A new temperature-induced deposition method for anchoring metallic nanoparticles onto smooth/refelective polycrystalline Au (Au-poly) and classy carbon (GC) substrates has been developed for in situ infrared reflection-absorption spectroscopy (IRAS). Characteristic vibrational spectra for CO adsorbed on anchored nanoparticles of Pt/C, Pt3Sn/C, Pt3Mo/C, and Pt2Ru3/C are presented. When An is used as a substrate, CO adsorbed on An can interfere with bands for CO adsorbed on nanoparticles. By contrast, if GC is used as a substrate, CO adsorbed on nanoparticles are as expected from corresponding spectra obtained from Pt and Pt-bimetallic electrodes.