The separation of nickel has been carried out from a waste solution containing 3.18 g/L Ni with other impurities such as Fe, Zn, Cu and As. Iron was removed by precipitation and Cu and Zn were removed by solvent extraction using LIX 622N and NaTOPS-99, respectively. After removal of all these impurities nickel was extracted by 1.5 M NaTOPS-99 in two counter-current stages at A:O ratio of 3:1 and the loaded organic was stripped with 30 g/L H2SO4 at phase ratio of unity. The strip solution of nickel was treated with Al-2(NO)(3) center dot 9H(2)O for co-precipitation by increasing the pH of solution with 1 M NaOH up to 10. The Ni-Al layered double hydroxide was confirmed through XRD characterization. (C) 2014 Elsevier Ltd. All rights reserved.