Abstract: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 ULα line and ZrKα line 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 was 0.999 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.
Bertin E P. Intensity ration technique for X-ray spectrometric analysis of binary samples[J].Anal .Chem.,1964,36(6):826-832.
[2]
WU Wen-qi,XU Tao, HAO Qian, et al. Applications of X-ray fluorescence analysis of rare earths in China[J]. Journal of Rare Earths, 2010,28(suppl.1):30-36.
[3]
宋游,郑维明. 二元比例-X射线荧光光谱法测定模拟MOX燃料中U和Ce含量[J].核化学与放射化学(Journal of Nuclear and Radiochemistry),2005,27(1):7-10.
[4]
PELLA P A, FENG L Y, SMALL J A. An analytical algorithm for calculation of spectral distributions of X-ray tubes for quantitative X-ray fluorescence analysis[J].X-ray Pectrometry,1985,14(3): 125-135.
[5]
阳亚玲,颜文斌,蔡俊,等. 溶液制样-偏振能量色散X射线荧光光谱法分析石煤钒矿中五氧化二钒[J].冶金分析,2014,34(12):13-16. YANG Ya-ling,YAN Wen-bin, CAI Jun, et al. Determination of vanadium pentoxide in stone coal vanadium ore by polarized energy dispersive X-ray fluorescence spectrometry with sample solution preparation[J]. Metallurgical Analysis, 2014,34(12):13-16.
[6]
高新华,殷凤艳. 用XRF二元比例法测定钨铼合金中的钨和铼[J].冶金分析,1994,22(4):22-25. GAO Xin hua, YIN Feng-yan. Determination of W and Re in alloy containing tungsten and rhenium by binary ratio XRF method[J]. Metallurgical Analysis, 1994,22(4):22-25.
[7]
关乃杰,邓玉福,谷珊,等. 二元比例X射线荧光光谱法测定BaFe12O19中Fe和Ba的含量[J].光谱学与光谱分析,2013, 33(10):2858-2860. GUAN Nai-jie, DENG Yu-fu, GU Shan, et al. Determination of Fe and Ba in BaFe12O19 samples by binary ratio and X-ray fluorescence spectrometry[J]. Spectroscopy and Spectral Analysis, 2013,33(10):2858-2860.
[8]
焦继岳,陈和乐. 铌铜合金的X-荧光光谱分析——二元比例外标法[J].分析试验室(Chinese Journal of Analysis Laboratory),1983,2(2):14-18.
[9]
李丹,赖万昌,陈小强,等. 黄铜合金主元素Cu、Zn含量的XRF分析[J]. 核电子学与探测技术,2012,32(2):200-202. LI Dan, LAI Wan-chang, CHEN Xiao-qiang, et al. Determination of main element Cu,Zn in brass alloy by X-ray fluorescence analysis[J]. Nuclear Electronics & Detection Technology, 2012,32(2):200-202.
[10]
宋游,郑维明. 二元比例法分析UO2-CeO2混合粉末[J]. 中国原子能科学研究院年报(Annual Report for China Institute of Atomic Energy),2002:104.