Abstract: 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(s_r) of ≤1% for Nb and ≤2% for Ti, confirming superior method reproducibility. Long-term stability assessments over 30 days revealed s_r 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.