电感耦合等离子体原子发射光谱法测定氧化钼中镧和钇

氧化钼掺杂稀土元素改性是近年来的研究热点,目前尚没有针对氧化钼中稀土元素分析的国家标准方法。实验采用硝酸-过氧化氢溶解样品,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定氧化钼样品中镧和钇。实验研究了样品溶液中钼基体和试液介质酸度的影响,结果表明:高浓度的钼对镧和钇的测定产生基体效应,而氧化钼质量浓度小于2 mg/mL时对镧和钇的测定几乎没有影响;介质中硝酸酸度不影响样品中镧、钇的测定。按照实验方法测定含镧量不同的4个样品中镧,测定结果的相对标准偏差(RSD,n=7)为0.95%～3.2%,回收率为97%～98%;按照实验方法测定含钇量不同的4个样品中钇,测定结果的相对标准偏差(RSD,n=7)为4.3%～5.5%,回收率为101%～103%;镧和钇的测定值与参考值相吻合。

Determination of lanthanum and yttrium in molybdenum oxide by inductively coupled plasma atomic emission spectrometry

The modification of molybdenum oxide by doping with rare earth elements is a research hotspot in recent years. At present, there is no national standard method for the analysis and measurement of rare earth elements in molybdenum oxide. The samples were dissolved by nitric acid and hydrogen peroxide in experiments, and the contents of lanthanum and yttrium in molybdenum oxide were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The matrix effect of molybdenum in sample solution and the influence of acidity were studied. The results showed that high-concentration molybdenum had matrix effect on the determination of lanthanum and yttrium. When the mass concentration of molybdenum oxide was less than 2 mg/mL, it had little influence on the determination of lanthanum and yttrium. The acidity of nitric acid in the medium had no influence on the determination of lanthanum and yttrium in the sample. The content of lanthanum in four samples with different lanthanum contents was determined according to the experimental method. The relative standard deviations (RSD, n=7) of determination results were between 0.95% and 3.2%, and the recoveries were between 97% and 98%. The content of yttrium in four samples with different yttrium contents was determined according to the experimental method. The RSDs (n=7) of determination results were between 4.3% and 5.5%, and the recoveries were between 101% and 103%. The determination results of lanthanum and yttrium were consistent with the reference values.