Unidirectional <001> NiSO4 doped triglycine sulphate (TGS) single crystal of 15 mm in diameter and 150 mm in length was successfully grown in aqueous solution by Sankaranarayanan-Ramasamy (S-R) method. The characterization of the grown crystal was made by powder X-ray diffraction, UV-Vis. spectroscopy, Fourier transform infrared spectroscopy (FTIR), Vicker’s microhardness studies. The X-ray diffraction analysis revealed a monoclinic structure for the grown crystal. UV–Vis. analysis showed high transmittance for the doped TGS crystal in the entire visible region. FTIR spectrum verified the presence of various functional groups in the grown specimen. Vicker's microhardness studies of the doped TGS crystal showed that it is harder than pure TGS crystal. The density of the doped crystal was found to be higher than that of the undoped one