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Abstract: Use of highly monodispersed, easily recyclable and cheap nickel nanoparticles for oxidative coupling of aliphatic, aromatic, cyclic and heteroaromatic thiols to their corresponding disulfides has been reported. Ni-nanoparticles act as a green catalyst that can selectively catalyse oxidative coupling of thiols to disulfides without producing any over-oxidized products. The catalytic reaction occurred at room temperature with excellent yield under air atmosphere and high TON and TOF value could be achieved. Effect of solvent polarity and size distribution of the Ni-nanoparticles on the catalytic efficiency have been investigated. Nickel nanoparticles could be easily recovered by mild centrifugation. [Copyright &y& Elsevier]