Our study aims to decompose phosphogypsum (PG), mainly composed of CaSO 4 .2H 2 O, by reduction in an acidic medium. We evaluated the decomposition of PG by various reaction mechanisms. Sulfate ions from the acid digestion of PG are reduced to sulfide by the hydrogen gas produced in the solution by hydrochloric attack of the metal iron. The solid residues obtained have been determined and monitored by X-Ray Diffraction, Fourier-Transform Infrared spectroscopy and Ultraviolet-visible spectroscopy. The microstructure of residues was observed by scanning electron microscope (SEM). The results show that hydrogen gas formed by hydrochloric acid attack of iron reduces the sulfur from S(VI) to S(-II). CaSO 4 .2H 2 O, insoluble in water, gives a residue containing CaS, which is only sparingly soluble in water. The residue also contains anhydrite, bassanite and ferrous chloride. The monitoring of the quantities of residue obtained under varying experimental conditions (temperature, attack time, mass of iron and PG and volume of acid on PG) and volume of HCl showed that the amounts of residue obtained are less than 32% of mass. When the volume of the HCl added increases, the obtained mass of the solid residue decreases sharply. The residue stabilizes at 10% of mass when the volume of HCl added is higher than that required to attack metal iron.