Arsenic mitigation behavior in aqueous systems is being evaluated for Mn-Al-Fe, Cu-Al-Fe nano adsorbents. Morphological, and vibrational spectroscopy analysis are observed with As-OH, and As-O surface complexes. XPS study of individual As(3d) spectra at different parameters is observed with multiplet peak behavior attributed to redox behavior of Mn-Al-Fe, Cu-Al-Fe. Significant proportions of As(0) signal (similar to 25 at.% in pH 7, similar to 78 at% in pH 2, 58 at.% in pH 12) implicate an environmentally stable behavior of these adsorbents to address the arsenic leaching issue. Adsorption kinetics are observed with Pseudo Second Order (PSO) model, and Freundlich model supported multilayer adsorption behavior is observed for adsorption isotherms. Trace metal voltammetry studies are observed with 75-90 % of As(III) mitigation in aliquot samples. Detailed study of Mn (2p), Cu(2p), Fe(2p), and O(1 s) spectra explains redox active, and surface ligand exchange synergism in arsenic adsorption. Low equilibrium concentrations (Ce < 10 ppb) in As(V) systems (C-i similar to 100 and 500 ppb) indicate the drinking water application of these systems. Cyclic-voltammetry (CV) studies implicate the mitigation and immobilization of arsenic species onto adsorbent by both reduction, and sorption phenomenon.