This work describes the quantitative analysis of (NH 4 ) 2 CO 3 and NH 4 HCO 3 using a simple solution phase titration method. Back titration results at various (NH 4 ) 2 CO 3 -NH 4 HCO 3 ratios demonstrated that 6:4 ratio caused a 3% error in their differentiation, but very high errors were found at other ratios. A similar trend was observed for the double indicator method, especially when strong acid HCl was used as a titrant, where still less errors (2.5%) at a middle ratio of (NH 4 ) 2 CO 3 -NH 4 HCO 3 was found. Remaining ratios with low (NH 4 ) 2 CO 3 (2:8, 4:6) show high +ve error (found concentration is less) and high (NH 4 ) 2 CO 3 (7:3, 8:2, and 9:1) show high -ve error (found concentration is higher) and vice versa for NH 4 HCO 3 . In replacement titration using Na 2 SO 4 , at both higher end ratios of (NH 4 ) 2 CO 3 -NH 4 HCO 3 (2:8 and 9:1), both -ve and +ve errors were minimized to 75% by partial equilibrium arrest between (NH 4 ) 2 CO 3 and NH 2 COONH 4 , instead of more than 100% observed in back titration and only double indicator methods. In the presence of (NH 4 ) 2 SO 4 both -ve and +ve error% are completely reduced to 3+/-1 at ratios 2:8, 4:6, and 6:4 of (NH 4 ) 2 CO 3 -NH 4 HCO 3 , which demonstrates that the equilibrium transformation between NH 2 COONH 4 and (NH 4 ) 2 CO 3 is completely controlled. The titration conducted at lower temperature (5 o C) in the presence of (NH 4 ) 2 SO 4 at higher ratios of (NH 4 ) 2 CO 3 -NH 4 HCO 3 (7:3, 8:2,and 9:1) shows complete minimization of both -ve and +ve errors to 2+/-1%, which explains the complete arresting of equilibrium transformation. Finally, the developed method shows 2+/-1% error in differentiation of CO 3 2 - and HCO 3 - in the regeneration process of NaHCO 3 from crude desulfurized sample. The developed method is more promising to differentiate CO 3 2 - and HCO 3 - in industrial applications.