The freezing behavior of freely suspended piggery wastewater, pulp mill effluent and oil sands tailings pond water droplets was investigated in a specially designed vertical wind tunnel. The entire freezing process was recorded by video cameras and observed visually. The droplets were frozen under different ambient air temperature conditions while floating in the cold air stream. The video images revealed that ice nucleation in the freely suspended water droplets started at the edge of the bottom of the droplets and propagated over the entire surface enclosing the drop in an ice shell under all temperature conditions. The speed of the droplet surface freezing was a function of the ambient air temperature and the chemical characteristic of the water. Most droplets decreased in terminal velocity after freezing. Fracture of ice shell with concentrate discharge was observed for the frozen pulp mill effluent and oil sands tailings pond water droplets.