The investigation of ancient pottery has become important over the past century and provides the archaeologist with information on the technology, trade and culture of the past [1]. An analytical study of potsherds is usually complex and includes spectroscopic techniques, X-ray diffraction, electron and visual microscopy, chemical analysis and so on. Thermal analysis is a good tool for checking quality in the production of ceramics [2]. It allows to evaluate the conditions of firing and to analyze raw clay materials and products. The main temperature effects are: for dehydration 22-350oC, for dehydroxylation 350-600 oC and for decomposition of carbonates, mica, etc. 600-850 oC, so usual experimental temperature interval is from room temperature up to 950 oC. The results of measurements were shown [3] to depend on temperature profile throughout the wall of a pot during the thermal treatment under the firing and cooking meal. Here it will be reported the results of thermal analysis of shreds samples from Rakushechny Yar and Serteya excavations of Early-Late Neolithic in Dnepr-Dvina region [4]. TG and DSC investigation in temperature range up to 1200 oC (STA 409 C/CD NETZSCH) was held. Difference in mass loss and values of temperatures shows that samples of pottery from different excavations have different sources of clay. Inner and outer sides of shreds are different by mass loss with increasing of temperature: inner sides lose more as result of the contact with cooking meal. According to DSC curves there are thermal effects above 1000 oC in both cases due to mullite formation. Presented results will be used in the analysis of ceramics manufacture techniques and useful for further integrated ancient pottery investigations and their interpretations. The work was performed in Thermogravimetric and Calorimetric Research Center of Saint Petersburg State University.