A convenient and accurate analytical procedure has been developed for the trace determination of tetramethylthiuram disulphide in commercial fungicides and rubber accelerators for the purpose of quality control. Thiuram disulphide gives a well defined, diffusion controlled cathodic wave in 0.01 M pyridinium perchlorate in dimethylformamide with half-wave potential -0.36 V against a saturated calomel electrode. Determination has been made by normal pulse and differential pulse polarography using linear calibration plots.