A new, to the best of our knowledge, internal reference method has been developed for the study of the upconversion luminescence of nanoparticle suspensions. This method provides correct analysis and comparison of the luminescent signals obtained under different conditions. To excite the echo signals of samples, it is proposed to use the radiation from an optical parametric oscillator at two wavelengths for the simultaneous excitation of the upconversion luminescence of particles and the Raman scattering signal of the medium in the Stokes region of the spectrum. Due to the linear dependence of the intensity of the Raman scattering of the medium on the excitation power density, the normalization of the upconversion luminescence signal of particles to the intensity of the Raman scattering of the medium makes it possible to eliminate the influences of the instability of the intensity of the laser radiation, light scattering by the medium, inaccuracies in alignment, etc. on the luminescence signal.