1 Risø National Laboratory for Sustainable Energy, Technical University of Denmark
Simultaneous determination of N-15 and total N using an automated nitrogen analyser interfaced to a continuous-flow isotope ratio mass spectrometer (ANA-MS method) was evaluated. The coefficient of variation (CV) of repeated analyses of homogeneous standards and samples at natural abundance was lower than 0.1%. The CV of repeated analyses of N-15-labelled plant material and soil samples varied between 0.3% and 1.1%. The reproducibility of repeated total N analyses using the automated method was comparable to results obtained with a semi-micro Kjeldahl procedure. However, the automated method gave results which were 3% to 5% higher than those obtained with the Kjeldahl procedure. Since only small samples can be analysed, careful sample homogenization and fine grinding are very important. Evaluation of a diffusion method for preparing nitrate and ammonium in solution for automated N-15 analysis showed that the recovery of inorganic N in the NH3 trap was lower when the N was diffused from water than from 2 M KCl. The results also indicated that different proportions of the NO3- and the NH4+ in aqueous solution were recovered in the trap after combined diffusion. The method is most suited for diffusing either NO3- or NH4+ alone, but can be used for combined diffusion of the two ions.