A simple and reliable method based upon impregnation of Cyanex302 on octadecyl bonded silica membrane disk has been developed for separation and atomic absorption spectrometric determination of nickel. The influence of various parameters like aqueous phase pH, flow rate and volume of eluent were investigated systematically to optimize the conditions for quantitative sorption and desorption of nickel. The break through volume for nickel was greater than 1.0 dm(3), enrichment factor more than 100 and a detection limit of 2.1 mu g dm(-3) was achieved. The method applied for detection of nickel in tap water and effluent sample had a relative standard deviation (R.S.D.) of 0.4%. (C) 2008 Elsevier B.V. All rights reserved.