The efficiency of Mehlich‐3 reagent as an extractant for aluminum (Al) and iron (Fe) was studied in Galician coal mine soils, in the process of reclamation. Mehlich‐3 Al and Fe values were compared to those from other Al and Fe tests and with phosphorus (P) sorption. The soils are very heterogeneous, consisting mainly of carbonaceous and non‐carbonaceous clays and shales, which are often rich in pyrite. Some of them have been amended with topsoil or fly ash. One hundred forty samples, from 0 to 15 or 15 to 30 cm, were analyzed. The pH values ranged from 2.7 to 8.4; oxalate and pyrophosphate Al from 0 to 1.17%, and 0.02 to 0.58%, respectively; and oxalate and pyrophosphate Fe from 0.02 to 2.25% and 0 to 1.28%, respectively; PSI (P sorption index) values varied between 0 and 55.1. The Mehlich‐3 Al values ranged from 24 to 2600 mg kg‐1. A close relationship was observed between Mehlich‐3 and oxalate Al values (r=0.77), although the regression line tended to be curvilinear. Mehlich‐3 Al was better correlated than oxalate Al to pyrophosphate Al (r=0.66 vs. r=0.59) and also to pH‐NaF (r=0.89 vs. r=0.74). The Mehlich‐3 Al is almost as good as oxalate Al in estimating non‐crystalline Al, the correlation coefficients between log PSI and log (Mehlich‐3 Al) or log (oxalate Al) being 0.51 and 0.57, respectively. The Mehlich‐3 Fe correlated to available (r=0.63), exchangeable (r=0.65) and soluble Fe (r=0.66), but not to non‐crystalline Fe.