电感耦合等离子体原子发射光谱法测定铬铁中痕量硼

在钢铁冶炼过程中,铬铁合金作为钢的添加料,应用非常广泛。在某些优质钢种中,硼元素指标要求非常严格,因此,准确测定铬铁中痕量硼含量具有重要意义。实验研究了溶样酸对样品溶解的影响,采用盐酸-硝酸-氢氟酸体系溶解样品,同时优化了工作参数(分析功率和雾化气流量),并研究了分析谱线及基体效应对硼测定结果的影响,最终选择B 208.95 nm为分析谱线,使用基体匹配法绘制校准曲线消除基体效应的影响,建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定铬铁中痕量硼的方法。校准曲线的线性相关系数r为0.999 4;硼的检出限为0.000 42%,定量限为0.001 4%。按照实验方法测定铬铁样品中硼,结果的相对标准偏差(RSD,n＝11)不大于10%,回收率为95%~110%。

Determination of trace boron in ferrochrome by inductively coupled plasma atomic emission spectrometry

As an additive to steel, ferrochrome is widely used in the process of steel smelting. In some high-quality grade steels, the index requirements of boron element are very strict. Therefore, it is of great significance to accurately determine trace boron content in ferrochrome. The influence of acid type on the sample dissolution was studied in experiments. The hydrochloric acid-nitric acid-hydrofluoric acid system was selected to dissolve samples. Meanwhile, the working parameters (analytical power and atomizing gas flow) were optimized. The influence of analytical lines and matrix effect on the determination results of boron were also studied. B 208.95 nm was finally selected as the analytical line. The matrix matching method was adopted to prepare calibration curve to eliminate the influence of matrix effect. The method for the determination of trace boron in ferrochrome by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The linear correlation coefficient (r) of calibration curve was 0.999 4. The limit of detection for boron was 0.000 42%, and the limit of quantification was 0.001 4%. The content of boron in ferrochrome sample was determined according to the experimental method. The relative standard deviation (RSD, n=11) of the results not more than 10%. The recoveries were between 95% and 110%.