Nanotechnology has received much attention in treating contaminated waters. In the present study, a facile co-precipitation method was employed to synthesize a novel iron and magnesium based binary metal oxide using a stoichiometrically fixed amount of FeNO3.9H2O and MgNO3.6H2O in a proportion of molar concentration 1:1 and was later evaluated in removing As (III) from contaminated waters. Characterization of the prepared nanomaterial was done using X-ray diffraction (XRD), scanning electron microscopy (SEM), Energy Dispersive X-Ray Analysis (EDAX) and ultraviolet–visible spectrophotometry (UV-VIS). Experimental studies on batch scale were carried out, examining the effect of varying initial concentrations of metal, adsorbent dosage, application time and initial pH on removal efficiency. Arsenic removal increased on increasing adsorbent dosage (0.1–1 g/L) but trend reversed on increasing initial arsenic concentration attaining qmax of 263.20 mg/g. Adsorption was quite efficient in pH range 4–8. Freundlich fitted better for adsorption isotherm along with following Pseudo-2nd order kinetics. The reusability and effect of co-existing ions on arsenic adsorption, namely SO42−, CO32− and PO43− were also explored with reusability in 1st and 2nd cycles attained adsorptive removal up to 77% and 64% respectively. The prepared nano-adsorbent showed promising results in terms of high arsenic uptake (qmax of 263.20 mg/g) along with facile and cost-effective synthesis. Thus, the co-precipitation technique used in this work is a simple one step procedure without any use of any precursor as compared to most of the other procedures used for synthesis.