Nickel hydroxide samples freshly settled as well as stored over I month, 2 months and 6.5 years were examined for their solubility rate in diluted H2SO4 solutions of pH 1.9 and 2.8 as a function of time. Samples with a longer ageing history dissolved less readily than freshly settled ones. It was determined that the resistance to dissolving rose with sample ageing time and the solubility of the 6.5 years stored sample was particularly low. X-ray examination evidenced that during storage the crystallinity of Ni(OH)(2) subsequently rose. The parallelity of both time-dependent phenomena allows the conclusion that with nickel hydroxide ageing the transformation of disordered nickel hydroxide species into crystalline Ni(OH)(2) (without phase changes) is responsible for increasing nickel hydroxide resistance to dissolving in acidic solutions. Such decrease of nickel hydroxide solubility with ageing in case of waste nickel hydroxide, is worth to notice in a view of environment protection against pollution with electroplating waste. (C) 2004 Elsevier B.V. All rights reserved.