We report an instantaneous room-temperature phase separation of 1 mM bovine serum albumin solution in the presence of (20% acetic acid+0.2 M NaCl), a routinely used food preservative; an opaque liquid-like phase (L) coexists in equilibrium with a granular gel like phase (G). Interestingly, neither 20% acetic acid nor 0.2 M NaCl individually induces such a phase separation. Field emission scanning electron microscopy (FESEM) and high-resolution transmission electron microscopy (HRTEM) imaging show aggregated proteins to be dispersed in the upper phase, while the lower phase is composed of cross-linked fibrils (hydrogels). Mid-IR FTIR, Raman scattering, and circular dichroism (CD) experiments reveal a significant increase in the β-sheet content in BSA, which confirms the formation of amyloids in the presence of the excipient. Both L and G phases undergo distinct visual and microscopic changes upon …