电感耦合等离子体原子发射光谱法测定工业硅中痕量硼

Determination of trace boron in industrial silicon by inductively coupled plasma atomic emission spectrometry

样品经硝酸和氢氟酸混合酸分解后,采用电感耦合等离子体原子发射光谱(ICP-AES)法测定工业硅中痕量硼杂质元素。试验发现,控制加热温度在140～180℃,可以有效抑制硼元素的挥发。对分析谱线的选择进行探讨,选定B208.959nm{161}作为B的分析谱线,而且,适当的扣除背景点,基体和其它共存元素在实验条件下均未对B208.959nm{161}线产生光谱干扰现象。在仪器最佳工作条件下,方法检出限为0.03μg/mL,回收率在90%～105%,相对标准偏差≤7.0%(n=11)。用本方法测定工业硅标准样品中硼,测定值与认定值相吻合。

Trace boron in industrial silicon was determined by inductively coupled plasma atomic emission spectrometry （ICP-AES） after the sample was decomposed with HNO3-HF mixed acid. The results showed that the volatilization of boron could be effectively inhibited by controlling the heating temperature at 140-180 ℃. The analytical spectral lines were investigated, and B 208.9 nm{161}was selected. Moreover, by properly deducting the background under the experimental conditions, the matrix and other coexiting elements had no interference with the spectra of B 208.9 nm{161}. Under the optimal working conditions of instrument, the detection limit of method was 0.03 μg/mL and the recovery was 90 %-105 % with the relative standard deviation （RSD） of no more than 7.0 % （n=11）. The proposed method has been applied to the determination of boron in industrial silicon certified reference materials, and the results were consistent with the certified values.