A very relevant aspect of using DEMS is to determine the on-set potential for gas release when charging the positive electrode of LIBs or SIBs. In this case, gas release can be due to electrolyte oxidation and/or due to structural degradation of the electrode . This is especially relevant for SIBs, as the highly studied family of layered oxides show a very sloping voltage profile, which complicates the determination of an upper cutoff potential that enables safe and prolonged cycling. Most of the layered oxides studied for SIBs are cycled above 4 V which may easily cause electrolyte decomposition. For precisely determining the relevant electrode potentials, the use of a 3-electrode setup is generally of advantage.