The ever-growing contamination of surface water due to various catchment activities poses threats and stress to downstream water treatment entities. Specifically, the presence of ammonia, microbial contaminants, organic matter, and heavy metals has been an issue of paramount concern to water treatment entities since stringent regulatory frameworks require these pollutants to be removed prior to water consumption. Herein, a hybrid approach that integrates struvite crystallization (precipitation) and breakpoint chlorination (stripping) for the removal of ammonia from aqueous solution was evaluated. To fulfil the goals of this study, batch experimental studies were pursued through the adoption of the well-known one-factor-at-a-time (AFAAT) method, specifically the effects of time, concentration/dosage, and mixing speed. The fate of chemical species was underpinned using the state-of-the-art analytical instruments and accredited standard methods. Cryptocrystalline magnesium oxide nanoparticles (MgO-NPs) were used as the magnesium source while the high-test hypochlorite (HTH) was used as the source of chlorine. From the experimental results, the optimum conditions were observed to be, i.e., Stage 1 – struvite synthesis, 110 mg/L of Mg and P dosage (concentration), 150 rpm of mixing speed, 60 min of contact time, and lastly, 120 min of sedimentation while optimum condition for the breakpoint chlorination (Stage 2) were 30 min of mixing and 8:1 Cl2:NH3 weight ratio. Specifically, in Stage 1, i.e., MgO-NPs, the pH increased from 6.7 to ≥9.6, while the turbidity was reduced from 9.1 to ≤1.3 NTU. Mn removal efficacy attained ≥97.70% (reduced from 174 μg/L to 4 μg/L) and Fe attained ≥96.64% (reduced from 11 mg/L to 0.37 mg/L). Elevated pH also led to the deactivation of bacteria. In Stage 2, i.e. breakpoint chlorination, the product water was further polished by eliminating residual ammonia and TPC at 8:1 Cl2–NH3 weight ratio. Interestingly, ammonia was reduced from 6.51 to 2.1 mg/L in Stage 1 (67.74% removal) and then from 2.1 to 0.002 mg/L post breakpoint chlorination (99.96% removal), i.e., stage 2. Overall, synergistic and complementary effects of integrating struvite synthesis and breakpoint chlorination hold great promise for the removal of ammonia from aqueous solutions thus confirming that this technology could potentially be used to curtail the effects of ammonia in the receiving environments and drinking water.