波长色散X射线荧光光谱法测定铀铌钛合金中铌和钛含量OA

Uranium-niobium-titanium alloy has important application value in the nuclear energy field due to its excellent corrosion resistance and mechanical properties.Accurate and efficient determination of niobium(Nb)and titanium(Ti)content in uranium-niobium-titanium(U-Nb-Ti)alloys is critical for ensuring the performance of nuclear materials.Conventional analytical methods,such as gravimetry,spectrophotometry,and inductively coupled plasma atomic emission spectroscopy(ICP-AES),are hindered by complex procedures,prolonged analysis time,and matrix interferences.This study introduces a novel methodology based on wavelength-dispersive X-ray fluorescence spectrometry(WDXRF)for simultaneous quantification of Nb(w=1.0%-7.0%)and Ti(w=0.2%-0.9%)in U-Nb-Ti alloys,addressing the limitations of traditional techniques while enhancing analytical efficiency and reliability.The alloy samples were dissolved in a mixture of nitric acid(HNO3)and hydrofluoric acid(HF)under controlled heating.To prevent hydrolysis of Nb and Ti during solution stabilization,saturated citric acid was added prior to volumetric dilution,ensuring homogeneity and long-term stability of the solution.The resulting solution was immobilized on polyester filter paper to form uniform thin-film specimens,effectively minimizing matrix effects.Calibration standards were prepared using certified reference solutions of U,Nb,and Ti,with critical instrumental parameters—including crystal selection,detector configuration,and operating conditions optimized to establish a robust linear relationship between elemental mass ratios(Nb/U,Ti/U)and their characteristic X-ray intensity ratios(Nb Kα/U Lβ2,Ti Kα/U Lβ2).Calibration curves exhibit excellent linearity,with correlation coefficients(r2)exceeding 0.99.Method validation confirms that the measured values agree well with those obtained by ICP-AES and chemically prepared standards,demonstrating excellent consistency.Precision tests on six parallel samples yield relative standard deviations(sr)of≤1%for Nb and≤2%for Ti,confirming superior method reproducibility.Long-term stability assessments over 30 days revealed sr below 2%,underscoring the effectiveness of citric acid in stabilizing Nb/Ti solutions and maintaining the integrity of thin-film specimens.The integration of citric acid not only suppresses hydrolysis but also enhances measurement consistency,particularly for low-concentration Ti(w=0.2%-0.9%).This WDXRF-based method achieves high instrumental efficiency,with a measurement time of only 50 seconds per sample,eliminating time-consuming separation steps and offering a practical solution for industrial quality control of U-based alloys.The thin-film preparation technique combined with citric acid stabilization effectively mitigates matrix interference and hydrolysis-related challenges.Future research should focus on extending this approach to major element analysis in other alloy systems or complex matrices,leveraging its adaptability to advance nuclear material characterization technologies.