(1) Background: In this investigation, a composite of MgO nanoparticles with Itsit biochar (MgO-IBC) has been used to remove arsenate from contaminated water. The reduced adsorption capacity of biochar (IBC), due to loss of functionalities under pyrolysis, is compensated for with the composite MgO-IBC. (2) Methods: Batch scale adsorption experiments were conducted by using MgO-IBC as an adsorbent for the decontamination of arsenate from water. Functional groups, elemental composition, surface morphology, and crystallinity of the adsorbent were investigated by using FTIR, EDX, SEM and XRD techniques. The effect of pH on arsenate adsorption by MgO-IBC was evaluated in the pH range of 2 to 8, whereas the temperature effect was investigated in the range of 303 K to 323 K. (3) Results: Both pH and temperature were found to significantly influence the overall adsorption efficiency of MgO-IBC for arsenate adsorption with lower pH and higher temperature being suitable for higher arsenate adsorption. A kinetics study of arsenate adsorption confirmed an equilibrium time of 240 min and a pseudo-second-order model well-explained the kinetic adsorption data, whereas the Langmuir model best fitted with the equilibrium arsenate adsorption data. The spontaneity and the chemisorptive nature of arsenate adsorption was confirmed by enthalpy, entropy, and activation energy. Comparison of adsorbents in the literature with the current study indicates that MgO-IBC composite has better adsorption capacity for arsenate adsorption than several previously explored adsorbents. (4) Conclusions: The higher adsorption capacity of MgO-IBC confirms its suitability and efficient utilization for the removal of arsenate from water.