电感耦合等离子体原子发射光谱法测定工业硅中8种杂质元素

Determination of eight impurity elements in industrial silicon by inductively coupled plasma atomic emission spectrometry

采用电感耦合等离子体原子发射光谱仪的耐氢氟酸惰性进样系统,在样品用氢氟酸、硝酸、高氯酸溶解完全后无需赶尽氢氟酸和硅基体,直接进样,电感耦合等离子体原子发射光谱法同时测定了工业硅粉中铁、铝、钙、钛、锰、镍、硼和磷8种杂质元素。因为在溶样过程中大部分基体硅已挥发除去,基体效应对铁、铝、钙、钛、锰、镍的测定没有影响,但是对硼和磷的测定仍有影响,这种影响可以采用垂直观测方式克服。按照空白值的3倍标准偏差计算方法的检测限,得到铁、铝、钙、钛、锰、镍、硼和磷的检测限(w/%)分别为0.004,0.001,0.004,0.001,0.000 1,0.000 1,0.000 04和0.000 06。方法已用于工业硅中上述8种杂质元素的测定,测定值与标准方法(GB/T 14849.4—2008)的测定值或认定值相符。

The inert sample injection system resistant hydrofluoric acid of inductively coupled plasma atomic emission spectrometer was used. The sample solution was injected directly without removing hydrofluoric acid and silicon matrix after sample was dissolved in hydrofluoric acid, nitric acid and perchloric acid. Eight impurities including iron, aluminum, calcium, titanium, manganese, nickel, boron and phosphorus in industrial silicon powder were simultaneously determined by inductively cou- pled plasma atomic emission spectrometry （ICP-AES）. Most of matrix silicon had been volatilized and removed in sample dissolution process, so the matrix effect had no influence on the determination of i-ron, aluminum, calcium, titanium, manganese and nickel. However, the determination of boron and phosphorus was still affected, which could be eliminated by vertical observation method. The detec- tion limit of the method was calc＇ulated by three times of standard deviation of blank. The detection limits （w/%） for iron, aluminum, calcium, titanium, manganese, nickel, boron and phosphorus were 0. 004, 0. 001, 0. 004, 0. 001, 0. 0001, 0. 0001, 0. 000 04 and 0. 000 06, posed method was applied to the determination of eight impurities in industrial respectively. The pro silicon. The found resuhs were consistent with the certified values or those obtained by standard method （GB/T 14849.4- 2008）.