Abstract

Iron (Fe) redox cycling and sorption/complexation reactions influence numerous soil biogeochemical processes, and the precise, rapid, and low-cost determination of reactive Fe pools is critical for understanding these dynamics. Colorimetric methods areoften used to measure Fe,yet assay conditions vary widely among studies, and the robustness of these methods and their potential interferences remain poorly characterized. Here, we developed optimized ferrozine methods (modified from water and sediment protocols) to determine Fe concentrations in three common soil extractions: reduced (Fe(II)) and oxidized Fe (Fe(III)) in 0.5 M HCl (FeHCl), and Fe extracted by citrate-ascorbate (Feca) and citrate-dithionite (Fecd). These methods were adapted for 96-well microplates by employing increased buffer concentrations and longer incubation times relative to published cuvette methods. Iron quantitation was sensitive to the final pH of the reaction mixture and duration of incubationperiod,factorsthathavevariedwidelyinpreviousstudies. Weobtainedconsistent resultswithanassay pH near 7, half hour incubations for FeHCl, and 1 h incubations for Feca and Fecd. These ferrozine methods compared favorably with inductively coupled plasma optical emission spectrometry (ICP-OES) across a broad range of soils, including Oxisols, Mollisols, and Inceptisols with as much as 18% organic C. Iron determination in HCl extractions from 158 tropical forest soil samples with widely varying C content was not influenced by dissolved organic carbon (DOC) or phenolics at lower Fe concentrations (< 2.5 mg g−1 soil), and showed only minor effects (< 6% overestimation) at higher Fe concentrations. This was likely due to co-variation between Fe and DOC, which measured as high as 691 mgC L−1 in a cloud forest soil extract. These microplate-based ferrozine methods can be applied to quantify several reactive soil Fe phases with high precision and throughput, minimal interference, and low cost relative to ICP-OES.

Citation

Huang, W., Hall S.J. (2017): Optimized high-throughput methods for quantifying iron biogeochemical dynamics in soil. Geoderma. DOI: 10.1016/j.geoderma.2017.07.013

This Paper/Book acknowledges NSF CZO grant support.