The generation of ammonium hydrogen sulfate from ammonium sulfate is of current interest because of its potential as a process component of bio-based organic acid production from biomass. An organic acid, for example succinic acid, is a chemical product that is used in food, cosmetics, deicing applications, etc. and a potential key carbon building block for numerous other materials. Its production from biomass (corn, etc.) makes it a renewable chemical resource, and the regeneration process described here minimizes the use of additional acid and base value reagents and byproduct (low value salt) waste. In the present work ammonium hydrogen sulfate (acid) and ammonia (base) were regenerated from ammonium sulfate using a thermal cracking method. Raman spectroscopy was used for primary analysis of the ammonium hydrogen sulfate product formed to determine the optimal reaction rate (80°C/min) and to study the role of ammonium pyrosulfate in this reaction.