We propose a simple chemiluminescence (CL) method for investigation of the surface of Co-based nanocrystals (NCs). Using a combination of CL and spin-trap electron paramagnetic resonance techniques, we systematically studied the generation of reactive oxygen species (ROS) at the surface of differently sized CoPt3 spherical NCs and CoPt3/Au nanodumbbells. We have shown that differently sized CoPt3 NCs can promote the formation of ROS and as a result can lead to the oxidation of luminol accompanied by the emission of the light. CL allows monitoring the stability of transition-metal-based NCs against oxidation and dissolution. We found by CL that cobalt ions slowly leach from the surface of CoPt3 NCs even under very mild conditions, however, the amount of the leached cobalt ions does not exceed the maximal concentration of cobalt at the NC surface indicating that only surface atoms can go into solution