In this study, iron oxide (IO) nanoparticles from various precursors have been synthesized using sonochemical method and characterized for their structural variability and toxicity. e iron oxide (IO) precursor solutions were prepared from iron acetate (IA), iron pentacarbonyl (IP), decalin, PEG (poly(ethylene glycol)), EG (ethylene glycol), PVA (poly(vinyl alcohol)), -cyclodextrin (CD), and distilled water. ese precursor solutions were irradiated with high power ultrasound for 3 hours and heat treated as needed. ese as-prepared iron oxide nanoparticles were characterized using X-ray diffraction (XRD), Mössbauer spectroscopy, transmission electron microscopy (TEM), and magnetization measurements. XRD results show that all the particles are highly crystalline in nature and the particles sizes measured from TEM are approximately 5-20 nm. e maximum magnetization was observed for IO-IP at approximately 60.17 emu/g and the minimum was approximately 30.56 emu/g for IO-IA. ese results con�rm that the particles are superparamagnetic (SPM) in nature. Mössbauer spectroscopy veri�ed the magnetic nanoparticles are purely Fe 3 O 4 and particles sizes varied by the nature of the precursor and coatings.