The spray freezing process, a natural freezing technology, was used to treat pulp mill effluent and oil sands tailings pond water. The wastewaters froze partially or completely (i.e. with or without runoff generation) during the spraying operation. Greater than 60% impurity reduction in the spray ice was obtained when 30% of the total volume of the sprayed water was released as runoff. Organic and inorganic contaminants were rejected with different efficiencies. The impurities were uniformly distributed within the ice columns when the spray ice was produced without generating any runoff. While a significant increase in impurity concentration was observed at the bottom of the ice formed with runoff production. The spray freezing process is an effective and economically feasible technique for wastewater treatment in cold regions. To achieve higher impurity removal efficiency, the wastewater should be only partially frozen during spray ice production.