Analysis of dissolved 15N2 gas standards by Membrane Inlet Mass Spectrometry

Website: https://www.bco-dmo.org/dataset/778021
Data Type: experimental
Version: 1
Version Date: 2019-10-02

Project
» EAGER: Collaborative Research: Detection limit in marine nitrogen fixation measurements - Constraints of rates from the mesopelagic ocean (EAGER NitFix)
ContributorsAffiliationRole
Granger, JulieUniversity of Connecticut (UConn)Principal Investigator
Bourbonnais, AnnieUniversity of Massachusetts Dartmouth (UMass Dartmouth)Co-Principal Investigator
Wilson, SamuelUniversity of Hawaii (UH)Co-Principal Investigator
Biddle, MathewWoods Hole Oceanographic Institution (WHOI BCO-DMO)BCO-DMO Data Manager

Abstract
In order to verify that measurements of the 15N2 atom% of dissolved N2 gas samples effectuated by Membrane Inlet Mass Spectrometry are accurate, we developed a specific protocol to prepare dissolved 15N2 gas standards. We detail the protocol herein, and report representative MIMS measurements of the prepared standards.


Dataset Description

Analysis of dissolved 15N2 gas standards by Membrane Inlet Mass Spectrometry


Methods & Sampling

We determined that the most reliable way to prepare dissolved 15N2 gas standards involves equilibration of the liquid phase with a headspace, rather than injection of a 15N2 gas aliquot into a sealed bottle without a headspace. Standards were prepared in a room with a relatively constant ambient temperature. Serial aliquots of 15N2 gas were each injected into the headspace of crimp-sealed 120 mL serum bottles containing 80 mL of air-equilibrated seawater (at room temperature) and a stir bar with an unpressurized air headspace. The vials were equilibrated for 72 hours on a stir plate (at low rpm) prior to analysis on the MIMS or IRMS. 


Data Processing Description

BCO-DMO Processing Notes:
- table was extracted from original spreadsheet.
- added conventional header with dataset name, PI name, version date
- modified parameter names to conform with BCO-DMO naming conventions

 


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Data Files

File
dis_15n2_gas.csv
(Comma Separated Values (.csv), 8.56 KB)
MD5:8e5f605dd89f3b778bc7754c9683daf9
Primary data file for dataset ID 778021

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Related Publications

White, A. E., Granger, J., Selden, C., Gradoville, M. R., Potts, L., Bourbonnais, A., Fulweiler, R. W., Knapp, A. N., Mohr, W., Moisander, P. H., Tobias, C. R., Caffin, M., Wilson, S. T., Benavides, M., Bonnet, S., Mulholland, M. R., & Chang, B. X. (2020). A critical review of the 15N2 tracer method to measure diazotrophic production in pelagic ecosystems. Limnology and Oceanography: Methods, 18(4), 129–147. Portico. https://doi.org/10.1002/lom3.10353
Results

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Parameters

ParameterDescriptionUnits
Bottle_volvolume of the bottle mililiters (mL)
Sampletype of sample unitless
Injection_15N2amount of Injection of 15N2 mililiters (mL)
Expected_15N_At_pcntexpected 15N At % unitless
Time_of_analysistime of analysis in 24 hour format unitless
m_z_28mass-to-charge unitless
m_z_29mass-to-charge unitless
m_z_30mass-to-charge unitless
m_z_32mass-to-charge unitless
m_z_40mass-to-charge unitless
N2_ArN2/Ar ratio unitless
ratio_28_2928/29 ratio unitless
ratio_28_3028/30 ratio unitless
At_15N_pcnt15N At% unitless
At_15N_pcnt_avg15N At% average unitless


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Instruments

Dataset-specific Instrument Name
Isotope Ratio Mass Spectrometer
Generic Instrument Name
Isotope-ratio Mass Spectrometer
Dataset-specific Description
continuous flow Delta V Isotope Ratio Mass Spectrometer (Smith et al. 2015), and continuous flow-GV Isoprime IRMS (Charoenpong et al., 2014)
Generic Instrument Description
The Isotope-ratio Mass Spectrometer is a particular type of mass spectrometer used to measure the relative abundance of isotopes in a given sample (e.g. VG Prism II Isotope Ratio Mass-Spectrometer).

Dataset-specific Instrument Name
Membrane Inlet Mass Spectrometer
Generic Instrument Name
Membrane Inlet Mass Spectrometer
Dataset-specific Description
Membrane Inlet Mass Spectrometer (Bay Instruments)
Generic Instrument Description
Membrane-introduction mass spectrometry (MIMS) is a method of introducing analytes into the mass spectrometer's vacuum chamber via a semipermeable membrane.


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Project Information

EAGER: Collaborative Research: Detection limit in marine nitrogen fixation measurements - Constraints of rates from the mesopelagic ocean (EAGER NitFix)

Coverage: North Atlantic Ocean, Pacific Ocean


NSF Award Abstract:
The availability of nitrogen is required to support the growth and production of organisms living in the surface of our global ocean. This element can be scarce. To alleviate this scarcity, a special class of bacteria and archaea, called nitrogen fixers, can derive the nitrogen needed for growth from nitrogen gas. This project would carefully examine one specific method for measuring nitrogen fixation that has been used recently to suggest the occurrence of small amounts of nitrogen fixation in subsurface ocean waters. If these reports are verified, then a revision of our understanding of the marine nitrogen cycle may be needed. The Ocean Carbon and Biogeochemistry program will be used as a platform to develop community consensus for best practices in nitrogen fixation measurements and detection of diversity, activity, and abundances of the organisms responsible. In addition, a session will be organized in a future national/international conference to communicate with the broader scientific community while developing these best practices.

The goal of this study is to conduct a thorough examination of potential experimental and analytical errors inherent to the 15N2-tracer nitrogen fixation method, in tandem with comprehensive molecular measurements, in mesopelagic ocean waters. Samples will be collected and experimental work conducted on a cruise transect in the North Atlantic Ocean, followed by analytical work in the laboratory. The specific aims of this study are to (1) determine the minimum quantifiable rates of 15N2 fixation based on incubations of mesopelagic waters via characterization of sources of experimental and analytical error, and (2) seek evidence of presence and expression of nitrogen fixation genes via comprehensive molecular approaches on corresponding samples. The range of detectable rates and diazotroph activity from the measurements made in this study will be informative for the understanding of the importance of nitrogen fixation in the oceanic nitrogen budget.



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Funding

Funding SourceAward
NSF Division of Ocean Sciences (NSF OCE)

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