The 0.9FeTiO3–0.1Fe2O3 solid solution was prepared by solid state reaction with FeTiO3 and α-Fe2O3 powders, and studied by x-ray diffraction, Mössbauer spectroscopy, and vibrating sample magnetometer (VSM). The crystalline structure was found to be single phase rhombohedral structure with lattice constant a = 5.089 Å and c = 14.051 Å. Mössbauer spectra of 0.9FeTiO3–0.1Fe2O3 solid solution were taken at various temperatures ranging from 4.5 to 300 K. The anomalous absorption curves at low temperature are observed. Mössbauer spectra at 4.5 K was fitted to four six-line hyperfine pattern with magnetic hyperfine fields H hf = 504, 424, 115, and 58 kOe, respectively. At 40 K the spectrum shows the mixture of ferromagnetic six-line pattern and paramagnetic two-line and above 50 K it show asymmetry two-line patterns. The fitted curves at room temperature are obtained by superimposing two doublets corresponding to Fe2 + and Fe3 +. The isomer shift δ and quadrupole splitting ΔE Q of sample are 0.92 and 0.69 mm/s for Fe2 + and 0.14 and − 0.29 mm/s for Fe3 +, respectively. Corresponding relative absorption subspectral areas are 89.2% for Fe2 + and 10.8% for Fe3 +. Magnetization measurements indicate ferromagnetic behaviour with 92 Oe coercivity value at 50 K but at 300 K it show no hysteresis loop.