AbstractIntense biogeochemical transformations in sediments and biofilms may occur over sub‐mm distances. Our current understanding of those transformations in such narrowly stratified environments has been facilitated by the introduction of microsensors. Until now most studies have been conducted using individual sensors for the various chemical species, and careful vertical alignment of the sensor tips is then essential for the meaningful interpretation of the resulting data. For instance, the determination of total dissolved sulfide (TDS) at high resolution requires perfect alignment of sensors for H₂S and pH, as the pKa for H₂S is close to ambient pH. In this study, we show how a recently developed TDS sensor and a new combined H₂S/O₂microsensor can improve the analysis of sulfidic environments including the oxygen–sulfide interface. The TDS sensor does not require pH correction unlike the conventional H₂S sensor, and it thus eliminates the need for a simultaneous pH measurement. The combined sensor allows for perfect alignment of H₂S and O₂micro profiles and makes it possible to not only more accurately estimate fluxes, but also to determine overlapping zones of oxygen and dissolved sulfide at very high resolution.