The potential removal and preconcentration of lead (II), copper (II), chromium (III) and iron (III) from wastewaters were investigated and explored. Three new alumina adsorbents of acidic, neutral and basic nature (I-III) were synthesized via physical adsorption and surface loading of 1-nitroso-2-naphthol as a possible chelating ion-exchanger. The modified alumina adsorbents are characterized by strong thermal stability as well as resistance to acidic medium leaching processes. High metal up-take was found providing this order: Cu(II)>Cr(III)>Pb(II) owing to the strong contribution of surface loaded 1-nitroso-2-naphthol. The outlined results from the distribution coefficient and separation factor evaluations (low metal ion concentration levels) were found to denote to a different selectivity order: Pb(II)>Cu(II)>Cr(III) due to the strong contribution of alumina matrix in the metal binding processes. The potential applications of alumina adsorbents for removal and preconcentration of Pb(II), Cu(II), Cr(III) from wastewaters as well as drinking tap water samples were successfully accomplished giving recovery values of (89-100 +/- 1-3%) and (93-99 +/- 3-4%), respectively without any noticeable interference of the wastewater or drinking tap water matrices. (C) 2009 Elsevier B.V. All rights reserved.