Abstract: Measurement of sulfur content of solid and liquid fuels is restricted by the lack of certified reference material (CRM) of organic pure substance for sulfur, which can not meet the demand for traceability. In this paper, the CRM of dibenzothiophene for sulfur content labeled as GBW 06204 was developed, and an internationally advanced method for determining the elemental content of organic pure substances was adopted, that is, based on the content of each component and its molecular content of the element to be measured, the elemental content of the standard substance was calculated to obtain the determined value. Among them, the organic impurity content was determined by using gas chromatography-spectrometry and differential scanning calorimetry. The water content was determined by Karl Fischer coulometric titration. The inorganic impurity content was determined by the residue on ignition. The certified value of CRM was traceable to the mass of pure substances, temperature, and atomic weight. The certified sulfur content of CRM was 17.403% with an uncertainty (U) of 0.005%, which has reached the international advanced level. This CRM is suitable for the calibration of elemental analyzers such as the Dumas method, and the preparation of CRM of petroleum for sulfur content, which is helpful for the accuracy and reliability of sulfur content results of fuels.