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Citric acid traps to replace sulphuric acid in the ammonia diffusion of dilute water samples for 15N analysis



The analysis of 15N in aqueous samples requires the concentration of dissolved nitrogen (N) into a small volume that can be analysed by mass spectrometry. This is conveniently achieved by the NH3 diffusion technique, where NHmath image is captured on small acidified filters enclosed in PTFE. NOmath image can be analysed the same way by reducing it to NHmath image with Devarda's alloy. H2SO4 is commonly used for the acidification of the filters. During combustion, however, this acid leads to the production of SO2 and elemental sulphur, which both have detrimental effects on the mass spectrometer. We propose here to replace H2SO4 with citric acid because it is combusted completely to CO2 and H2O in the elemental analyser before entering the mass spectrometer. Citric acid was found to give comparable results in terms of N recovery and 15N values, both for NHmath image and for NOmath image samples. Blank samples revealed that N contamination was slightly lower using citric instead of sulphuric acid as acidifier of the glass filters. NHmath image samples first concentrated over cation-exchange columns were strongly acidic and several methods were tested to raise the pH for the subsequent diffusion. These samples gave incomplete N recoveries, but this problem was independent of the acid used on the filters and of the final pH of the sample. Complete recovery was achieved only by increasing the volume of the eluate from the columns. Citric acid can thus generally be recommended instead of H2SO4 for ammonia diffusion. Copyright © 2006 John Wiley & Sons, Ltd.

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