL. For I = 233.76c +86.94, the linear correlation coefficient r = 0.997, the detection limit was 0.027μg / mL. The relative standard deviations (RSDs) were 1.35% ~ 2.79% (n = 6), and the recoveries were 97.6% ~ 108.0%. This method is feasible to determine the total free silicon content in silicon carbide.