High-purity lead discs were prepared using several combinations of polishing, rinsing and ultrasonic treatment. Physical degradation of the lead surface and the premature generation and deposition of oxides on the surface were observed for certain combinations of preparation steps. Ultrasonic treatment of the discs was found to be particularly detrimental as it induced significant crystal growth and, in several instances, deterioration of the polished surface. Simple air drying of freshly rinsed discs also led to oxide formation on the surface after as short a time as 1 min. An effective method for preparing discs from high-purity lead is described.