核化学与放射化学
覈化學與放射化學
핵화학여방사화학
HE HUAXUE YU FANGSHE HUAXUE
2014年
6期
352-356
,共5页
龙绍军%廖志海%安身平%王鹏%乔洪波%郭蓉%费浩
龍紹軍%廖誌海%安身平%王鵬%喬洪波%郭蓉%費浩
룡소군%료지해%안신평%왕붕%교홍파%곽용%비호
铀铌混合氧化物%钐%铕%钆%镝%电感耦合等离子体质谱
鈾鈮混閤氧化物%釤%銪%釓%鏑%電感耦閤等離子體質譜
유니혼합양화물%삼%유%구%적%전감우합등리자체질보
U and Nb mixed oxide%Sm%Eu%Gd%Dy%ICP-MS
建立了应用电感耦合等离子体质谱(ICP-MS)测定铀铌混合氧化物中痕量的稀土元素(Sm、Eu、Gd、Dy)的方法。这四种稀土元素在核燃料中的含量在10-7 g/g以下,但热中子截面很大,准确测定其在核燃料中的含量对于核燃料的研究至关重要。样品经 HNO3-HF 快速溶解后,应用 CL-TBP 萃淋树脂分离 U 基体,以115 In作为测定内标校正基体干扰和仪器漂移,标准模式下应用 ICP-MS定量测定淋洗液中 Sm、Eu、Gd和 Dy,半定量分析基体 U。四种稀土元素的质量浓度为0.01~1.00μg/L,线性关系良好,线性相关系数(r)均大于0.999,检出限为0.001~0.002μg/L。对于添加0.2μg/L的稀土元素,稀土元素的回收率为84.3%~97.3%,相对标准偏差(s r )为5.3%~8.7%(n=6),能够满足实际样品测定需要。
建立瞭應用電感耦閤等離子體質譜(ICP-MS)測定鈾鈮混閤氧化物中痕量的稀土元素(Sm、Eu、Gd、Dy)的方法。這四種稀土元素在覈燃料中的含量在10-7 g/g以下,但熱中子截麵很大,準確測定其在覈燃料中的含量對于覈燃料的研究至關重要。樣品經 HNO3-HF 快速溶解後,應用 CL-TBP 萃淋樹脂分離 U 基體,以115 In作為測定內標校正基體榦擾和儀器漂移,標準模式下應用 ICP-MS定量測定淋洗液中 Sm、Eu、Gd和 Dy,半定量分析基體 U。四種稀土元素的質量濃度為0.01~1.00μg/L,線性關繫良好,線性相關繫數(r)均大于0.999,檢齣限為0.001~0.002μg/L。對于添加0.2μg/L的稀土元素,稀土元素的迴收率為84.3%~97.3%,相對標準偏差(s r )為5.3%~8.7%(n=6),能夠滿足實際樣品測定需要。
건립료응용전감우합등리자체질보(ICP-MS)측정유니혼합양화물중흔량적희토원소(Sm、Eu、Gd、Dy)적방법。저사충희토원소재핵연료중적함량재10-7 g/g이하,단열중자절면흔대,준학측정기재핵연료중적함량대우핵연료적연구지관중요。양품경 HNO3-HF 쾌속용해후,응용 CL-TBP 췌림수지분리 U 기체,이115 In작위측정내표교정기체간우화의기표이,표준모식하응용 ICP-MS정량측정림세액중 Sm、Eu、Gd화 Dy,반정량분석기체 U。사충희토원소적질량농도위0.01~1.00μg/L,선성관계량호,선성상관계수(r)균대우0.999,검출한위0.001~0.002μg/L。대우첨가0.2μg/L적희토원소,희토원소적회수솔위84.3%~97.3%,상대표준편차(s r )위5.3%~8.7%(n=6),능구만족실제양품측정수요。
A method was developed for determination of trace rare earth elements (Sm,Eu, Gd and Dy )in U-Nb mixed oxide using inductively coupled plasma mass spectrometry (ICP-MS).Though the contents of these four rare earth elements in nuclear fuel are below 10-7 g/g, the accurate determination of their contents in nuclear fuel is crucially important to the research of nuclear fuel for their thermal neutron-absorption cross-sections are large.After the sample was dissolved fast by HNO3-HF acids,U matrix was separated using CL-TBP extraction resin.115 In was used as internal standard to correct matrix interference and instru-ment drift for quantitative determination of Sm,Eu,Gd and Dy in eluate,semi-quantitative determination of U in eluate by ICP-MS.The method has a good linear correlation (r>0.999)in the range of 0.01-1.00μg/L and the detection limit is between 0.001-0.002μg/L. For the add concentrations of rare earth elements is 0.2 μg/L,the recovery is between 84.3%-97.3% and the relative standard deviation (sr)is between 5.3%-8.7% (n=6).The method can be available in practical application.