电感耦合等离子体原子发射光谱法测定高镁中包干式料中硼

高镁中包干式料作为钢铁冶炼过程中必须的一种原材料,其元素含量对于元素追踪起着至关重要的作用。试验对称样量、溶解方法、分析谱线等条件进行讨论,建立了使用电感耦合等离子体原子发射光谱法(ICP-AES)测定高镁中包干式料中硼元素的方法。称取0.4000g高镁中包干式料样品,采用先加氢氧化钾溶液进行碱溶,再加盐酸和硝酸消解的方法处理样品,选择B 182.577nm或B 249.678nm为分析线,在体系没有明显干扰的情况下,选择自动匹配法(FITTED)进行谱线校正扣除背景,采用基体匹配法配制标准溶液系列并绘制校准曲线,实现了电感耦合等离子体原子发射光谱法对高镁中包干式料中硼的测定。硼的质量分数为0.0005%~0.020%(B 182.577nm)或0.0006%~0.020%(B 249.678nm)范围内校准曲线呈线性,相关系数均大于0.9995;方法中硼的检出限为0.0001%。方法应用于高镁中包干式料样品中硼的测定,结果的相对标准偏差(RSD,n=6)小于5%;加标回收率为92%~108%。按照实验方法测定1个成分含量与高镁中包干式料相似的镁砂标样(镁质量分数为48.87%)中硼,结果与标准值相吻合。

Determination of boron in high magnesium tundish dry material by inductively coupled plasma atomic emission spectrometry

High magnesium tundish dry material was a necessary raw material in iron and steel smelting process. The elemental content in high magnesium tundish dry material played an important role in element tracking. The experimental conditions including sample mass, dissolution method and analytical line were investigated, then a determination method of boron in high magnesium tundish dry material by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. 0.4000g of high magnesium tundish dry material sample was dissolved with potassium hydroxide followed by treatment with hydrochloric acid and nitric acid. B 182.577nm or B 249.678nm was chosen as the analytical line. In the absence of obvious interference of system, the automatic matching method (FITTED) was selected for spectral correction and background deduction. The standard solution series were prepared by matrix matching method for the drawing of calibration curve. Consequently, the determination of boron in high magnesium tundish dry material was realized by inductively coupled plasma atomic emission spectrometry. The mass fraction of boron in range of 0.0005%-0.020% (B 182.577nm) or 0.0006%-0.020% (B 249.678nm) had good linearity with correlation coefficients higher than 0.9995. The limit of detection for boron was 0.0001%. The proposed method was applied for the determination of boron in high magnesium tundish dry material samples. The relative standard deviations (RSDs, n=6) of determination results were all less than 5%. The recoveries were between 92% and 108%. The content of boron in one certified reference material of magnesia (magnesium mass fraction of 48.87%) with similar content as high magnesium tundish dry material was determined according to the experimental method. The results were consistent with the standard value.