This article is the first to report the direct, one-step synthesis of molybdenum blue (MB) in solid state, via application of cyclic voltammetry. Electrochemical synthesis of MB was carried out in a three-electrode cell in 1.0 M sulfuric acid and at the appropriate amount of sodium molybdate dihydrate. Both a pencil graphite electrode and a platinum plate electrode were used as working electrodes. The structure of electrochemically synthesized MB was characterized using such techniques as Ultraviolet-visible spectroscopy, Fourier Transform Infrared Spectroscopy, Resonance Raman Spectroscopy, Scanning Electron Microscopy, Energy-Dispersive X-Ray Spectroscopy, X-Ray Powder Diffraction, X-ray Fluorescence Spectroscopy, and X-Ray Photoelectron Spectroscopy. In addition, the electrochemical behavior of the synthesized MB was examined via cyclic voltammetry. Finally, the determination of phosphate was conducted using a UV-vis spectrometer with electrochemically synthesized MB.