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The development of Fricke gel (FG) dosimeters based on poly(vinyl alcohol) (PVA) as the gelling agent and glutaraldehyde (GTA) as the cross-linker has enabled significant improvements in the dose response and the stability over time of spatial radiation dose distributions. However, a standard procedure for preparing FG in terms of reagent concentrations is still missing in the literature. This study aims to investigate, by means of spectrophotometric analyses, how the sensitivity to the radiation dose and the range of linearity of the dose–response curve of PVA-GTA-FG dosimeters loaded with xylenol orange sodium salt (XO) are influenced by ferrous ammonium sulphate (FAS) and XO concentrations. Moreover, the effect of different concentrations of such compounds on self-oxidation phenomena in the dosimeters was evaluated. PVA-GTA-FG dosimeters were prepared using XO concentrations in the range 0.04–0.80 mM and FAS in the range 0.05–5.00 mM. The optical absorbance properties and the dose response of FG were investigated in the interval 0.0–42.0 Gy. The results demonstrate that the amount of FAS and XO determines both the sensitivity to the absorbed dose and the interval of linearity of the dose–response curve. The study suggests that the best performances of FG dosimeters for spectrophotometric analyses can be obtained using 1.00–0.40 mM and 0.200–0.166 mM concentrations of FAS and XO, respectively. [ABSTRACT FROM AUTHOR]