Owing to the extraordinary characteristics Carbon Nanotubes exhibit, these have been employed for wide range of applications. The recognition of chemical contaminants is one such area of research which always involve advancement in concern to the environmental protection and public health. In this regard, Carbon nanotubes decorated with nickel nanoparticles (CNT@Ni) nano-hybrid has been fabricated and characterized with scanning electron microscopy, Transmission electron microscopy, energy dispersive X-Ray analysis, X-Ray Diffraction and Fourier transform infrared spectroscopy. Anion recognition studies were performed for CNT@Ni nano-hybrid, a significant response was observed for Cyanide ion (CN À ) detection and exhibited a detection limit of 7.2 nM. Further, detected CN À was electrochemically reduced to non-toxic OCN À in order to prevent the environment from its toxic effects while disposing off.