Adsorptive desulfurization (ADS) of thiophene containing n-octane at low S-concentrations (≤70 ppmw) was performed under dynamic (flow) conditions in a fixed bed of Cu/Ni nanoparticles (NPs)-dispersed carbon nanofibers (CNFs). Briefly, Cu-CNFs were prepared using chemical vapor deposition with acetylene as the carbon source and the Cu NPs as the catalyst. The metal NPs also served as a support for the CNF-growth. The Ni/Cu-CNFs of different particle sizes (0.20, 0.35 and 0.50 mm) were synthesized by impregnating the heat treated Cu-CNF with Ni salt, pelletizing it using the phenolic resin binder, followed by calcination, H2-reduction, and pulverization to the required particle sizes. The adsorbent showed the BET surface area of ∼350 m2/g, metal nanoparticle-size of 5–25 nm, and thermal stability over 30–900 °C. The prepared adsorbent material was easily pelletized to the cylindrical shape, with the pellet showing high mechanical strength (∼1900 kPa). Breakthrough experiments showed the adsorbent to be capable of suppressing concentrations at or below 1 ppmw-S, with the breakthrough and saturation capacities determined to be 0.25 and 0.60 mg-S/g-adsorbent, respectively at 30 °C and 35 ppm (w/w) S-concentration, which were comparable with those of adsorbents discussed in literature for the ADS of lean sulfur containing fuels.