电感耦合等离子体原子发射光谱法测定高纯氧化钇铕中13种杂质稀土元素

摘要

Thirteen rare earth elements present as impurities in the high-purity yttrium (+europium) oxide were determined directly by ICP-AES. One (1.000 0)g of the Y(Eu)2O3 sample was dissolved in 10 mL of conc.HCl and diluted quantitatively to 100 mL, which was used for ICP-AFS analysis. Analytical spectral lines of the 13 RE elements were selected and the working parameters of the instrument were optimized and given as follows: ① flow-tare of cooling gas: 12 L · min-1; ② flow-rate of sheathing gas: 0. 20 L · min-1; ③ flow-rate of carrier gas:3.0 L·rain-1; ④ frequency of the RE high-frequency generator: 40.68 MHz, with power of 1.1 kW; and ⑤ height of observation: 10-12 mm. Recovery and precision of the method were tested by standard addition method with 11 determinations, giving values of recovery in the range of 78. 5％-99.6％, and of RSD's ranged from 0.02％ to 0.94％.%采用电感耦合等离子体原子发射光谱法(ICP-AES)测定了高纯氧化钇铕中13种杂质稀土元素.取样品1.000 0 g溶于盐酸10 mL中,加水定容至100 mL,供ICP-AES分析,选定了所测定的13种杂质稀土元素的分析谱线.测定中所选用的仪器工作参数为:①冷却气流量12 L·min-1;②护套气流量0.20 L·min-1;③载气流量3.0 L·min-1;④高频发生器频率40.68 MHZ,功率1.1 kW;⑤观测高度10～12 mm.用标准加入法对方法的回收率及精密度作了试验,所得回收率在78.5%～99.6%之间;测定值的相对标准偏差(n=11)在0.02%～0.94%之间.