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The structural analysis of strontium hexaferrites SrFe x O 19 (for x = 12, 11 and 10) and substituted samples Sr 0.7 Nd 0.3 Fe 12−y Co 0.3 O 19 (for y = 0.3, 1.3 and 2.3) prepared through the citrate precursor method is shown. Nd and Co substitution modifies saturation magnetization (M S ) and increases coercivity (H c ) in samples heat-treated at 1100 • C for two hours. Mössbauer analyses show different iron occupancy and the influence of the Fe 3+ content is particularly emphasized. Hematite segregation is observed for some compositions. Samples with low Fe 3+ content show the best magnetic properties with no secondary phase segregation.