To develop a recovery process of valuable materials like Ag, Au and polycarbonate from used CD-R and DVD-R, the separation and recovery of Ag and polycarbonate in a CD-R were investigated. Ag leaching from a CD-R was carried out using HNO(3) and thiourea solution as a leachant. The total amount of Ag in the CD-R can be dissolved with over 3.5 mol/dm(3) HNO(3). In the case of Ag leaching with below 2.0 mol/dm(3) HNO(3), it is possible to increase both leaching velocity and leaching percentage by increasing the leaching temperature. In this HNO(3) concentration range, ultrasonic irradiation also promotes Ag leaching from the CD-R. Ag leaching increases with an increase in the concentration of thiourea solution, but the blue pigment component in the CD-R is not dissolved by thiourea solution. Ag leaching can be improved by increasing the leaching temperature, in leaching with thiourea solution and a lower concentration of HNO(3). By this method, the Ag and pigment component in the CD-R can be recovered in the leachant, and the polycarbonate is also obtained as a residue.