A newly designed spectroelectrochemical cell was constructed for surface X-ray scattering (SXS) to study single crystal electrodes. Electrochemical characteristics of a specific face of a single crystal electrode can be investigated in the meniscus mode, and SXS measurement can be easily carried out using the spectroelectrochemical cell. The usefulness of the present cell was demonstrated by studying the electrochemical deposition of thin Pd layers on Au(111) and An(100) that require precise amounts of Pd deposits.