The determination of mercury in coal is of interest due to its extreme volatility during coal combustion and its potential to be toxic if released into the environment. However, the low concentration of mercury in coal, frequently at the low μg/g level, makes analysis extremely difficult. In addition, mercury`s volatility makes sample cross-contamination more likely. Despite the emphasis placed on mercury analysis, the analytical method of choice to give accurate, reproducible results for coal samples remains debatable. This report describes the radiochemical neutron activation analysis method based on pyrolysis followed by double gold amalgamation. During pyrolysis, volatile elements such as mercury and selenium are liberated, and the mercury is preferentially collected by amalgamation with the gold.