The development of a spectroelectrochemistry assembly for substractively normalized interfacial FTIR spectroscopy (SNIFTIRS), based on the commercial spectrophotometer Unicam Research Series 1, is presented. The sample chamber has been modified to achieve a vertical orientation of the cell and a special support was constructed for the same purpose. The original path of the IR radiation has been modified by using two black anodized aluminium 30° wedges, both supporting a parabolic mirror. This allows the radiation to reach the working electrode forming 60° with the vertical. The cell holder allows vertical and horizontal displacement of the cell. The electrochemical cell was made of Pyrex glass and permits an easy manipulation even in the sample chamber of the spectrometer, making it unnecessary to open this chamber in the manipulation of either the solution or the electrodes. The working electrode was a polished polycrystalline gold electrode. A computer‐based potentiostat was also constructed. To control the system, a set of 16‐bits Visual‐Basic programs was developed allowing the synchronization between the spectra acquisition and the application of potentials. A variety of sequences of operation can be selected. The system was checked with the ferrocyanide/ferricyanide redox couple, concluding that the system here described is useful to make SNIFTIRS experiments, being versatile enough to design new operational sequences that help improve the knowledge of the electrode processes.