微波消解试样-萃取色谱分离-电感耦合等离子体原子发射光谱法测定涂铌二氧化铀微球中10种痕量元素  

ICP-AES Determination of Trace Elements in Microsphere UO_2 Coated Ni with Microwave Assisted Sample Digestion and Extraction Chromatographic Separation

作　　者：费浩[1] 廖志海[1] 乔洪波[1] 

机构地区：[1]中国核动力研究设计院核燃料及材料国家重点实验室,成都610005

出　　处：《理化检验（化学分册）》2012年第10期1222-1224,1237,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：涂铌二氧化铀微球试样经硝酸-氢氟酸(3+2)混合溶液消解,所得消解液通过CL-TBP萃取柱使其中的铀与钴、铬、铁、镁、锰、钼、镍、钛、钒和铜等10种元素分离,用5.5mol.L-1硝酸溶液进行淋洗。用电感耦合等离子体原子发射光谱法测定淋洗液中各元素的含量。10种元素分别在一定的质量浓度范围内呈线性,检出限(3s)在0.01～0.08mg.L-1之间。以涂铌二氧化铀微球为基体加入两种不同浓度的标准溶液按试验方法分析后,求得方法的回收率在85.0%～106%之间,测定值的相对标准偏差(n=6)在0.9%～4.8%之间。Sample of microspheres of UO2 coated Ni was digested with a mixture of HNO3-HF （3＋2）, and the solution obtained was passed through CLTBP extraction column for separation of the 10 elements, i. e. , Co, Fe, Cr, Mg, Mn, Mo, Ni, Ti, Cu and V from U. 5.5 mol · ^-1 HNO3 was used as mobile phase in elution. The eluate was used for ICP-AES determination of the 10 elements. Values of detection limit （3s） found were in the range of 0. 01 - 0. 08 mg·L^-1. Tests for recovery and precision were made by standard addition method at 2 different concentration levels, giving values of recovery and RSD＇s （n=6） in the ranges of 85. 0%- 106% and 0. 90%-4. 8% respectively.

关 键 词：电感耦合等离子体原子发射光谱法 微波消解试样 涂铌二氧化铀微球 痕量元素 

分 类 号：O657.31[理学—分析化学]