电感耦合等离子体光谱-质谱法联合测定铀化合物粉末中20种杂质元素  

Determination of 20 impurity elements in uranium compound by inductively coupled plasma spectroscopy and mass spectrometry

作　　者：付琳 王玉学 魏代东 霍丹阳 赵路 唐昊 FU Lin;WANG Yuxue;WEI Daidong;HUO Danyang;ZHAO Lu;TANG Hao(Research Institute NO.240,CNNC,Shenyang 110135,China)

机构地区：[1]核工业二四0研究所,沈阳110135

出　　处：《化学分析计量》2022年第8期17-21,共5页Chemical Analysis And Meterage

摘　　要：建立电感耦合等离子体光谱-质谱法联合测定铀化合物粉末中铝、钙、铬等20种杂质元素的方法。用硝酸溶解铀化合物粉末,采用CL-TBP萃淋树脂为吸附树脂,以硝酸溶液分离铝、钙、铬等19种杂质元素后,再以盐酸溶液继续分离钍元素,从而达到一次溶样连续分离的效果,采用等离子体光谱法与质谱法联合测定20种杂质元素,其中光谱法测定铝、钙、铁、镁、钛、钒、钼,质谱法测定铬、钴、镍、铜、锌、铬、钐、铕、钆、镝、铅、铋、钍元素。各杂质元素校正曲线线性相关系数均不小于0.9990。用该法测定八氧化三铀标准物质中的杂质含量,测定结果均在标准值的不确定度范围内,测定值的相对标准偏差为2.50%~5.85%(n=6)。该方法样品用量小(仅需0.2 g),可在一天内完成20种元素的同时测定,满足日常生产检测需要。A method for the determination of 20 impurity elements such as Al,Ca,Cr,etc in uranium compound by inductively coupled plasma spectroscopy and mass spectrometry was established.Uranium powder was dissolved in nitric acid,using CL-TBP extraction resin as absorption resin,19 impurities such as aluminum,calcium,chromium etc were separated by nitric acid solution,and then thorium element was further separated by hydrochloric acid solution,so as to achieve the effect of continuous separation.Twenty impurity elements were determined by plasma spectrometry and mass spectrometry,among which Al,Ca,Fe,Mg,Ti,V,Mo were determined by spectrometric method,Cr,Co,Ni,Cu,Zn,Cr,Sm,Eu,Gd,Dy,Pb,Bi,Th were determined by mass spectrometry.The linear correlation coefficients of correction curves of each impurity element were all not less than 0.9990.Uranium reference materials was determined by this method,and the detection results were consistent with the standard vaule within the detection uncertaity,the relative standard devitions of the detection results were between 2.50%and 5.85%(n=6).The method has a small sample amount(only 0.2 g),and can be used for the simultaneous determination of 20 elements in one day,meeting the needs of daily production.

关 键 词：等离子体光谱法 质谱法 铀化合物 CL-TBP萃淋树脂 

分 类 号：O657.3[理学—分析化学]