For volume reduction of organic alpha waste and plutonium recovery, a pyrohydrolytic process has been developed in laboratory scale up to 4.16 × 10−4. kg waste/s (1.5 kg/h). In this process the organic compounds are reacted with steam in the temperature range of from 873 to 1123 K. This new process shows some remarkable benefits—good control of the temperature by its endothermic course and therefore easy plutonium recovery from the ashes; low quantities of secondary waste and high decontamination factors resulting from low gas velocities; the ability to complete the process using metal-made equipment. The technical design of a pilot plant with a throughput of from 6.94 × 10−3 to 1.38 × 10−2 kg waste/s (25 to 50 kg/h) is available.