Determination of nitrogen-15 enrichment of nitrate and nitrite using thermospray liquid chromatography-mass spectrometry
A new method has been developed for the determination of percent /sup 15/N enrichment in NO/sub 2//sup -/ and NO/sub 3//sup -/ that is both rapid and sensitive. NO/sub 2//sup -/ and NO/sub 3//sup -/ separation was done by use of reverse-phase liquid chromatography with a mobile phase consisting of ammonium acetate with tetrabutylammonium acetate as the ion pair reagent. The % /sup 15/N in isotopically enriched anions was determined by using thermospray liquid chromatography-mass spectrometry (LC-MS). Enrichment values were obtained on as little as 20 ng of NO/sub 2//sup -/-N/20 ..mu..L and 4 ng of NO/sub 3//sup -/-N/20 ..mu..L. The linear regression curve was plotted for the observed enrichment vs. the actual enrichment over the range from the natural abundance to 25% enrichment for each anion and the equation for the linear regression calculated (y = 1.16x + 0.7577 for NO/sub 2//sup -/ and y = 0.951x + 0.447 for NO/sub 3//sup -/). The coefficient of determination for the NO/sub 2//sup -/ and NO/sub 3//sup -/ curves was 0.988 and 0.987, respectively. The dynamic range of the method was found to be suitable for the range of NO/sub 2//sup -/ and NO/sub 3//sup -/ expected in plant xylem sap. Xylem sap samples obtained from NO/sub 3//sup -/ fed pea, Pisum sativum cv. Homesteader (3.9 ..mu..g of NO/sub 3//sup -/-N/mL, 24.7% /sup 15/N), contained a /sup 15/N enrichment of 25.4% +/- 0.7%.
- Research Organization:
- National Research Council of Canada, Saskatoon, Saskatchewan
- OSTI ID:
- 5109735
- Journal Information:
- Anal. Chem.; (United States), Vol. 58:13
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
NITRATES
LIQUID COLUMN CHROMATOGRAPHY
QUANTITATIVE CHEMICAL ANALYSIS
NITRITES
NITROGEN 15
ISOTOPE RATIO
MASS SPECTROSCOPY
EXPERIMENTAL DATA
SPRAYS
TRACE AMOUNTS
CHEMICAL ANALYSIS
CHROMATOGRAPHY
DATA
INFORMATION
ISOTOPES
LIGHT NUCLEI
NITROGEN COMPOUNDS
NITROGEN ISOTOPES
NUCLEI
NUMERICAL DATA
ODD-EVEN NUCLEI
OXYGEN COMPOUNDS
SEPARATION PROCESSES
SPECTROSCOPY
STABLE ISOTOPES
400102* - Chemical & Spectral Procedures
400105 - Separation Procedures
400104 - Spectral Procedures- (-1987)