The synthesis and thermoluminescence (TL) characterization of self-agglomerating pellet-shaped CaSO 4 phosphors, through a low cost and environmentally friendly method is reported. In order to investigate their TL features, some samples were exposed to beta particle irradiation in the dose range from 0.07 to 10 Gy. Characteristic TL glow curve consists of a single main maximum located at 216 °C, which is considered stable, hence, suitable for dosimetry applications. The dose-response was remarkable linear. Moreover, the lower detection limit was determined to be 6.0 μGy, and the relative TL sensitivity twice the one from the commercial TLD-100 dosimeter.