A method for simultaneous investigation of the diffusion of atoms and molecules in gas buffers and their reflection at the vessel walls is proposed. It is experimentally tested to obtain the diffusion coefficient of Mg atoms in neon and the coefficient of the reflection of these atoms from the metallic wall in the afterglow plasma of a pulsed hollow cathode at 320 K temperature. The diffusion coefficient value is compared with the theoretical calculation previously reported by Redko et al.