Intermetallic nanoparticles of PtPb have been prepared by femtosecond pulsed laser ablation in methanol and their steady-state electrochemical response for oxidation of formic acid was reported. The weight based average particle size was 29 +/- 20 nm. The steady-state current-voltage (J-E) response of the nanoparticles for oxidation of formic acid was examined and the onset potential for oxidation was 200 mV vs. NHE, the peak current potential was 440 mV vs. NHE, and the mass activity was 130 mA mg(-1) Pt. The composition and crystal structure of the particles were probed using X-ray crystallographic techniques. The method produced intermetallic particles without the use of surface modifying groups, resulting in nanoparticles which had an electrochemical response similar to bulk PtPb without further purification. The size, composition, and crystal structure of the particles obtained with this method are discussed. (C) 2012 The Electrochemical Society. [DOI: 10.1149/2.055302jes] All rights reserved.