萃取色层-ICP-MS法测定金属钚中杂质元素

Impurity analysis of plutonium metal by extraction chromatography combined with ICP-MS

采用HNO_3(1+1)和少量HF溶解金属钚,建立了利用TEVA(三烷基甲基胺盐,烷基为C8-C10)分离大量Pu中微量Zr等杂质元素,ICP-M S分析的方法。采用H_2O_2调节Pu的价态,样品在3 mol/L HNO3上柱-3 mol/L HNO_3淋洗Zr等杂质元素,并利用ICP-MS测量了分离后样品中Zr,Mo,Ru等杂质元素的含量。结果表明,Pu的去污系数达到104,Zr等24种杂质元素加标回收率多为90%~115%,相对标准偏差优于15%(n=6),方法的检测限为0.2~150 ng/g(以Pu计)。

Studies on the determination of impurities in plutonium metal are described. The bulk of the matrix Pu was dissolved with HNO3-HF solution and then separated by extraction chromatography using TEVA resin. The collected aqueous fraction containing the impurities was analyzed by ICP-MS. The sample was loaded into TEVA extraction chromatography column with 3 mol/L HNO3 as loading buffer and 3 mol/L HNO3 as elution buffer after adjustion of Pu valence by H2O2. The impurity elements such as Zr,Mo and Ru in the separated samples were determined by ICP-MS. The results show the decontamination factor of Pu is higher than 104. The recoveries of most impurity elements are between90%-115% and the relative standard deviations（RSD） are better than 15%. The detection limits of the elements are less than 150 ng/g Pu.