The accumulation of phosphorus in activated sludge in wastewater treatment plants (WWTPs) provides potential for phosphorus recovery from sewage. This study delves into the potential for releasing phosphorus from waste activated sludge through two distinct treatment methods—thermal hydrolysis and pH adjustment. The investigation was conducted with activated sludge sourced from four WWTPs, each employing distinct phosphorus removal strategies. The findings underscore the notably superior efficacy of pH adjustment in solubilizing sludge phosphorus compared to the prevailing practice of thermal hydrolysis, widely adopted to enhance sludge digestion. The reversibility of phosphorus release within pH fluctuations spanning 2 to 12 implies that the release of sludge phosphorus can be attributed to the dissolution of phosphate precipitates. Alkaline sludge treatment induced the concurrent liberation of COD, nitrogen, and phosphorus through alkaline hydrolysis of sludge biomass and the dissolution of iron or aluminium phosphates, offering potential gains in resource recovery and energy efficiency.