Existing methods for dissolving poorly crytalline Fe oxides (primarily ferrihydrite) in soils and mineral mixtures are simple and rapid but often lack selectivity. In this work, we-tested a more selective, alternative ascorbate-based extractant. Ascorbate combined with citrate was found to be highly effective in dissolving poorly crystalline Fe oxides while dissolving little goethite and hematite, Citrate-ascorbate and oxalate extracted similar amounts of Fe from most of the soils and Fe-rich materials studied. However, citrate-ascorbate was more selective than oxalate, since it dissolved only negligible amounts of allophane or imogolite and magnetite, The recommended citrate-ascorbate extraction procedure (0.2 M sodium citrate-0.05 M sodium ascorbate, pH 6, 16 h) is simple to implement and relatively inexpensive, and uses nontoxic chemicals. Thus, it can be used on a routine basis for estimating poorly crystalline Fe oxides in soils. By subtracting citrate-extractable Fe and Al from citrate-ascorbate-extractable Fe and Al values, respectively, one can estimate Fe and Al contained in poorly crystalline Fe oxides. The citrate-ascorbate extraction, combined with others (oxalate, Tiron, hydroxylamine) can help detect and quantify other soil components such as allophane and magnetite.