Mixed solvent system has been found as an excellent method for the preparation of well dispersed barium sulphate nanoparticles. Spherical and elliptical shaped barium sulphate nanoparticles with barite structure were synthesized through precipitation in water medium and water – chloroform mixed solvent system. Six different compositions of mixed solvents, including pure water, 20 vol.%, 30 vol.%, 50 vol.%, 70 vol.% and 90 vol.% of chloroform were used. Particle characterization was accomplished by X-ray diffraction (XRD), Field Emission Scanning Electron Microscopy (FESEM) with Energy Dispersive X-ray Spectrum (EDX) and Fourier Transform Infrared Spectroscopy (FTIR) techniques. The synthesized particles are having orthorhombic structure with elliptical morphology with an average size of 46.6 nm. It is seen that the water – chloroform mixed solvents protect the nanoparticles against agglomeration.