Properties of physical vapor deposited diamond-like carbon films and the migration of hydrogen in co-deposited samples were studied. Measurements utilizing Rutherford backscattering spectrometry and Doppler-shift-attenuation techniques were used to obtain the average mass density of the films. Distributions of co-deposited hydrogen and deuterium were measured by the nuclear resonance reaction 1H (15N,αγ)12C, and the elastic recoil detection technique, respectively. Secondary ion mass spectrometry was also used in combination with these two methods. It was observed that in H and CH4 co-deposited DLC films the temperature of H release varied between 950 and 1070°C depending on the H concentration.