Nanoparticles have gained huge attention in the last decade due to their applications in electronics, medicine, and environmental clean-up. Iron oxide nanoparticles (IONPs) are widely used for the wastewater treatment due to their recyclable nature and easy manipulation by an external magnetic field. Here, in the present research work, iron oxide nanoparticles were synthesized by the sonochemical method by using precursors of ferrous sulfate and ferric chloride at 70 °C for one hour in an ultrasonicator. The synthesized iron oxide nanoparticles were characterized by diffraction light scattering (DLS), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), electron diffraction spectroscopy (EDS), high-resolution transmission electron microscopy (HRTEM) and vibrating sample magnetometer (VSM). The FTIR analysis exhibits characteristic absorption bands of IONPs at 400–800 cm−1, while the Raman spectra showed three characteristic bands at 273, 675, and 1379 cm−1 for the synthesized IONPs. The XRD data revealed three major intensity peaks at two theta, 33°, 35°, and 64° which indicated the presence of maghemite and magnetite phase. The size of the spherical shaped IONPs was varying from 9–70 nm with an average size of 38.9 nm while the size of cuboidal shaped particle size was in microns. The purity of the synthesized IONPs was confirmed by the EDS attached to the FESEM, which clearly show sharp peaks for Fe and O, while the magnetic behavior of the IONPs was confirmed by the VSM measurement and the magnetization was 2.43 emu/g. The batch adsorption study of lead (Pb) and chromium (Cr) from 20% fly ash aqueous solutions was carried out by using 0.6 mg/100 mL IONPs, which exhibited maximum removal efficiency i.e., 97.96% and 82.8% for Pb2+ and Cr ions, respectively. The fly ash are being used in making cements, tiles, bricks, bio fertilizers etc., where the presence of fly ash is undesired property which has to be either removed or will be brought up to the value of acceptable level in the fly ash. Therefore, the synthesized IONPs, can be applied in the elimination of heavy metals and other undesired elements from fly ash with a short period of time. Moreover, the IONPs that have been used as a nanoadsorbent can be recovered from the reaction mixture by applying an external magnetic field that can be recycled and reused. Therefore, this study can be effective in all the fly ash-based industries for elimination of the undesired elements, while recyclability and reusable nature of IONPs will make the whole adsorption or elimination process much economical.