A new method for collection of nitrate from fresh water and the analysis of nitrogen and oxygen isotope ratios

Journal of Hydrology
By: , and 

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Abstract

A new method for concentrating nitrate from fresh waters for δ15N and δ18O analysis has been developed and field-tested for four years. The benefits of the method are: (1) elimination of the need to transport large volumes of water to the laboratory for processing; (2) elimination of the need for hazardous preservatives; and (3) the ability to concentrate nitrate from fresh waters. Nitrate is collected by, passing the water-sample through pre-filled, disposable, anion exchanging resin columns in the field. The columns are subsequently transported to the laboratory where the nitrate is extracted, converted to AgNO3 and analyzed for its isotope composition. Nitrate is eluted from the anion exchange columns with 15 ml of 3 M HCl. The nitrate-bearing acid eluant is neutralized with Ag2O, filtered to remove the AgCl precipitate, then freeze-dried to obtain solid AgNO3, which is then combusted to N2 in sealed quartz tubes for δ15N analysis. For δ18O analysis, aliquots of the neutralized eluant are processed further to remove non-nitrate oxygen-bearing anions and dissolved organic matter. Barium chloride is added to precipitate sulfate and phosphate; the solution is then filtered, passed through a cation exchange column to remove excess Ba2+, re-neutralized with Ag2O, filtered, agitated with activated carbon to remove dissolved organic matter and freeze-dried. The resulting AgNO3 is combusted with graphite in a closed tube to produce CO2, which is cryogenically purified and analyzed for its oxygen isotope composition. The 1σanalytical precisions for δ15N and δ18O are ±0.05‰ and ±0.5‰, respectively, for solutions of KNO3 standard processed through the entire column procedure.

Publication type Article
Publication Subtype Journal Article
Title A new method for collection of nitrate from fresh water and the analysis of nitrogen and oxygen isotope ratios
Series title Journal of Hydrology
DOI 10.1016/S0022-1694(99)00205-X
Volume 228
Issue 1-2
Year Published 2000
Language English
Publisher Elsevier
Contributing office(s) Toxic Substances Hydrology Program
Description 15 p.
First page 22
Last page 36
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