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Determination of ??18O and ??15N in Nitrate

Analytical Chemistry

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Abstract

The analyses of both O and N isotopic compositions of nitrate have many potential applications in studies of nitrate sources and reactions in hydrology, oceanography, and atmospheric chemistry, but simple and precise methods for these analyses have yet to be developed. Testing of a new method involving reaction of potassium nitrate with catalyzed graphite (C + Pd + Au) at 520 ??C resulted in quantitative recovery of N and O from nitrate as free CO2, K2CO3, and N2. The ??18O values of nitrate reference materials were obtained by analyzing both the CO2 and K2CO3 from catalyzed graphite combustion. Provisional values of ??18OVSMOW for the internationally distributed KNO3 reference materials IAEA-N3 and USGS-32 were both equal to +22.7 ???? 0.5???. Because the fraction of free CO2 and the isotopic fractionation factor between CO2 and K2CO3 were constant in the combustion products, the ??18O value of KNO3 could be calculated from measurements of the ??18O of free CO2. Thus, ??18KNO3 = a??18OfreeCO2 - b, where a and b were equal to 0.9967 and 3.3, respectively, for the specific conditions of the experiments. The catalyzed graphite combustion method can be used to determine ??18O of KNO3 from measurements of ??18O of free CO2 with reproducibility on the order of ??0.2??? or better if local reference materials are prepared and analyzed with the samples. Reproducibility of ??15N was ??0.1??? after trace amounts of CO were removed.

Additional Publication Details

Publication type:
Article
Publication Subtype:
Journal Article
Title:
Determination of ??18O and ??15N in Nitrate
Series title:
Analytical Chemistry
Volume
69
Issue:
21
Year Published:
1997
Language:
English
Larger Work Type:
Article
Larger Work Subtype:
Journal Article
Larger Work Title:
Analytical Chemistry
First page:
4375
Last page:
4380
Number of Pages:
6