微波消解-电感耦合等离子体质谱法测定氟化铈中13种稀土杂质

准确称取0.10 g(精确至0.000 1 g)待分析样品于微波消解罐中,加入3 mL盐酸,将微波消解仪由室温升温到120 ℃并保持5 min,再继续升温到180 ℃并保持15 min进行微波消解,以10 ng/mL Cs溶液为内标,建立了电感耦合等离子体质谱法(ICP-MS)测定氟化铈中13种稀土杂质(La、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu)含量的方法。实验表明,13种稀土杂质的线性范围为1.0~100 ng/mL,线性相关系数均不小于0.999 5,方法的检出限为0.002～0.050 μg/g。用所建立方法测定氟化铈粉末样品中La、Pr、Nd、Sm、Gd的结果与电感耦合等离子体原子发射光谱法(ICP-AES)基本一致。将方法应用于氟化铈粉末样品中13种稀土杂质的分析,相对标准偏差(RSD, n=7)均小于5.0%,加标回收率为95%~105%。

Determination of thirteen rare earth impurities in cerium fluoride by microwave digestion-inductively coupled plasma mass spectrometry

0.10 g (accurate to 0.000 1 g) of analytical sample was weighted and transferred into microwave digestion tank. After adding 3 mL of hydrochloric acid, the microwave digestion machine was heated from room temperature to 120 ℃ (kept for 5 min) and then to 180 ℃ (kept for 15 min) for microwave digestion. The determination method of 13 rare earth impurities (La, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu) in cerium fluoride by inductively coupled plasma mass spectrometry (ICP-MS) was established using 10 ng/mL of Cs solution as internal standard. The results showed that the linear range of 13 rare earth impurities was 1.0-100 ng/mL. The linear correlation coefficients were higher than 0.999 5. The detection limit of method was 0.002-0.050 μg/g. The proposed method was applied to the determination of La, Pr, Nd, Sm and Gd in cerium fluoride powder sample, and the found results were consistent with those obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES). The proposed method was also used to analyze the 13 rare earth impurities in cerium fluoride powder sample. The relative standard deviations (RSD, n=7) were all less than 5.0%, and the recoveries of standard addition were between 95% and 105%.