Recently the use of brown sugar has increased due to its nutritional characteristics, thus requiring a more rigid quality control. The development of a method for water content analysis in soft brown sugar is carried out for the first time by TG/DTA with application of different statistical tests. The results of the optimization study suggest that heating rates of 5 °C min−1 and an alumina sample holder improve the efficiency of the drying process. The validation study showed that thermo gravimetry presents good accuracy and precision for water content analysis in soft brown sugar samples. This technique offers advantages over other analytical methods as it does not use toxic and costly reagents or solvents, it does not need any sample preparation, and it allows the identification of the temperature at which water is completely eliminated in relation to other volatile degradation products. This is an important advantage over the official method (loss on drying).