To develop an effective process for the recovery of precious metals from scrap, we investigated a new platinum extraction process using alloy formation by magnesium vapor and successive leaching with an aqueous solution. Pure platinum plates were reacted with magnesium vapor at constant temperatures ranging between 873 and 1173 K for 3 h, and Mg–Pt alloy samples were synthesized. The obtained Mg–Pt alloy was then dissolved in aqua regia or in an aqueous HCl solution at room temperature. Platinum was recovered from the leaching solution by conventional precipitation technique, and the platinum obtained by each process was analyzed chemically. It was found that 94% of the platinum was recovered by this process. After Mg vapor treatment, 100% of the platinum was dissolved when kept in aqua regia for 1 h, whereas only 25% of untreated pure platinum was dissolved when kept in aqua regia for 4 h.