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Published in Soil Sci Soc Am J 58:1108-1116 (1994)
© 1994 Soil Science Society of America
677 S. Segoe Rd., Madison, WI 53711 USA
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Determining Nitrogen-15 in Nitrite or Nitrate by Producing Nitrous Oxide

R. J. Stevens* and R. J. Laughlin

Department of Agriculture for Northern Ireland, Food and Agricultural Chemistry Research Division, Newforge Lane, Belfast BT9 5PX, Northern Ireland

*Corresponding author (gacd6023{at}uk.ac.qub.agv1).

ABSTRACT

Determining 15N in NO3 or NO2 is important when studying soil N transformations directly. Analysis of 15N in NO3 by standard methods is time consuming and subject to errors such as cross-contamination. The 15N content of NO2 is determined conventionally as the difference between NO3 + NO2 and NO3 alone. Since NO3 concentrations are usually much greater than NO2 concentrations in soil, determination of 15N in NO2 has a poor detection limit. We developed new direct methods for determining 15N in NO3 or NO2 in 2 M KCl soil extracts, based on the production of N2O from NO2 + NH2OH. For NO2, N2O was produced by adding NH2OH at pH 1.7. For NO3, NO2 and NH2OH were produced as intermediates during the reduction of NO3 by Cd-Cu at pH 4.7. The 15N content of the N2O was determined by automated continuous flow isotope-ratio mass spectrometry. Measured values of 15N in N2O were closely related to the theoretical values for 15N in NO2 or NO3. Five micromoles of NO3 or 0.5 µmol of NO2 at 0.1 atom % excess 15N could be determined with coefficients of variation of <4%. The new methods are fast, simple, and not subject to contamination from the atmosphere or from other samples. They should facilitate studies on the simultaneous measurement of gross rates of mineralization, immobilization, nitrification, and NO3 reduction.

Received for publication July 8, 1993.


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