Electrical properties of detonation diamond nanoparticles (NDs) with individual diameters of ∼5 nm are important for many applications. Although diamond is an insulator, it is known that hydrogen-terminated bulk diamond becomes conductive when exposed to water. We show that heating ND in hydrogen gas at 600-900 °C resulted in a remarkable decrease in resistivity from 107 to 105 Ω cm, while the resistivity was essentially unchanged after treatment at 400 °C and lower temperatures. Fourier Transform Infrared Spectroscopy and X-ray photoelectron spectroscopy (XPS) studies revealed that hydrogenation of ND occurs at 600-900 °C, suggesting that the decrease in resistivity is based on transfer doping at the hydrogenated ND surface. Oxidation of the hydrogenated sample at 300 °C recovers resistivity to its original value. The resistivity of treated ND as a function of the O/C atomic ratio showed a transition from resistive (O/C ratio > 0.033) to conductive (O/C ratio < 0.033) state. This is consistent with the idea that the change in the resistivity is caused by the shift of the valence band maximum to above the Fermi level due to the dipole of the C-H bonds leading to transfer doping.