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Carbon nanotubes (CNT) were synthesized by floating catalytic chemical vapor deposition method using ferrocene and benzene as hydrocarbon source. The prepared CNTs were oxidized with nitric acid (CNT-OX) followed by coating with nano zerovalent iron (ZVI) to yield nano ZVI decorated CNTs (CNT-Fe(0)). The prepared adsorbents were characterized by various techniques. Using spectral techniques like infra red, Raman and X-ray photoelectron spectroscopy, the mechanism of adsorption between the adsorbent and adsorbate has been postulated. Using CNT-Fe(0) at pH 5, the maximum adsorption capacity of Sb(III) and Sb(V) was found to be 250 mg g−1. The high sorption capacity could be attributed to the high surface area of the prepared CNTs and the reactive nature of the nano zerovalent iron particles on CNTs. A pseudo second order kinetics was followed by CNT-Fe(0) with both Sb(III) and Sb(V …