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The objective of the work was to study inhibition efficiency of 4, 4 ¿¿[(4¿methoxyphenyl)methanediyl]dimorpholine (MPMM) and MPMM assembled on NiONPs for the corrosion of mild steel(MS). With increase in concentration, inhibition efficiency was found to increase but it was better for nanoparticles. As we increase the temperature the inhibition efficiencr was found to increase for nanoparticles but decreases for MPMM. Almost negligible change in inhibition efficiency was found with increase in time for nanoparticles and decreases for MPMM. HOwever, MPMM assembled on NiONPs were found to be superior for the anti-corrosion of mild steel as compared to MPMM.