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Nitrous Oxide (N2O) Isotopic Composition in the Troposphere: Instrumentation, Observations at Mace Head, Ireland, and Regional Modeling

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Nitrous Oxide (N2O) Isotopic Composition in the Troposphere: Instrumentation, Observations at Mace Head, Ireland, and Regional Modeling Nitrous oxide (N2O) isotopic composition in the troposphere: instrumentation, observations at Mace Head, Ireland, and regional modeling by Katherine Ellison Potter B.S. Chemistry & Environmental Science College of William and Mary, 2004 SUBMITTED TO THE DEPARTMENT OF EARTH, ATMOSPHERIC, AND PLANETARY SCIENCES IN PARTIAL FULFULLMENT OF THE REQUIREMENTS FOR THE DEGREE OF DOCTOR OF PHILOSOPHY IN CLIMATE PHYSICS AND CHEMISTRY AT THE MASSACHUSETTS INSTITUTE OF TECHNOLOGY SEPTEMBER 2011 © 2011 Massachusetts Institute of Technology. All rights reserved. Signature of Author: _____________________________________________________________ Department of Earth, Atmospheric, and Planetary Sciences 19 August 2011 Certified by: ___________________________________________________________________ Ronald G. Prinn TEPCO Professor of Atmospheric Chemistry Thesis Supervisor Certified by: ___________________________________________________________________ Shuhei Ono Assistant Professor Thesis Co-Supervisor Accepted by: ___________________________________________________________________ Maria T. Zuber E.A. Griswold Professor of Geophysics and Planetary Science Department Head 2 Nitrous oxide (N2O) isotopic composition in the troposphere: instrumentation, observations at Mace Head, Ireland, and regional modeling by Katherine Ellison Potter Submitted to the Department of Earth, Atmospheric, and Planetary Sciences on 19 August 2011 in partial fulfillment of the requirements for the degree of Doctor of Philosophy in Climate Physics and Chemistry Abstract Nitrous oxide (N2O) is a significant greenhouse gas and main contributor to stratospheric ozone destruction. Surface measurements of N2O mole fractions have been used to attribute source and sink strengths, but large uncertainties remain. Stable isotopic ratios of N2O (here considered 14N15N16O, 15N14N16O, 14N14N18O, relative to the abundant 14N14N16O) linked to source and sink isotopic signatures can provide additional constraints on emissions and counter-balancing stratospheric sink. However, the isotopic composition in the troposphere has been regarded and measured as a fixed value, limited by insufficient measurement precision and few data. This thesis provides the foundation for high-frequency, high-precision measurements and utilization of N2O tropospheric isotopic composition. This is achieved through the development of a new measuring capability with sufficient precision to detect the subtle signals of N2O isotopic composition in tropospheric air and uniquely fully-automated and high-frequency capable. This instrument was applied to produce the first set of tropospheric air observations gathered at a remote research station covering a full annual cycle, paired with air origin information, and providing a valuable assessment of tropospheric composition and its potential utility. The first regional model of tropospheric N2O isotopic composition was developed for further assessment of expected variability and utility of isotopic composition data. The optimized fully-automated, liquid-cryogen-free pre-concentration device coupled to continuous flow IRMS resulted in 15N site-specific precisions markedly improved over other systems of 0.11 and 0.14‰ (1σ) for δ15Nα and δ15Nβ, respectively, and among the best bulk composition precisions of 0.05 and 0.10‰ for δ15Nbulk and δ18O, respectively. The high-precision, non-continuous 15 flask observations of N2O N site-specific composition (January 2010 to January 2011; Mace Head Atmospheric Research Station, Ireland) detected statistically significant signals on short-term and annual timescales, and when analyzed with air history information showed consistencies with source-receptor relationships. No seasonal cycle could be detected in the low-frequency observations, but regional model scenarios of the stratospheric seasonal signal resulted in amplitudes at the cusp of current measurement capabilities. This thesis illustrated detectable variations in tropospheric N2O isotopic composition which can potentially reduce uncertainty in the N2O budget with high-frequency, high-precision observations, now feasible by the instrumentation developed here. Thesis Supervisor: Ronald G. Prinn Title: TEPCO Professor of Atmospheric Chemistry Thesis Co-Supervisor: Shuhei Ono Title: Assistant Professor 3 Acknowledgments Ron Prinn and Shuhei Ono have supervised my work with equally valuable and perfectly distinct contributions, and cannot begin to enumerate their assets to me. I have been blessed to have them both at my back. Eric Davidson and Peter Simmonds on my committee provided a marvelous amount of constant inspiration for me as a scientist; through initial nitrogen cycle ignition in Brazil many years ago, to continual ideas and new approaches, to images of ideal scientist models and experience to crave. The instrumentation work in this thesis began with the dedication and invaluable tutoring of Brian Greally, who jumpstarted Stheno into being. Simon O’Doherty generously made this entire thesis feasible with the welcome at the University of Bristol and munificent lending of Stheno’s structure. Gerry Spain at the Mace Head Atmospheric Research Station was beyond air-sample- collector and provided me with valuable measurement knowledge, experience, insights, and confidence. My instrumentation support team including Ben Miller, Jens Mühle, Peter Salameh, Ray Weiss, and Dickon Young never failed to provide on-call instrument support and replies to many many emails regarding instrument failures, breakdowns, and other bits bringing frustration and love of experimental work. Bill Olszewski on-site never failed to serve as an incredible source of knowledge regarding anything lab equipment. Alistair Manning provided the priceless NAME air history estimates for each of my observations, without which this data might be interpreted as simply noise. Matt Rigby deserves thanks for the numerous discussions, insights, and pursuits regarding modeling of N2O isotopes which educated this experimentalist in the ways of modelers. I am honored to have the enduring collaboration and friendship of Naohiro Yoshida and Sakae Toyoda, and am thankful for the opportunity to work alongside them at the Tokyo Institute of Technology, in the past and in the future, to further isotopomer research. Additionally, outside of the science realm for keeping me going day-to-day, thanks to Mary Ellen Rhinehart and Erika Johnson for the maintenance and attention, and Mary Elliff for smiles, tokens, and friendship, and always leaving me higher and more hopeful than before. 4 Contents Chapter 1: Introduction and thesis overview...................................................... 7 1.1 Background........................................................................................................................................7 1.2 Research goals and approach.....................................................................................................14 Chapter 1 References...........................................................................................................................17 Chapter 2: Isotopic analysis of N2O................................................................. 25 Part I. Optimized fully automated pre-concentration system for the isotopic analyses of tropospheric nitrous oxide by continuous flow isotope ratio mass spectrometry .................26 Introduction...........................................................................................................................................26 2.1 Stheno+CF-IRMS pre-concentration system........................................................................28 2.2 Stheno optimization and special measures............................................................................36 2.3 Performance....................................................................................................................................43 Conclusion .............................................................................................................................................47 Part II. Isotope ratio mass spectrometry of nitrous oxide..........................................................49 2.4 Isotope ratio mass spectrometry of N2O ................................................................................49 2.5 IRMS set-up and optimization..................................................................................................51 2.6 Standards .........................................................................................................................................53 2.7 Continuous flow analysis and optimization ..........................................................................55 2.8 Precision...........................................................................................................................................58 15 Part III. Nitrous oxide (N2O) isotopomer calibration by the N site-specific synthesis of N2O from ammonium nitrate (NH4NO3)..........................................................................................61 2.9 N2O isotopomer calibration .......................................................................................................61 2.10 Methods.........................................................................................................................................63 2.11 Results & Discussion..................................................................................................................65
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