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• Rapid devolatilization of carbonaceous materials investigated for HIsarna technology. • Rapid heating via drop tube furnace with quadrupole mass spectrometer (DTF-QMS). • Explained the effect of temperature on variation of light gases in the rapid devolatilization. • Revealed the effect of temperature on the rate of carbon conversion for coal and charcoal. • R-factor obtained to give solid residual efficiency for different carbon sources. A drop-tube furnace coupled with quadrupole mass spectrometer (DTF-QMS) was employed to simulate rapid heating conditions that carbonaceous materials experience during HIsarna injection with the measurement of gas composition change as a result. A devolatilization study for thermal coal (TC) and charcoal (CC) samples was carried out at three temperatures of 1000, 1250 and 1500 °C under an initial high purity Ar gas environment. The volatiles released were measured online by QMS, while the char yield was determined directly by the weight of particles collected and the deficit was calculated by subtracting the gas yielded from the total weight loss. The study reveals that working temperature has a strong impact on the devolatilization rate, the maximum weight loss and the variation in gas species produced. Due to intensification in the carbon oxidation and secondary reactions at higher temperatures, there was an increase in the weight loss, which led to a greater yield of H 2 and CO but less yield of hydrocarbons, CO 2 and H 2 O. Despite lower volatile matter content in charcoal, the weight loss for charcoal (29%) was higher than that for thermal coal (23%) at 1500 °C. Although the amount of H 2 produced for both materials is similar, the amount of CO produced by charcoal is twice of that by thermal coal, and accounts for 79% of the total gas weight formed by charcoal. This suggests that a higher rate of carbon oxidation takes place through O 2 containing groups within the charcoal, which results in lower char efficiency. It was found that thermal coal produces a significant amount of tar, while a large number of particles in the form of soot/dust escaped from the bulk material during charcoal injection but no tar formation was observed. [ABSTRACT FROM AUTHOR]