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Determination of the δ15N of total nitrogen in solids; RSIL lab code 2893

Techniques and Methods 10-C11

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Abstract

The purpose of the Reston Stable Isotope Laboratory (RSIL) lab code 2893 is to determine the δ(15N/14N), abbreviated as δ15N , of total nitrogen in solid samples. A Carlo Erba NC 2500 elemental analyzer (EA) is used to convert total nitrogen in a solid sample into N2 gas. The EA is connected to a continuous flow isotope-ratio mass spectrometer (CF-IRMS), which determines relative difference in the isotope-amount ratios of stable nitrogen isotopes (15N/14N)of the product N2 gas. The combustion is quantitative; no isotopic fractionation is involved. Samples are placed in a tin capsule and loaded into the Costech Zero Blank Autosampler of the EA. Under computer control, samples are dropped into a heated reaction tube that contains an oxidant, where the combustion takes place in a helium atmosphere containing an excess of oxygen gas. Combustion products are transported by a helium carrier through a reduction tube to remove excess oxygen and convert all nitrous oxides into N2 and through a drying tube to remove water. The gas-phase products, mainly CO2 and N2, are separated by a gas chromatograph. The gas is then introduced into the isotope-ratio mass spectrometer (IRMS) through a Finnigan MAT (now Thermo Scientific) ConFlo II interface, which also is used to inject N2 reference gas and helium for sample dilution. The IRMS is a Thermo Scientific Delta V Plus CF-IRMS. It has a universal triple collector, two wide cups with a narrow cup in the middle, capable of measuring mass/charge (m/z) 28, 29, 30, simultaneously. The ion beams from N2 are as follows: m/z 28 = N2 = 14N14N; m/z 29 = N2 = 14N15N primarily; m/z 30 = NO = 14N16O primarily, which is a sign of contamination or incomplete reduction.

Additional Publication Details

Publication type:
Report
Publication Subtype:
USGS Numbered Series
Title:
Determination of the δ15N of total nitrogen in solids; RSIL lab code 2893
Series title:
Techniques and Methods
Series number:
10-C11
Edition:
Version 1.0 - 2006, Version 1.1 - 2007, Version 1.2 - September 2012
Year Published:
2006
Language:
English
Publisher:
U.S. Geological Survey
Publisher location:
Reston, VA
Contributing office(s):
Reston Stable Isotope Laboratory
Description:
viii, 30 p.
Larger Work Type:
Report
Larger Work Subtype:
USGS Numbered Series
Larger Work Title:
Chapter 11 of Book 10, Methods of the Reston Stable Isotope Laboratory, Section C, Stable Isotope-Ratio Methods
Number of Pages:
40
Online Only (Y/N):
Y