4.0 Article Proceedings Paper

A new approach to determining the content and 15N abundance of total dissolved nitrogen in aqueous samples:: TOC analyser-QMS coupling

Journal

ISOTOPES IN ENVIRONMENTAL AND HEALTH STUDIES
Volume 38, Issue 4, Pages 215-225

Publisher

TAYLOR & FRANCIS LTD
DOI: 10.1080/10256010208033267

Keywords

analysis; aqueous samples; continuous flow; nitrogen 15; quadrupole mass spectrometer; TOC analyser; total dissolved nitrogen

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The standard method for determining the N-15 abundance of total dissolved nitrogen (TDN) in aqueous samples (e.g., soil leachate, sewage, urine.) is currently Kjeldahl digestion followed by steam distillation or diffusion to isolate the ammonium, and then N-15 measurement using IRMS. However, this technique is both time-consuming and laborious. One way of overcoming these disadvantages could be to couple a TOC analyser to determine the TDN with a sufficient quadrupole MS to determine the N-15 abundance. The highTOC analyser (Elementar Analysensysteme Hanau, Germany), which catalytically oxidises the sample's total nitrogen with a high, constant yield to nitrogen monoxide (NO), appeared particularly suitable. The quadrupole-MS ESD 100 (InProcess Instruments Bremen, Germany) proved to be a suitable mass spectrometer for the N-15 determination of NO. This combination of instruments was found to provide a workable method in numerous measurements of standard and actual samples. The detection limit concerning the N amount required per analysis is 2 mug, corresponding to an N concentration of 0.7 mg/l in a maximum sample volume of 3 ml Depending on the N concentration, N-15 abundances starting from 0.5 at.% can be measured with the required precision of better than 3% (simple standard deviation). For example, measuring the abundance of 0.5 at.% requires about 50 mug N, whereas for 1 at.% or more only about 5 mug N is needed per analysis.

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