电感耦合等离子体原子发射光谱法测定高纯氧化镥中14种稀土杂质元素

ICP-AES Determination of 14 Rare Earth Elements as Impurities in High-Purity Lutecium Oxide

采用电感耦合等离子体原子发射光谱法（ICP—AES）测定了高纯氧化镥中14种稀土杂质元素。取氧化镥试样0．5000g溶于盐酸（1＋1）溶液20mL及过氧化氢0．5mL中，所得溶液于100mL容量瓶中定容后供ICP—AES测定。为选择合适的分析线，先根据光谱波长表预选几条强度大，激发电位低的谱线，然后对此谱线进行轮廓扫描，从而选出一条背景平坦，信背比大，基体及共存元素干扰少或无的谱线作为分析线。用基体匹配法配制标准溶液，以5g·L-1氧化镥溶液为基体，用交叉方式配成3个标准溶液系列，所提出方法可满足纯度在99％～99．99％范围的氧化镥的分析。方法的相对标准偏差（n=11）在0．56％～4．2％之间，用标准加入法对方法的回收率做试验，测得回收率在95％～106％之间。

Fourteen rare earth elements as impurities in high purity lutecium oxide were determined by ICP-AES. 0. 500 0 g of Lu203 sample was taken and dissolved in HCI（1＋1） 20 mL with addition of 0. 5 mL of H202. The solution was diluted to 100 mL in a volumetric flask and used for ICP-AES analysis. For choice of analytical spectral lines for each of the 14 RE elements, several spectral lines having higher intensities and lower excitation potentials were chosen preliminarily by referring to the spectra table, and then by sketch scanning of these spectral lines, the spectral lines with flat background, larger SIN values and less interferences from matrix and co-existing elements were finally chosen as the analytical spectral lines. Standards were prepared by additon of 5 g · L -1 Lu2 03 solution for matrix matching, and alternate additon of the RE oxide standards. The proposed method was feasible for analysis of Lu2O3 with their purities in the range of 99%-99. 99%. Precision of the method was tested and values of RSD＇s （n=11） were found in the range of 0.56%-4. 2%. Values of recovery found by standard addition method were in the range of 95%--106%.