The change in magnetic characteristics of NiFe2O4 nanoparticles upon the absorption of oleic acid and their desorption by heat treatment was examined in this research. With a heat treatment at 600 °C, the median diameter increased from 5.4 to 16.2 nm. However, the saturation magnetization varied by only 0.3%. On the other hand, with the coating of oleic acid, the saturation magnetization of NiFe2O4 nanoparticles decreased from 31.7 to 30.0 emu/g. After desorption by heat treatment at 600 °C, the saturation magnetization was increased. From these results, it was clear that coating NiFe2O4 nanoparticles with oleic acid decreased the saturation magnetization. This phenomenon may enable us to control the magnetization characteristics of nanoparticles.