The normalized distillation procedure is not a universal test for measuring the volatility of pitch. It has been found that during this test the liquid sample is exposed to temperatures in excess of 400ยฐC and decomposes extensively. Therefore, the distillate measured includes not only the low-boiling constituents originally present in the sample but also those formed by thermal decomposition. This has been observed in the case of petroleum pitches and not with coal-tar pitches. A new method has been developed for measuring the volatility of pitches, based on the diffusion through a small orifice into a stream of nitrogen of hydrocarbon vapours emanating from a large-size sample maintained at 200ยฐC. The hydrocarbons in the stream of nitrogen are measured with a flame-ionization detector. The peak height obtained during this measurement is calibrated against a standard mixture of methane in nitrogen. The signals from it are related to the concentration of volatile hydrocarbons over the heated sample of pitch and are expressed in gram atoms carbon per cubic metre of gas at the temperature of measurement. The volatility method was compared with the distillation test ASTM D-2569 for pitches and evaluation test ASTM D-972-56 for lubricating oils and greases. The procedure was found suitable for routine control testing of hydrocarbon materials (pitches) with very low volatility.