波长色散X射线荧光光谱法测定进口八氧化三铀中的铀  

Determination of Uranium in Imported Uranium Trioxide by Wavelength Dispersive X-ray Fluorescence Spectrometry

作　　者：柳金良 张鑫[1,2] 刘朝 宋茂生[1,2] 鄢飞燕 朱曙光 王龙[4] 刘悦 杨立远 LIU Jinliang;ZHANG Xin;LIU Chao;SONG Maosheng;YAN Feiyan;ZHU Shuguang;WANG Long;LIU Yue;YANG Liyuan(Research Institute No.230,CNNC,Changsha 410007,China;Hunan Engineering Technology Research Center for Evaluation and Comprehensive Utilization of Associated Radioactive Mineral Resources,Changsha 410007,China;Hubei 303 Warehuose,Wuhan 430000,China;China Nuclear Uranium Co.,Ltd.,Beijing 100013,China;China Nuclear Energy Industry Corporation Co.,Ltd.,Beijing 100032,China)

机构地区：[1]核工业二三〇研究所,湖南长沙410007 [2]湖南省伴生放射性矿产资源评价与综合利用工程技术研究中心,湖南长沙410007 [3]湖北三〇三库,湖北武汉430000 [4]中核铀业有限公司,北京100013 [5]中国原子能工业有限公司,北京100032

出　　处：《湿法冶金》2024年第2期206-213,共8页Hydrometallurgy of China

基　　金：中国核工业地质局项目(2019-17-04)。

摘　　要：为满足天然铀贸易复检对准确性和时效性的要求,对采用波长散射X射线荧光光谱法测定进口八氧化三铀中的铀工作条件进行了优化研究,对消解方式、消解器皿、消解时间和温度、麦拉膜、测定用样品质量等样品前处理条件进行了优化选择,确定了X光管电压电流、分光晶体、波峰和背景角度(2θ)、测定时间等仪器测定条件,并对方法的精密度、准确度、可靠性等进行了评估。结果表明:该法工作曲线的线性相关系数为0.9996,相对标准偏差(RSD)在0.029%~0.056%之间;测定结果与标准物质推荐值之间相对偏差≤0.027%;与滴定法相比,该法绝对偏差在0.003%~0.093%之间,结果准确可靠,工作效率是滴定法的5倍。该法可满足进口八氧化三铀样品快速批量分析的要求。In order to meet the accuracy and timeliness requirements of natural uranium trade reinspection,the working conditions for determining uranium in imported uranium trioxide by wavelength scattering X-ray fluorescence spectroscopy were optimized.Suitable digestion methods,digestion vessels,digestion time and temperature,mylar film,sample quality for determination,and other sample pre-treatment conditions were selected for optimization.The measuring conditions of X-ray tube voltage and current,spectroscopic crystal,wave crest and background angle(2θ),measure the time were determined.The precision,accuracy and reliability of the method were evaluated.The results show that the linear correlation coefficient of the working curve of the method is 0.9996,and the relative standard deviation(RSD)is 0.029%~0.056%.The relative error between the measurement results and the recommended value of the reference material is≤0.027%.Compared with the titration method,the absolute deviation of the method is 0.003%~0.093%,the results are accurate and reliable,and The efficiency is 5 times that of titration.The method can meet the requirements for rapid batch analysis of imported uranium trioxide samples.

关 键 词：波长色散X射线荧光光谱法 八氧化三铀 测定 铀 消解 

分 类 号：O657.34[理学—分析化学] TL271[理学—化学]