Separating Soil Iron‐ and Manganese‐Oxide Fractions for Microelement Analysis

Abstract

Since sodium dithionite (Na2S2O4) is often contaminated with zinc (Zn) and can form metal sulfide precipitates, it is not suitable for solubilizing iron (Fe) oxides in fractionation schemes for soil microelements. The objective was to find an alternate method to solubilize crystalline Fe oxides that would fit into a scheme including extractants for amorphous Fe and manganese (Mn) oxides. Three soils were extracted with seven reagents designed to remove amorphous and/or crystalline Fe or Mn oxides [0.1M Na4P2O7, pH 10.0; 0.2M (NH4)2C2O4 in 0.2M H2C2O4, pH 3.0 (oxalate); 0.1M NH2OH‐HCl, pH 2.0; 1.0M NH2OH‐HCl in 25% acetic acid; 0.1M ascorbic acid in the oxalate solution; 0.1 g SnCl2 per gram of soil in the oxalate solution; and 1.0 g dithionite per gram of soil in citrate buffer]. The Na4P2O7, an extractant for elements associated with the organic fraction, extracted amounts of Fe similar to that for the oxalate solution. The two NH2OH‐HCl extractants solubilized very little Fe (<1% total), but NH2OH‐HCl alone solubilized as much Mn as most of the other extractants indicating that it is specific for Mn oxides. The ascorbic acid‐oxalate and SnCl2‐oxalate experimental methods extracted amounts of Fe similar to the dithionite method and amounts of Al higher than the dithionite method. Of the amorphous Fe‐oxide extractants, the oxalate solution solubilized the most Zn and Cu, whereas of the crystalline Fe‐oxide extractants, the ascorbic acid‐oxalate solubilized the highest amounts of Zn and Cu. The extractants suggested for a fractionation scheme are NH2OH‐HCl for Mn oxides, oxalate solution shaken with the soil in the dark for amorphous Fe oxides, and ascorbic acid‐oxalate for crystalline Fe oxides.

Effect of earthworms (Eisenia fetida) on the fractionation and bioavailability of rare earth elements in nine Chinese soils

“…Amorphous iron (Fe) and aluminum (Al) oxides were determined by ammonium oxalate extraction method (Blakemore et al, 1987), and crystalline Fe and Al oxides by the oxalate-ascorbic acid extraction method of Shuman (1982). Manganese oxide content was determined by extraction with 0.1 mol l À1 of hydroxyl-ammonium hydrochloride (Shuman, 1982).…”

Effects of low-molecular-weight organic acids and residence time on desorption of Cu, Cd, and Pb from soils

“…Amorphous iron (Fe) and aluminum (Al) oxides were determined by ammonium oxalate extraction (McKeague and Day, 1966). Crystalline Fe and Al oxides were determined by the oxalate-ascorbic acid extraction method of Shuman (1982). Manganese oxide content was determined by extraction with 0.1 mol l À1 of hydroxyl-ammonium hydrochloride (Shuman, 1982).…”

“…Crystalline Fe and Al oxides were determined by the oxalate-ascorbic acid extraction method of Shuman (1982). Manganese oxide content was determined by extraction with 0.1 mol l À1 of hydroxyl-ammonium hydrochloride (Shuman, 1982). Specific surface areas were obtained via Brunauner-Emmett-Teller (BET)-N 2 adsorption method (Brunauer et al, 1938).…”

Effect of organic acids on adsorption and desorption of rare earth elements

“…Amorphous iron (Fe) and aluminum (Al) oxides were determined by ammonium oxalate extraction (McKeague and Day, 1966). Crystalline Fe and Al oxides were determined by the oxalateascorbic acid extraction method of Shuman (1982). These properties of the soils are given in Table 1.…”