The presented article describes the method for determining one of the trace elements occurring in coalbismuth. The subjects of the analysis were coal type 34, 35 and their fly ashes derived from Jastrzębska Spółka Węglowa. The main reason for the research was the extensive use of bismuth in many industry sectors. Additionally, bismuth is on the list of deficit elements, therefore the possibility of obtaining an alternative for its recycling source of it is needed, is required. The research was carried out using atomic absorption spectrometry with electrothermal atomization in a graphite cuvette. The samples were incinerated at 800°C and microwave mineralization in a high-pressure closed system was performed until the spectrometric analysis was achieved. In order to achieve mineralization, a mixture of HF and HNO3 acids was used to turn the samples into acidic solutions. The preparation of the samples was based on available literature data and own observations. In the experiment, the effects of the additive modifier was modified by changing the temperature in further steps: drying, incineration, cooling, atomization and burning were described. In addition, the palladium modifier was used in order to limit secondary reactions and enable the evaporation of matrix components. The measurement conditions which are presented in this article allow for a linear calibration curve to be established. However, this is not clear and the definitive method for determining the bismuth in coal is carried out through the use of ET-AAS.