Abstract: | An electrochemical detection of free chlorine using carbon‐metal (C?M) composite powder, with a nickel‐metal nanoparticle combined with a multilayered graphene nanoshell (Ni metal@multilayered graphene) as the main component, synthesized from CH4 via multimode microwave‐assisted catalytic decomposition, was studied. Morphological analysis of the C?M composite powder was performed by TEM–EDX and Raman spectroscopy. The C?M composite powder was packed in a porous microelectrode (PME), and its electrochemical activity with respect to free chlorine was evaluated using a potential sweep method. The C?M composite powder exhibited a sufficient activity against free chlorine. A current based on the reduction of free chlorine was observed in the potential < around+0.3 V vs. Ag/AgCl. A linear relationship was observed between the current and the concentration. |