The objectivesof thiswork wereto fabricate Cu(I)–Y zeolite nanoparticlesforthe delsulfurizationof commercial gasoline and diesel using fixed-bed adsorption processes at room temperature. The Cu(I)–Y zeolite prepared in the present study showed that the breakthrough capacities of 21 and 9 mg/g of adsorbents of diesel and gasoline, respectively at 298 K for sulfur removal. Under the same experimental conditions, the saturation loadings were 36 and 23 mg/g for diesel and gasoline, respectively. Moreover, the structural morphology, crystallinity, fine structure and characteristics of the adsorbents were also systematically investigated. TPR profile of Cu(II)–Y zeolite indicated that the two reduction steps at 462 and 509 K, respectively were observed. A reduction temperature of about 462 K is sufficient to obtain the cuprous species required for π-complexation. EXAFS spectra showed that the bond distances of Cu–S in Cu2S and CuS were 2.35 and 2.47 A, respectively in the sulfur-adsorbed Cu–Y adsorbent.