SrSO4:Dy,Tb nanocrystalline with crystalline size in the range of 44–54 nm was prepared by co-precipitation method followed by thermal treatment and characterized by X-ray diffraction(XRD), scanning electron microscopy(SEM), energy dispersive X-ray spectroscopy(EDX) and UV-visible spectrometry. Our results provided direct evidence of incorporation of impurities into nanocrystalline SrSO4. The thermoluminescence(TL) properties of SrSO4:Dy,Tb nanocrystalline pellets irradiated with gamma rays at different doses were studied. The TL glow curve of SrSO4:Dy,Tb nanocrystalline pellets had a prominent peak at around 490 K and a small peak at around 430 K. The major peak in the TL glow curve was almost resolved from other peaks, which was analyzed using Chen’s peak shape method to determine the TL kinetic parameters such as activation energy, E and kinetic order, b. The intensity of main dosimetric peak of SrSO4:Dy,Tb nanocrystalline pellets at around 490 K increased linearly with the increase in gamma dose. The TL response was linear in the range of 0.1–7 kGy. These properties made it a candidate as a dosimeter to be used for estimating the high dose of gamma rays. SrSO4: Dy, Tb nanocrystalline with crystalline size in the range of 44-54 nm was prepared by co-precipitation method followed by thermal treatment and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X- The results of incorporation of impurities into nanocrystalline SrSO4. The thermoluminescence (TL) properties of SrSO4: Dy, Tb nanocrystalline pellets irradiated with gamma rays at different doses were studied. The TL glow curve of SrSO4: Dy, Tb nanocrystalline pellets had a prominent peak at around 490 K and a small peak at around 430 K. The major peak in the TL glow curve was almost resolved from other peaks, which was analyzed using Chen’s peak shape method determine the TL kinetic parameters such as activation energy, E and kinetic order, b. The intensity of main dosimetric peak of SrSO4: Dy, Tb nanocrystalline pellets at around 490 K increased linearly with the increa se in gamma dose. The TL response was linear in the range of 0.1-7 kGy. These properties made it a candidate as a dosimeter to be used for estimating the high dose of gamma rays.