The location of transition ions in copper- and copper-zinc-loaded Y type zeolites prepared by different procedures has been studied by temperature-programmed reduction, infrared spectroscopy of CO adsorbed on pretreated samples and X-ray photoelectron spectroscopy. Samples outgassed at 673 K showed Cu+ species due likely to reduction of Cu2+ ions under vacuum. Over exchanged CuY zeolites copper species in exchange sites were detected, while an impregnated sample exhibited bands of CO adsorbed on both Cu2+ and Cu+ ions developed at the surface of CuO crystals, and small proportions of Cu+ ions located in accessible exchange sites S-II and S-II’. Similar findings were observed in Zn- and Cu-exchanged zeolites although the relative proportion of Cu in S-I positions was decreased due to competition between Cu2+ and Zn2+ ions. Samples reduced in hydrogen at 523 K showed the appearance of Cu-0 species in impregnated samples, whereas Cu+ dominated in the exchanged counterparts. Reduction at 598 K led to substantial changes in Cu-exchanged samples in water. The proportion of Cu+ species decreased by reduction to CuO and simultaneously migration to Cu+ to S-II’ sites occurred. While Cu2+ or Cu+ were found on outgassed samples, only Cu-0 and intrazeolite Cu+ were observed after Hz-reduction at 623 K. Changes in copper exposure as a function of sample pretreatments were also revealed by X-ray photoelectron spectroscopy.