Superparamagnetic maghemite (gamma-Fe2O3) nanoparticles of controllable morphology were successfully synthesized using a flame spray pyrolysis (FSP) technique. Their physico-chemical properties, size, morphology, and surface chemistries were determined using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), selected area electron diffraction patterns (SAED), SEM-EDX, scanning electron microscopy (SEM), and pHzpc(6.3). Elemental contents before and after adsorption were identified using energy dispersive X-ray fluorescence (ED-XRF), energy dispersive X-ray analysis (EDX) and elemental mapping. Surface area (SBET 79.35 m(2)/g) and size distribution analyses were conducted using a surface area analyzer and dynamic light scattering (DLS), respectively. The magnetic moment (44.5 at 300 I(and 50.16 at 2K) was determined using a physical properties measurement system (PPMS). The first adsorption study using gamma-Fe2O3 nanoparticles synthesized by FSP to successfully remediate Pb2+ and Cu2+ from water is reported. Batch adsorption studies were carried out. An optimum pH of 5.0 was studied for Pb2+ and Cu2+ removal. Pb2+ and Cu2+. removal mechanisms by these maghemite nanoparticles were presented. The adsorption of Pb2+ and Cu2+ was highly pH-dependent. The metal ion uptake was mainly governed by electrostatic attractions. Sorption kinetic data followed the pseudo-second-order model. The Freundlich, Langmuir, Redlich-Peterson, Radice and Sips adsorption isotherm models were applied to interpret equilibrium data. The Freundlich and Langmuir isotherm equations best fit the respective equilibrium data for Pb2+ and Cu2+. The maximum Langmuir adsorption capacities of these maghemite nanoparticles were 68.9 mg/g at 45 degrees C for Pb2+ and 34.0 mg/g at 25 degrees C for Cu2+. Thus, these maghemite nanoparticles made by FSP were readily prepared, characterized and showed promise for remediating heavy metal ions from aqueous solutions. (C) 2016 Elsevier Inc. All rights reserved.