电感耦合等离子体原子发射光谱法测定铌铁中硅

Determination of silicon in ferro-niobium by inductively coupled plasma atomic emission spectrometry

在常温下用HNO3和HF溶解样品,采用标准加入法消除样品基体的干扰,通过电感耦合等离子体发射光谱仪的专利分析软件选择适当的背景点扣除背景,解决了传统的标准加入法只能用于数量少的样品分析和不能消除背景干扰的缺点。通过编辑分析程序自动绘制工作曲线和计算结果,采用钇内标加入法提高了方法的稳定性,实现了采用电感耦合等离子体原子发射光谱法(ICP-AES)铌铁中硅的测定。考察并选择了电感耦合等离子体光谱仪的RF功率、雾化气流量、辅助气流量等最佳分析参数。对一铌铁试样中硅进行10次测定,测定结果的相对标准偏差为2.4%,标样的测定值与认定值相符。

The sample was dissolved with HNO3 and HF at room temperature.The interference of matrix was eliminated by standard addition method.The background was deducted by selecting proper background points in patented analysis software of inductively coupled plasma atomic emission spectrometer,which solved the shortcomings of conventional standard addition method that it could be only used for the analysis of samples with small amounts and the background interference could not be eliminated.The analytical program was written to automatically plot working curve and calculate results.The stability of method was improved by adding yttrium internal standard,realizing the determination of silicon in ferroniobium by standard addition-inductively coupled plasma atomic emission spectrometry（ICP-AES）.The RF power,atomizing gas flow and auxiliary gas flow of inductively coupled plasma atomic emission spectrometer were investigated and optimized.The silicon in one ferroniobium sample was determined for 10 times,and the relative standard deviation（RSD） was 2.4 %.The determination results of standard sample were consistent with the certified values.