Improved diffusion methods for determination of inorganic nitrogen in soil extracts and water

Abstract

Diffusion methods previously developed for inorganic-N analysis of soil extracts were modified to improve reliability, increase the dynamic range, extend the scope of applications, and simplify the processing of samples for N-isotope analysis. In these methods, the soil extract is treated with MgO, or MgO plus Devarda‘s alloy, in a 473-ml (1-pint) wide-mouth Mason jar to convert NH₄ ⁺-N, NO₃ ^–-N, and/or NO₂ ^–-N to NH₃-N. The NH₃ thereby liberated is collected in H₃BO₃-indicator solution in a Petri dish suspended from the Mason-jar lid and determined quantitatively by acidimetric titration. With the modifications described, analyses can be performed on 10- to 100-ml samples of water, 0.5MK₂SO₄, 1MKCl, 2MKCl, or 4MKCl, at temperatures between 20 and 30°C. Recovery from 10 or 20ml was quantitative in 18–80h with up to 4mgN; recovery from 50 or 100ml was quantitative in 3–13 days with up to 2mgN. Removal of H₃BO₃ for N-isotope analysis by the Rittenberg process was effected using methanol. Mason-jar diffusion methods are much simpler and more convenient than conventional steam distillations. Comparative studies showed that quantitative determinations are more accurate and precise by diffusion than by distillation.