微波消解-电感耦合等离子体原子发射光谱法测定镍基合金中硅

使用盐酸-硝酸-氢氟酸以及微波消解的方式溶解镍基合金样品,选择Si 251.611 nm或Si 288.158 nm为分析线,Ar 420.069 nm为内标元素谱线,并用两点校正法扣除背景,采用基体匹配法配制标准溶液系列并绘制校准曲线以消除基体效应的影响,建立了使用电感耦合等离子体原子发射光谱法(ICP-AES)测定镍基合金中硅的分析方法。硅质量分数在0.008%～5.00%范围内(Si 251.611 nm),以及硅质量分数在0.015%～5.00%范围内(Si 288.158 nm)分别与其发射强度呈线性,相关系数均大于0.999;方法中硅的检出限不大于0.005%(质量分数)。方法应用于镍基合金样品中硅的测定,结果的相对标准偏差(RSD,n=10 )小于1%。按照实验方法测定镍基合金标准样品中硅,测定结果与认定值相吻合。

Determination of silicon in nickel base alloy by inductively coupled plasma atomic emission spectrometry after microwave digestion

The nickel based alloy sample was dissolved with hydrochloric acid-nitric acid-hydrofluoric acid by microwave digestion. Si 251.611 nm or Si 288.158 nm was selected as analytical line, and Ar 420.069 nm was used as the spectral line of internal standard. The background was deducted by two-point correction method. The standard solution series were prepared by matrix matching method for the plotting of calibration curves to eliminate the influence of matrix effect. The analysis method of silicon in nickel based alloy by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. When the mass fraction of silicon was 0.008%-5.00% (Si 251.611 nm) and 0.015%-5.00% (Si 288.158 nm), it showed linearity to its corresponding emission intensity. The correlation coefficients were high than 0.999. The detection limit of silicon was not higher than 0.005% (mass fraction). The proposed method was applied to the determination of silicon in nickel based alloy, and the relative standard deviations (RSD, n=10) were less than 1%. The content of silicon in certified reference material of nickel based alloy was determined according to the experimental method, and the results were consistent with the certified values.