Gallium arsenide (GaAs) has both high saturated electron velocity and high electron mobility, making it useful as a semiconductor material in a variety of applications, including light-emitting diodes (LEDs), integrated circuits (ICs), and microwave appliances. A side effect of the use of gallium (Ga) is the production of a relatively large amount of hazardous waste. This study aimed at the recovery of Ga and arsenic (As) from GaAs waste using hydrometallurgical methods involving leaching and coagulation and a dry annealing process that involves annealing, vacuum separation, and sublimation by heating. Our research has shown that GaAs can be leached using nitric acid (HNO3) to obtain 100% Ga and As with a leaching solution at pH 0.1, with subsequent adjustment of the leaching solution to pH 3 with sodium hydroxide (NaOH). Another method used a leaching solution at pH 2, then adjusting to pH 11 using NaOH. Ferric hydroxide (FeO(OH)) was added at 90°C after NaOH was added to the leaching solution. At pH 2 and 11, 55.5 and 21.9% of the As could be removed from the hazardous waste, respectively. The Ga could also be precipitated. When GaAs powder was heated to 1000°C over 3 h, 100% As removal was achieved, and 92.6% of the Ga was removed by formation of 99.9% gallium trioxide (Ga2O3). Arsenic was vaporized when the temperature was elevated to 1000°C, allowing arsenic trioxide (As2O3) to condense with 99.2% purity. The Ga2O3 powder produced was then dissolved and electrolyzed, allowing for 95.9% recovery of Ga with a purity of 99.9%.