A combustion system is described which makes possible the routine preparation of large numbers of biological samples for scintillation counting. The system accepts a variety of sample materials, and a method is provided for evaporating tissue homogenate in gelatin or plastic capsules. An operator drops a capsule in the furnace and collects the combustion products in scintillation solvent, ready for counting, at a rate of 1 sample every 3 min. The system accepts samples of at least 500 mg, limited by solvent capacity for water. A favorable comparison with the oxygen flask method is shown and there is minimum carryover of activity in successive samples. The method has a collection recovery of 96%, is calibrated by internal standards, and shows a coefficient of variation of 2.9%. © 1969.