电感耦合等离子体原子发射光谱法测定铁-硅软磁合金中铝铬锰硅

采用硝酸(1+1)和氢氟酸混合酸消解样品,基体匹配法绘制校准曲线,选择Al 396.152nm、Cr 267.716nm、Mn 257.610nm、Si 251.611nm为分析线,使用电感耦合等离子体原子发射光谱法(ICP-AES)对Al、Cr、Mn、Si进行测定,从而建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定Fe-Si软磁合金中Al、Cr、Mn、Si的分析方法。采用Y内标进行校正,可进一步提高测定结果的精密度。各元素校准曲线的线性相关系数均大于0.999;方法中各元素检出限为0.4~7.9μg/g。按照实验方法测定合金样品中Al、Cr、Mn、Si,结果的相对标准偏差(RSD,n=6)为0.86%~2.5%;回收率为95%~106%。按照实验方法测定Fe-Si软磁合金样品中Al、Cr、Mn、Si,并分别采用国标方法 GB/T 223.81-2007、GB/T 223.11—2008、GB/T 223.63—1988和GB/T 223.60—1997的测定结果进行比对,结果基本一致。

Determination of aluminium,chromium,manganese,silicon in iron-silicon magnetically soft alloy by inductively coupled plasma atomic emission spectrometry

The sample was dissolved with the mixed composed of nitric acid (1+1) and hydrofluoric acid, and the calibration curve was plotted with matix matching method. Consequently, a method for the determination of Al, Cr, Mn, Si in Fe-Si magnetically soft alloy by inductively coupled plasma atomic emission spectrometry (ICP-AES) is developed. Al 396.152 nm, Cr 267.716 nm, Mn 257.610 nm, Si 251.611 nm are selected as the analysis spectral lines for Al, Cr, Mn, Si. The results showed that Y as internal element is good for the precision of determination. The detection limits of elements were between 0.4 μg/g and 7.9 μg/g and their linear correlation coefficients were higher than 0.999. Under the selected experimental conditions, the relative standard deviations (RSD,n=6) of determination results were between 0.86% and 2.5%. The recoveries were between 95% and 106%. The comparison test showed that the values determined by ICP-AES were consistent with those by GB/T 223.81-2007, GB/T 223.11-2008, GB/T 223.63-1988 and GB/T 223.60-1997.