高纯稀土镱配合物中痕量氧化钙及氧化铁的测定

Determination of Trace Calcium Oxide and Iron Oxide in High Purity Ytterbium Complexes

采用标准加入法测定高纯稀土镱配合物中痕量的氧化钙和氧化铁,有效避免基体干扰。当钙元素分析谱线为393.366 nm和396.847 nm,铁元素分析谱线为259.940 nm和261.187 nm,硝酸酸度控制在5%,基体浓度为6 g/L时,高纯稀土镱配合物中痕量氧化钙和氧化铁的含量能准确测量。铝、镁、钠、硅、钾、锌、镍、铜、磷等元素对测定基本无干扰。该方法具有较好的精密度和准确度,CaO的相对标准偏差为4.29%,加标回收率在91.0%~105.5%之间;Fe_2O_3的相对标准偏差为5.88%,加标回收率在96.0%~104.0%之间。

Trace calcium oxide and iron oxide in high purity ytterbium complex were determined by standard addition method,effectively avoiding matrix interference. The optimum determination conditions were as follows： Ca 393. 366 nm,Ca 396. 847 nm,Fe 259. 940 nm and Fe 261. 187 nm,were used as the analytical lines,the acidity of nitric acid was 5%,and the concentration of matrix was 6 g/L. Al,Mg,Na,Si,K,Zn,Ni,Cu and P had no influence on determination. The method had well accuracy and recovery rate. The recovery of CaO was between 91. 0% ~105. 5%,and the relative standard deviation was 4. 29%. The recovery of Fe2O3 was between 96. 0% ~ 104. 0%,and the relative standard deviation was 4. 29%.