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An original method was proposed to reduce the quenching of the NIR fluorescence of colloidal solutions of 0.1 at. % Nd 3+ : LaF 3 nanoparticles (NPs) synthesized by aqueous co-precipitation method followed by hydrothermal microwave treatment. For this, an aqueous colloidal solution of NPs was precipitated by centrifugation and dissolved in the same volume of DMSO. The kinetics of static fluorescence quenching of Nd 3+ donors of doped NPs dispersed in two solvents was analyzed to determine and to compare the concentrations of OH- quenching acceptors uniformly distributed throughout the volume of the NPs. The dependences of the relative fluorescence quantum yield φ of colloidal solutions on the concentration of OH- groups in the NPs were calculated and were also used to determine concentration of acceptors in the volume of NPs in different solvents. It was found that the concentration of OH- groups in NPs dispersed in DMSO is almost two times lower than in NPs dispersed in water. This gives an almost two-fold increase in the relative fluorescence quantum yield φ for the former. The sizes of synthesized NPs were monitored by common TEM and by applying a rapid procedure based on optical visualization of the trajectories of the Brownian motion of NPs in solution using a laser ultramicroscope. The use of two different methods made it possible to obtain more detailed information about the studied NPs.