二元比例X射线荧光光谱法测定铀锆体系中铀和锆  

Determination of uranium and zirconium in uranium-zirconium system by binary ratio X-ray fluorescence spectrometry

作　　者：赵峰[1] 廖志海[1] 乔洪波[1] 王占明[1] 安身平[1] 王伟[1] 

机构地区：[1]中国核动力研究设计院反应堆燃料及材料重点实验室,四川成都610005

出　　处：《冶金分析》2015年第7期44-47,共4页Metallurgical Analysis

摘　　要：二元比例法可依据两元素谱线的强度比与两元素浓度比的对数关系实现元素的定量分析。实验将二元比例法与X射线荧光光谱法(XRF)相结合,用于定量分析铀锆体系中铀和锆含量,不论吸收-增强效应是否严重,校准曲线都保持线性关系。对仪器的工作参数进行优化,选择铀的Lα线以及锆的Kα线作为分析线。对铀、锆标准溶液系列,先测量各工作点的X射线荧光计数率,然后分别求取浓度比和信号比的对数,再绘制二元比例校准曲线,得校准曲线的相关系数(R2)为0.999 7。对同一铀锆体系样品进行精密度考察,结果的相对标准偏差(RSD)分别为0.035%(铀)和0.048%(锆)。对6批铀锆体系样品采用实验方法进行分析,同时分别采用滴定法对铀含量、直接X射线荧光光谱法对锆含量进行比对分析,结果基本一致;对自配铀、锆二元体系样品溶液进行分析,测定值与参考值的相对误差均小于3.00%。实验方法满足铀锆体系工艺中铀和锆含量的测试要求。The binary ratio method could be used for the quantitative analysis of elements according to the logarithmic relationship between the spectral intensity ratio and concentration ratio of two elements.The binary ratio method was combined with the X-ray fluorescence spectrometry(XRF)for the quantitative analysis of uranium and zirconium content in uranium-zirconium system.The calibration curve showed good linearity whatever the absorption-enhancing effect was serious or not.The working parameters of instrument were optimized.The ULαline and ZrKαline were selected as the analytical lines.For the standard solution series of uranium and zirconium,the X-ray fluorescence counting rate of each working point was firstly measured.Then,the logarithm between the concentration ratio and signal ratio was calculated to prepare the binary ratio-calibration curve.The correlation coefficient(R2)of calibration curve was0.999 7.The precision test was conducted using one uranium-zirconium system sample.The relative standard deviation(RSD)for uranium and zirconium was 0.035% and 0.048%,respectively.The proposed method was applied to the analysis of six batches of uranium-zirconium system samples.Meanwhile,the content of uranium and zirconium was also determined by titration method and direct XRF method,respectively.The found results were consistent.The self-prepared uranium-zirconium binary system sample solution was also analyzed,and the relative error between measured results and reference values was less than 3.00%.The proposed method could meet the determination requirements of uranium and zirconium content in uranium-zirconium system.

关 键 词：X射线荧光光谱 二元比例法 基体效应 铀 锆 铀锆体系 

分 类 号：TL271.7[核科学技术—核燃料循环与材料]