Improving the Accuracy of Diffusion for Inorganic 15N Analyses of Soil Extracts and Water

Sequential diffusion techniques used to speciate inorganic nitrogen-15 (¹⁵N) during soil or water analysis are complicated by incomplete recovery of ammonium (NH₄⁺)-N, introducing error in the subsequent determination of nitrate (NO₃^–)-N. Based on studies to evaluate different strategies for minimizing cross-contamination error in Mason-jar diffusions, a simple cleaning technique was developed that involves an additional 6-h diffusion using 0.6 M boric acid (H₃BO₃) at room temperature following the recovery of NH₄⁺-N. This technique was 60–87% effective for reducing cross-contamination of unlabeled NO₃^–-N by labeled NH₄⁺-N and became more effective for controlling analytical error with decreasing sample volumes, lower NH₄⁺-N enrichment, and larger quantities of NO₃^–-N. When used with the cleaning technique described, sequential diffusions were far superior for ¹⁵N analysis of NO₃^–-N, as compared to the nonsequential approach that involves an isotope dilution calculation after separate diffusions to determine NH₄⁺-N and total mineral N.