Correlation dependences of the Raman spectroscopy parameters of carbon materials on the heat treatment temperature (HTT) are obtained. It is proposed to use the ratio of the integral intensities of the bands D and G, I D /I G , to obtain the most accurate and reproducible results. The choice of carbon fiber (CF) based on polyacrylonitrile (PAN) as witness samples is experimentally justified. It is shown that, for the studied PAN-based CF samples after heat treatment in the treatment temperature range of 1000-3000°C, the parameter I D /I G correlates well with the parameters of X-ray diffraction analysis. A number of examples of the application of the Raman spectroscopy method of witness samples are considered for determination of the "effective" HTT of carbon materials in technological processes for the production of carbon-carbon composite materials, artificial graphite, and PAN-based CF, as well as determination of the temperature fields of both laboratory and industrial equipment designed for high temperature treatment of carbon materials in the temperature range of 1000-3000°C, in particular, in Tamman furnaces, resistance electric vacuum furnaces, and Acheson furnaces.