A kind of desulfurization adsorbent, (Ni/W)-gamma-Al2O3 microsphere, was prepared by a new method of in situ chemical reduction. The adsorbent consists of active components (transition metals Ni and W) and a carrier (gamma-Al2O3). Ni and W in gamma-Al2O3 microspheres are fine in size and can be distributed homogeneously on the surface and inside of the gamma-Al2O3 carrier. The desulfurization of the adsorbent made by the in situ chemical reduction method was carried out in model gasoline. Its desulfurization capacity increases 23% in comparison with that made by the conventional impregnation method. The composition and configuration of adsorbents were analyzed by scanning electron microscopy (SEM), electron energy dispersive X-ray spectroscopy (EDX), and X-ray diffraction (XRD). The in situ chemical reduction method offers a new and promising method for preparation of desulfurization adsorbents containing active components.