GdPO4:Eu3+ nanoparticles were prepared by precipitation method under different conditions with different pH, EDTA-2 Na and different annealing temperatures. The structure, morphology and luminescence characterization of GdPO4:Eu3+ nanoparticles were studied by XRD,SEM and luminescence spectrum. The results of XRD and SEM indicated that all of samples consisted of pure phase GdPO4:Eu3+, the size, and growth of crystal interface were related to synthesis conditions. The results of emission spectra and excitation spectra showed that the relative intensities of emission peaks increased with increasing of pH and annealing temperature, and the emission and excitation intensities of sample prepared with EDTA was lowered due to residual organic groups on the surface. The doping concentration of nanoparticles is about 8x%.