Quantitative analysis of the film thickness and the mass fraction of urea solution is extremely crucial in relevant industrial processes. The traditional method can measure the film thickness or the mass fraction alone independently. A method to simultaneously measure the thickness and the mass fraction of urea solution is proposed based on the Raman spectroscopy. Through setting the standard curves reflecting the dependence of the relative intensity of characteristic Raman peak (1004 cm-1, belonging to N-C-N symmetric stretching vibration) on the thickness and the mass fraction, mathematical models are established to retrieve the film thickness and the mass fraction of the urea solution. The results reveal that the intensity is linearly related to the thickness (2-10 mm) when the solution concentration is constant, and the average measurement error for the film thickness is 8.36%. The intensity is linearly related to the mass fraction (5%-40%) when the film thickness is constant, and the average measurement error for the mass fraction is 6.24%.