Use of Diffusion to Determine Inorganic Nitrogen in a Complex Organic Matrix
- R. L. Mulvaney and
- S. A. Khan
Serious interference can arise in carrying out quantitative or isotopic analyses of inorganic N in samples having a high content of labile organic N. Studies to evaluate existing Mason jar diffusion methods for interference by a high concentration of various amino acids and amino sugars showed the need to minimize the diffusion period. This was accomplished by increasing the volume of H3BO3-indicator solution (to 7 mL), and by carrying out diffusions from a fixed volume (10 mL) with a high salt concentration (4 M KCl). Quantitative recovery (≥98%) of 4 mg of NH4-N was achieved in the presence of 10 mg of organic N, either in 18 h at 25°C, or in 1.5 h by heating on a hot plate at 45 to 50°C. Under the same conditions, complete recovery of NO3-N and NO2-N was achieved in the presence of 4 mg of organic N by increasing the amount of Devarda's alloy from 0.3 to 1.5 g. The modified diffusion methods were much more accurate and precise than conventional steam distillation techniques for inorganic N analysis of animal waste or other complex samples treated with labeled NH4-N, NO3-N, or NO2-N. Recovery of the labeled N by diffusion ranged from 96 to 107%, and the coefficient of variation was usually <2%. The isotopic analyses from these diffusions were usually accurate to within 4%, as determined by isotope-dilution calculations. The latter finding provides ample evidence that no interference arises from labile organic N.Please view the pdf by using the Full Text (PDF) link under 'View' to the left.
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