Abstract: The accuracy and timeliness of total sulfur determination result are of vital importance for intelligent control of production process. For evaluating the accuracy of total sulfur determinations by prompt gamma neutron activation analysis (PGNAA) method and coulometric titration method (CTM), a study is made on the measuring accuracy of each method using bifactor method with the bunkered raw coal of a coal preparation plant as test sample. Study result shows that the standard deviation of CTM method is 0.042% while that of the PGNAA method is 0.018%; and comparatively, the PGNAA method is superior to the CTM method in terms of accuracy and timeliness.