Here, we report the development of a hydrogen-free, topotactic oxygen deintercalation technique using alkali metal aluminum gallium amalgams (A x AlGa, where A = Li, Na, K). These amalgams provide a uniquely tunable system where the choice of alkali metal, its concentration, and the Al:Ga composition alter its reductive properties. We demonstrate the utility of this method in topotactically removing oxygen from bulk and thin film specimens of LnNiO 3 (Ln = La, Nd) to form the infinite layer of nickelate LnNiO 2 (Ln = La, Nd). For example, Na 0.25 AlGa affords bulk LaNiO 2 from LaNiO 3 at 300 °C for 120 h, while the same amalgam at 265 °C for 48 h affords the intermediate La 2 Ni 2 O 5 (LaNiO 2.5 ). Other alterations in time and temperature as well as the choice of alkali metal (A) and its concentration (x) in A x AlGa allow further exploration of the topotactic reduction. Compared to standard techniques based on hydrogen gas or hydrides such as LiH, NaH, and CaH 2 , these amalgams offer an elegant tunability of the reduction potential, enabling control over the rate and degree of oxygen removal without the risk of hydrogen intercalation.