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A high-sulfur coking coal obtained from Shanxi province in northern China was desulfurized by microwave/HAc–H 2 O 2 treatment. The main properties of coal samples before and after desulfurization treatment, including the elemental composition, caking index, organic constituents and sulfur content were analyzed. Experimental results showed that microwaving treatment at 500 W for 40 s combined with HAc–H 2 O 2 (1:5 v/v) resulted in a yield of 99.27% clean coal and a desulfurization rate of 22.62%. Proximate and ultimate analyses showed that the ash content in coal was decreased from 9.09% to 7.90%, while the volatile matter significantly increased by 0.75%, and that the oxygen concentration in the coal increased from 4.15% to 7.08% following treatment. After desulfurization, the decreases in the caking index (from 72.4 to 45.42) and the impairment of calorific value was also observed. The negative impacts on the technological properties of coking coal may be attributed to oxidization caused by a HAc–H 2 O 2 addition with the acceleration of microwaving. Results from FT-IR and XPS analyses depicted a considerable increase in oxygen-bearing functional groups, in accordance with results obtained by an ion-exchange titration method. These findings confirmed that the oxidization plays an important role in the present desulfurization process, and takes a dominant responsible for the changes of various properties of coal. [ABSTRACT FROM AUTHOR]