电感耦合等离子体原子发射光谱法测定铀-钼合金中15种微量杂质元素

ICP-AES Determination of Micro-Amounts of 15 Elements Present as Impurities in Uranium-Molybdenum alloy

应用电感耦合等离子体原子发射光谱法（ICP-AES）测定了铀-钼合金中15种微量杂质元素。为消除作为基体存在的放射性铀的严重干扰,将试样（0.250 0 g）经硝酸加盐酸溶解后所得溶液（在2 mL体积中）通过用以聚氟乙烯为担体的磷酸三丁酯填充并预先经5 mol·L^-1硝酸平衡的色谱柱（高100 mm,内径6 mm）,即进行反相分配色谱柱上萃取分离,使铀离子留在柱上,而钼（Ⅵ）及15种元素的离子则在淋洗中洗脱而存在于淋洗液中。用所收集的淋洗液进行ICP-AES测定。对测定的分析条件及仪器的工作参数作了试验和优化,还进行了回收率及精密度试验,根据结果算得回收率及相对标准偏差（n=6）依次在93.8%～107.2%及2.9%～6.6%之间。

ICP-AES was applied to the determination of micro-amounts of 15 elements present as impurities in ranium-molybdenum alloy. To eliminate the interference of the radioactive matrix uranium ion, 0. 25 g of the sample after dissolution in HNO3-HCl mixture （in a volume of 2 mL） was passed through a column （100 mm in height and with i. ＆ 6 mm） which was filled with tributylphosphate supported on polyfluoroethylene and previously equilibriumed with 5 mol· L^-1 HNO3. By the reverse-phase partition chromatographic separation, uramium ion was retained on the column, while Mo（Ⅵ） and ions of the 15 elements as impurities were present in the eluate during elution. The eluate collected was used for ICP-AES determination. Analytical conditions and working parameters were studied and optimized. Recovery and precision of the method were tested and the values of recovery and RSD＇s （n=6） obtained were in the ranges of 93. 8%-107. 2% and 2. 9%-6.6% respectively.