Membrane inlet mass spectrometry method (REOX/MIMS) to measure 15N-nitrate in isotope-enrichment experiments

Using 15N stable isotope as a tracer to quantify N transformation rates in isotope-enrichment experiments improves understanding of the N cycle in various ecosystems. However, measuring 15N-nitrate (15NO3−) in small volumes of water for these experiments is a major challenge due to the inconvenience...

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Autores principales: Xianbiao Lin, Kaijun Lu, Amber K. Hardison, Zhanfei Liu, Xin Xu, Dengzhou Gao, Jun Gong, Wayne S. Gardner
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Publicado: Elsevier 2021
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Acceso en línea:https://doaj.org/article/b563f395770146ff884966fb2f5cc8e0
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spelling oai:doaj.org-article:b563f395770146ff884966fb2f5cc8e02021-12-01T04:50:10ZMembrane inlet mass spectrometry method (REOX/MIMS) to measure 15N-nitrate in isotope-enrichment experiments1470-160X10.1016/j.ecolind.2021.107639https://doaj.org/article/b563f395770146ff884966fb2f5cc8e02021-07-01T00:00:00Zhttp://www.sciencedirect.com/science/article/pii/S1470160X21003046https://doaj.org/toc/1470-160XUsing 15N stable isotope as a tracer to quantify N transformation rates in isotope-enrichment experiments improves understanding of the N cycle in various ecosystems. However, measuring 15N-nitrate (15NO3−) in small volumes of water for these experiments is a major challenge due to the inconvenience of preparing samples by traditional techniques. We developed a “REOX/MIMS” method by applying membrane inlet mass spectrometry (MIMS) to determining 15NO3− concentrations in a small volumes of water from isotope-enrichment experiments after converting the dissolved inorganic N to N2. The nitrates (NO3− + NO2−) were reduced to NH4+ with zinc powder, and the ammonium (NH4+) was then oxidized to N2 by hypobromite iodine solution. The resulting 29N2 and 30N2 were measured via MIMS. This optimized protocol provides a sensitive (~0.1 μM) and precise (relative standard deviation = 0.1–4.37%) approach to quantify 15NO3− concentrations (0.1–500 µM) in water samples over a wide range of salinities (0–35‰) and in 2 M KCl solution with excellent calibration curves (R2 ≥ 0.9996, p < 0.0001). The method was combined with 15NO3− isotope-enrichment incubation experiments to measure gross nitrification and gross NO3− immobilization rates in various ecosystems. It was rapid, accurate, and cost-effective. Future applications of this efficient approach will inform scientists, modelers and decision makers about mechanisms, sources, fates, and effects of NO3− delivered to or produced in numerous aquatic and terrestrial ecosystems.Xianbiao LinKaijun LuAmber K. HardisonZhanfei LiuXin XuDengzhou GaoJun GongWayne S. GardnerElsevierarticleREOX/MIMS15NO3−Gross nitrificationGross NO3− immobilizationIsotope dilution methodEcologyQH540-549.5ENEcological Indicators, Vol 126, Iss , Pp 107639- (2021)
institution DOAJ
collection DOAJ
language EN
topic REOX/MIMS
15NO3−
Gross nitrification
Gross NO3− immobilization
Isotope dilution method
Ecology
QH540-549.5
spellingShingle REOX/MIMS
15NO3−
Gross nitrification
Gross NO3− immobilization
Isotope dilution method
Ecology
QH540-549.5
Xianbiao Lin
Kaijun Lu
Amber K. Hardison
Zhanfei Liu
Xin Xu
Dengzhou Gao
Jun Gong
Wayne S. Gardner
Membrane inlet mass spectrometry method (REOX/MIMS) to measure 15N-nitrate in isotope-enrichment experiments
description Using 15N stable isotope as a tracer to quantify N transformation rates in isotope-enrichment experiments improves understanding of the N cycle in various ecosystems. However, measuring 15N-nitrate (15NO3−) in small volumes of water for these experiments is a major challenge due to the inconvenience of preparing samples by traditional techniques. We developed a “REOX/MIMS” method by applying membrane inlet mass spectrometry (MIMS) to determining 15NO3− concentrations in a small volumes of water from isotope-enrichment experiments after converting the dissolved inorganic N to N2. The nitrates (NO3− + NO2−) were reduced to NH4+ with zinc powder, and the ammonium (NH4+) was then oxidized to N2 by hypobromite iodine solution. The resulting 29N2 and 30N2 were measured via MIMS. This optimized protocol provides a sensitive (~0.1 μM) and precise (relative standard deviation = 0.1–4.37%) approach to quantify 15NO3− concentrations (0.1–500 µM) in water samples over a wide range of salinities (0–35‰) and in 2 M KCl solution with excellent calibration curves (R2 ≥ 0.9996, p < 0.0001). The method was combined with 15NO3− isotope-enrichment incubation experiments to measure gross nitrification and gross NO3− immobilization rates in various ecosystems. It was rapid, accurate, and cost-effective. Future applications of this efficient approach will inform scientists, modelers and decision makers about mechanisms, sources, fates, and effects of NO3− delivered to or produced in numerous aquatic and terrestrial ecosystems.
format article
author Xianbiao Lin
Kaijun Lu
Amber K. Hardison
Zhanfei Liu
Xin Xu
Dengzhou Gao
Jun Gong
Wayne S. Gardner
author_facet Xianbiao Lin
Kaijun Lu
Amber K. Hardison
Zhanfei Liu
Xin Xu
Dengzhou Gao
Jun Gong
Wayne S. Gardner
author_sort Xianbiao Lin
title Membrane inlet mass spectrometry method (REOX/MIMS) to measure 15N-nitrate in isotope-enrichment experiments
title_short Membrane inlet mass spectrometry method (REOX/MIMS) to measure 15N-nitrate in isotope-enrichment experiments
title_full Membrane inlet mass spectrometry method (REOX/MIMS) to measure 15N-nitrate in isotope-enrichment experiments
title_fullStr Membrane inlet mass spectrometry method (REOX/MIMS) to measure 15N-nitrate in isotope-enrichment experiments
title_full_unstemmed Membrane inlet mass spectrometry method (REOX/MIMS) to measure 15N-nitrate in isotope-enrichment experiments
title_sort membrane inlet mass spectrometry method (reox/mims) to measure 15n-nitrate in isotope-enrichment experiments
publisher Elsevier
publishDate 2021
url https://doaj.org/article/b563f395770146ff884966fb2f5cc8e0
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