The pressurized heavy water reactors use natural uranium oxide (UO2) as fuel and use cladding material made up of zircaloy, an alloy of zirconium. Pickling of zircaloy tubes and appendages viz., spacer and bearing pads is carried out to remove the oxide layer and surface contaminants. Experiments were conducted to optimize the composition of zircaloy pickling solution. The HF-HNO3 ratio in pickling solution and the effect of the optimized solution composition with both fresh and regenerated solution was studied. In this present paper, the authors present their experience about the recycling suitability of the used pickling solution and the rate of pickling reaction with the optimized solution.