高纯氮化硅粉体样品用氢氟酸、硝酸进行微波消解处理,采用电感耦合等离子体质谱法测定所得样品溶液中18种痕量元素的含量。选用合适的同位素和干扰校正方程消除了被测元素的干扰。方法的检出限(3s)在5.2~20.8 pg·g-1之间。方法用于高纯氮化硅粉体样品中痕量元素的测定,加标回收率在89.2%~105.2%之间,相对标准偏差(n=6)小于10%。

The sample of high-purity silicon nitride powder was treated with HF and HNO3 by microwave assisted digestion, and the contents of 18 trace elements in the sample solution were determined by ICP-MS. The interferences were eliminated by using suitable isotopes and applying correction formula. The values of detection limits (3s) of the found were in the range of 5.2-20.8 pg·g-1. The proposed method was applied to the analysis of sample trace elements of high-purity silicon nitride powder, giving values of recovery by standard addition method in the range of 89.20%-105.2%, and RSD′s (n=6) less than 10%.