The possibility of using a carbonate-containing industrial waste formed in water-treatment units of thermal power plants for treatment of aqueous solutions to remove nickel(II) ions was analyzed. The influence exerted by the time, temperature, and other factors on the degree of recovery of nickel(II) ions and sorbent expenditure was established. The possibility of separating nickel(II) and iron(III) ions simultaneously present in solution, using the waste under study, was demonstrated.