Nickel ferrite nanoparticles prepared by a microwave-assisted autocombustion method with different fuels and microwave powers were used as bare adsorbents for 2-nitrophenol removal from aqueous solutions. Characterization of the as-prepared samples revealed a fundamental variety with respect to their size and surface area. Meanwhile, the crystal phase, functional groups, surface polarity, and magnetic properties remained almost the same. After electing the most efficient adsorbent based on batch experiments, pH influence was established and optimized. Afterward, equilibrium studies were conducted. The kinetic models and adsorption isotherms further facilitated a better understanding of the adsorption mechanism that comprised mainly the multilayered condensation of 2-nitrophenol molecules through the hydrogen bonding.