The 0.9FeTiO 3 -0.1Fe 2 O 3 solid solution was prepared by solid state reaction with FeTiO 3 and α-Fe 2 O 3 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 0.9FeTiO 3 -0.1Fe 2 O 3 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 Fe 2+ and Fe 3+ . The isomer shift δ and quadrupole splitting ΔE Q of sample are 0.92 and 0.69 mm/s for Fe 2+ and 0.14 and −0.29 mm/s for Fe 3+ , respectively. Corresponding relative absorption subspectral areas are 89.2% for Fe 2+ and 10.8% for Fe 3+ . Magnetization measurements indicate ferromagnetic behaviour with 92 Oe coercivity value at 50 K but at 300 K it show no hysteresis loop.