微波消解-电感耦合等离子体原子发射光谱法测定铁硅铝磁芯中铝和硅

使用盐酸-硝酸-氢氟酸并采用微波消解法处理样品,选择Al 308.215nm和Si212.412nm作为分析线,基体匹配法配制标准溶液系列绘制校准曲线,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定铝和硅,从而建立了微波消解-电感耦合等离子体原子发射光谱法(ICP-AES)测定铁硅铝磁芯中铝和硅的方法。结果表明,铝和硅的质量分数分别为1.00%~9.00%和2.50%~12.50%时与其发射强度呈线性,线性相关系数均不小于0.999 4;方法中铝和硅的检出限分别为0.020%和0.021%(质量分数)。实验方法应用于铁硅铝磁芯样品中铝和硅的测定,结果的相对标准偏差(RSD,n=6)为1.4%~2.2%;将测定结果与滴定法(测定铝)和重量法(测定硅)的测定结果进行比对,二者相吻合。

Determination of aluminium and silicon in iron-silicon-aluminium magnetic core by inductively coupled plasma atomic emission spectrometry with microwave digestion

The sample was treated in hydrochloric acid-nitric acid-hydrofluoric acid system by microwave digestion method. Al 308.215 nm and Si 212.412 nm were selected as the analytical lines. The standard solution series were prepared by matrix matching method to plot the calibration curve. The contents of aluminum and silicon were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). Consequently, a determination method of aluminum and silicon in iron-silicon-aluminum magnetic core was established by ICP-AES with microwave digestion. The results showed that the mass fraction of aluminum and silicon in range of 1.00%-9.00% and 2.50%-12.50% were linear to their corresponding emission intensity, respectively. The linear correlation coefficients were not lower than 0.999 4. The detection limit of aluminum and silicon was 0.020% and 0.021% (mass fraction), respectively. The proposed method was applied to the determination of aluminum and silicon in iron-silicon-aluminum magnetic core samples. The relative standard deviations (RSD, n=6) were between 1.4% and 2.2%. The results were consistent with those obtained by titrametry (for aluminum) and gravimetry (for silicon).