镁铬质耐火材料的ICP-AES法测定

ICP-AES determination of micro amount constituents in magnesia-chrome refractory

采用电感耦合等离子体原子发射光谱法(ICP-AES)同时测定镁铬质耐火材料中Cr2O3、SiO2、Fe2O3、TiO2、CaO、Al2O3等次量及微量成分。通过试验确定了熔样方法、仪器最佳工作参数、ICP分析条件、分析谱线等,同时研究了基体效应。结果表明,样品用四硼酸锂和碳酸锂混合熔剂于1000℃左右熔融,可完全分解试样。引入试液中的大量锂和基体镁对测定有影响,可用基体匹配方法消除;样品中含量较高的铬、铁和铝对含量低的其它元素没有光谱干扰。用该法分析镁铬质耐火材料标样BCS369和BCS370的相对标准偏差RSD均小于1%,测定值与标准值一致。

The micro amount constituents （Cr2O3, SiO2, Fe2 O3, TiO2, CaO, Al2O3 ） in magnesia-chrome refractory were determined by inductively coupled plasma atomic emission spectrometry （ICP-AES）. The sample fusion method, optimum working parameters, ICP analytical conditions, and analysis spectral line were achieved through experiments. The matrix effect was investigated. The sample was completely decomposed at about 1000℃ using mixed Li2B4O7 and Li2CO3 as fusing agent. The effect of Li in reagent and Mg in matrix was overcome by matrix matching. The higher concentrations of Cr, Fe and Al in the sample did not interfere the determination of other lower concentration elements. The standard samples of magnesia-chrome refractory, BCS369 and BCS370, were analyzed with this method. The RSD was 〈1% （n=6） for all six constituents. The measured values agreed with centified values .