<p>This study focuses on the synthesis routes of monoammonium phosphate (MAP), a fertilizer widely used in modern agriculture and known for its high phosphorus and nitrogen content. MAP is produced through the controlled mixing of ammonia and industrial phosphoric acid, culminating in an equimolar ratio in the granulator. This acid–base neutralization reaction can follow two distinct pathways based on the titration mode, which are forward and back titration. The primary objective of this research is to conduct detailed physicochemical studies of the MAP product in order to assess and understand the influence of each synthesis pathway on the physicochemical properties of the granules with a focus on dust emission. Various techniques have been used to characterize the slurry and granulated MAP, such as SEM, NMR, TGA, XRD, dust and hardness measurements, as well as other chemical analyses. XRD, FTIR, and NMR analyses confirmed that both the back titration and the forward titration allowed to synthesis MAP at the molecular level. However, these pathways showed two effects: the first, on the morphology, texture, hardness of the MAP particles and dust generation, and the second, on the crystallization form of the impurities (Al, Fe) NH₄H₂(PO₄)₂·0.5H₂O and (Al, Fe) NH₄HF₂PO₄, which affect the physical behavior of MAP particles.</p>