电感耦合等离子体原子发射光谱法测定耐火材料中三氧化二硼

以碳酸钠为熔剂, 在约1 000 ℃的温度下熔融样品, 熔融物用盐酸溶解, 选择249.773 nm波长的谱线为分析线, 用电感耦合等离子体原子发射光谱法(ICP-AES)测定了耐火材料中三氧化二硼含量。熔样时引入大量钠盐, 产生的基体效应对测定有影响, 但可以采用基体匹配方法克服。耐火材料中铝、硅、铁、钛、钙、镁等共存元素对硼的测定没有影响。方法的检出限为0.2 μg/mL。用方法分析了自配含硼耐火材料合成样品, 三氧化二硼测定值与参考值基本一致, 相对标准偏差(RSD, n=6)小于5%。

Determination of boron oxide in refractories by inductively coupled plasma atomic emission spectrometry

After the sample was fused at about 1 000 ℃ with sodium carbonate as flux, the molten material was dissolved by hydrochloric acid, then the content of boron trioxide in refractories was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) with the spectral line of 249.773 nm as analysis line. The matrix effect generated by addition of the large amount of sodium salt in the sample fusion process showed an impact on the determination, which could be eliminated by matrix matching method. The coexistent elements in refractories including aluminum, silicon, iron, titanium, calcium and magnesium had no influence on the determination of boron. The detection limit was 0.2 μg/mL. This method was used to determine boron trioxide in the self-made boron-containing refractories synthetic sample. The results were basically consistent with the reference value, and relative standard deviations (RSD, n=6)were less than 5%.