The annealing treatment and pH were controlled to prepare a bimetallic PtRu/C anode catalyst by the citrate-stabilized chemical reduction method. X-ray diffraction and X-ray photoelectron spectra revealed that the catalyst before the annealing treatment showed smaller size particles mainly composed of metallic platinum and hydrous ruthenium oxide. The anhydrous RuO 2 increased with increase in the annealing temperature from 250°C to 400°C. The linear sweep voltammetry (LSV) results showed that the non-annealed catalyst had the highest current density at a given potential. Also, the particle size varied with the stabilizing pH. A homogenous catalyst was prepared at a pH of 7 in the laboratory. The particle size was about 2.39±0.46nm with 14.62at% ruthenium in the PtRu alloy. The maximum LSV current density was 66.4mAmg −1 PtRu at 0.45V with an onset potential of 0.12V (versus SCE). The catalyst when tested in a single cell DMFC produced a power density of 67.5mWcm −2 at a current density of 240mAcm −2 .