Distillation and Microdiffusion Modifications for total Nh4f Quantification and 15N Recovery
Gaius D. Eudoxie and Gregory A. Gouveia
DOI : 10.3844/ajabssp.2008.689.698
American Journal of Agricultural and Biological Sciences
Volume 3, Issue 4
Problem statement: Applying 15N techniques to accurately determine the fate of fixed ammonium (NH4f) in the strongly and weakly held pools require modifications to existing methodologies. Modifications are necessary for measurement of total NH4f in soils by direct digestion with 5 M HF: 1 M HCl, excluding alkali pretreatment, followed by distillation and quantification of NH4. Quantification by distillation was used as a precursor to optimize microdiffusion protocols for continuous flow-isotope ratio mass spectrometry (CF-IRMS). This paper reports on the modifications applied to these procedures since the direct 5 M HF: 1 M HCl digestion of soil samples may also dissolve some organic N fractions. Approach: Distillation followed by 15N microdiffusion trials were conducted on soil digests amended with rice husks, manure, compost or glycine, using different molarities (2, 5, and 10 M) and volumes (5, 10, 15, 25, 32.5, and 40 mL) of KOH. Results: The distillation study identified 32.5 mL of 2 M KOH to be the optimum volume and molarity of KOH that must be combined with 10-mL aliquots of direct 5 M HF: 1 M HCl digests of each of seven soils to ensure that only NH4 in the digest is recovered and none of the organic N is hydrolyzed during the process. Results also showed that a minimum incubation time of 192 h was needed to trap approximately 100 µg 15N on the disks for subsequent accurate analysis by CF-IRMS, with minimal recovery of organic N. Conclusions/Recommendations: These findings support the use of a direct-digestion/distillation method to quantify total NH4f and thereby provide opportunity to distinguish between strongly and weakly held NH4f in soils.
© 2008 Gaius D. Eudoxie and Gregory A. Gouveia. This is an open access article distributed under the terms of the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original author and source are credited.