电感耦合等离子体原子发射光谱法测定钕铁硼中钼钨铌锆钛

采用硝酸和硫酸处理样品后, 在5%(体积分数)硫酸介质中, 用电感耦合等离子体原子发射光谱法(ICP-AES)测定了钕铁硼中钼、钨、铌、锆、钛的含量。基体元素铁、钕和硫酸产生的光谱干扰或基体效应采用基体匹配的方法克服, 基体元素硼和其他共存元素对测定均没有干扰。方法的测定下限分别为0.10 μg/mL(钼)、0.20 μg/mL(钨)、0.15 μg/mL(铌)、0.10 μg/mL(锆)、0.10 μg/mL(钛)。方法应用于钕铁硼样品中钼、钨、铌、锆、钛的测定, 测定结果与电感耦合等离子体质谱法的测定结果或参考值相符, 加标回收率在98%～104%之间, 相对标准偏差(RSD, n=11)小于6%。

Determination of molybdenum,tungsten, niobium,zirconium and titanium in NdFeB alloy by inductively coupled plasma atomic emission spectrometry

After the sample was treated with nitric acid and sulphuric acid, the contents of molybdenum, tungsten, niobium, zirconium and titanium in NdFeB alloy were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) in 5% (V/V) sulfuric acid medium. Spectral interferences or matrix effects from the matrix elements including iron and neodymium and sulfuric acid were overcome with matrix matching method while the matrix element boron and other co-existing elements did not interfere with the determination. The lower limit of quantification were 0.10 μg/mL (Mo), 0.20 μg/mL (W), 0.15 μg/mL (Nb), 0.10 μg/mL (Zr) and 0.10 μg/mL (Ti), respectively. The method was applied to the determination of molybdenum, tungsten, niobium, zirconium and titanium in NdFeB alloy samples and the results were consistent with those obtained by inductively coupled plasma mass spectrometry or the reference values. The recoveries were in the range of 98%-104% and the relative standard deviations (RSD, n=11) were less than 6%.