Toluene nitration with mixed acid is a very complex process, because there are many reactions involved in the nitrotoluene production process, such as mononitration as a main reaction, dinitration, trinitration, oxidization, and decomposition of products as side reactions. Therefore, it is difficult to calculate an accurate MTSR for thermal hazard evaluation of the desired reaction. Here, isothermal reactions at 30 °C -70 °C were carried out by reaction calorimeter RC1e, and products in the organic phase were analyzed by GC-MS.