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

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

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。

The sample was treated in hydrochloric acid-nitric acid-hydrofluoric acid system by microwave di-gestion method. Al 308. 215 nm and Si 212. 412 nm were selected as the analytical lines. The standard so-lution series were prepared by matrix matching method to plot the calibration curve. The contents of alu-minum 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. 0000% and 2. 50%-12. 50% were linear to their corresponding e-mission intensity, respectively. The linear correlation coefficients were not lower than 0. 999 4. The detec-tion 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）.