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In the present work di-sodium hydrogen phosphate single crystals have been grown from aqueous solution by slow cooling technique using a constant temperature bath (+/-0.01 o C). The temperature of the solution was reduced at 0.5 o C/day and 0.15 o C/day from 40 o C to 35 o C. Good quality transparent single crystals have been obtained. The solubility of the material for different temperatures has been studied. The grown crystals were studied by powder and single crystal X-ray diffraction analyses. The FTIR and UV-visible spectra of the grown crystals were recorded. The thermal behaviour of the material was studied by simultaneously recorded thermo gravimetric and differential thermal plots.