Interaction of hydrogen with metallic multi-layered thin films remains as a hot topic in recent days Detailed knowledge on such chemically modulated systems is required if they are desired for application in hydrogen energy system as storage media. In this study, the deuterium concentration profile of Fe/V multi-layer was investigated by atom probe tomography (APT) at 60 and 30 K. It is firstly shown that deuterium-loaded sample can easily react with oxygen at the Pd capping layer on Fe/V and therefore, it is highly desired to avoid any oxygen exposure after D(2) loading before APT analysis. The analysis temperature also has an impact on D concentration profile. The result taken at 60 K shows clear traces of surface segregation of D atoms towards analysis surface. The observed diffusion profile of D allows us to estimate an apparent diffusion coefficient D. The calculated D at 60 K is in the order of 10(-17) cm(2)/s, deviating 6 orders of magnitude from an extrapolated value. This was interpreted with alloying, D-trapping at defects and effects of the large extension to which the extrapolation was done. A D concentration profile taken at 30 K shows nosegregation anymore and a homogeneous distribution at C(D) = 0.05(2) D/Me, which is in good accordance with that measured in the corresponding pressure-composition isotherm. (C) 2008 Elsevier B.V. All rights reserved.