Chemical Laboratory, R&D and Scientific Services, Tata Steel Limited, Jamshedpur-831 001, Jharkhand, India E-mail : shrenivas@tatasteel.com, r.chatti@tatasteel.com The estimation of sulfur in coal by combustion followed by iodometric titration is discussed in the present study. The inherent advantage of this method is a rapid and accurate analysis of sulfur content iu coal, when compared to the conventional techniques like the wet chemical method using Eschka mixture and followed by precipitation by BaC12 solution as barium sulfate and Eschka mixture method combined with Inductively Coupled Plasma Emission (ICP) Spectrometric analysis. The present work describes the use of a combustion-iodometric titration method in the subsequent sections of the paper. The method has been validated by measuring sulfur content in different certified reference materials and it was found that the values of sulfur measured by this method are in agreement with the certified values. The present method is also environment friendly due to avoidance of use of chromic oxide as the oxidant and perchloric acid as part of the absorption solution.