The advantages of polarography at higher temperatures are that degassing is not necessary, maxima are less frequent, and sensitivity is greatly increased. The variation of diffusion current was linear with molarity and with temperature. The half‐wave potentials tended to shift to more negative values with increasing temperature and concentration. The diffusion current varied inversely as the square root of the viscosity of the solvent. Benzaldehyde, fumaric acid, meta‐ and para‐nitrobenzoic acid, and nitrocycloheptane were reduced at the dropping mercury electrode. The supporting electrolyte was 0.1M lithium chloride, with silver‐silver chloride as a reference electrode. The temperature range was 70° to 120° C.