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Characterization of Insoluble Carbonaceous Material in Atmospheric Particulates by Pyrolysis/Gas Chromatography/Mass Spectrometry Procedures

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Characterization of Insoluble Carbonaceous Material in Atmospheric Particulates by Pyrolysis/Gas Chromatography/Mass Spectrometry Procedures Characterization of insoluble carbonaceous material in atmospheric particulates by pyrolysis/gas chromatography/mass spectrometry procedures Item Type text; Dissertation-Reproduction (electronic) Authors Kunen, Steven Maxwell Publisher The University of Arizona. Rights Copyright © is held by the author. Digital access to this material is made possible by the University Libraries, University of Arizona. Further transmission, reproduction or presentation (such as public display or performance) of protected items is prohibited except with permission of the author. Download date 27/09/2021 09:17:40 Link to Item http://hdl.handle.net/10150/565415 CHARACTERIZATION OF INSOLUBLE CARBONACEOUS MATERIAL IN ATMOSPHERIC PARTICULATES BY PYROLYSIS/GAS CHROMATOGRAPHY/MASS SPECTROMETRY PROCEDURES by Steven Maxwell Kunen A Dissertation Submitted to the Faculty of the DEPARTMENT OF GEOSCIENCES In Partial Fulfillment of the Requirements For the Degree of DOCTOR OF PHILOSOPHY In the Graduate College THE UNIVERSITY OF ARIZONA 1 9 7 8 THE UNIVERSITY OF ARIZONA GRADUATE COLLEGE I hereby recommend that this dissertation prepared under my direction by Steven Maxwell Kanen_________________________ entitled Characterization of Insoluble Carbonaceous Material in Atmospheric Particulates by Pyrolysis/G as Chromatography/Mass Spectrometry Procedures be accepted as fulfilling the dissertation requirement for the degree of Doctor of Philosophy__________________________________ /6 ///zsy'l '7 7 8 Dissertation Director Date As members of the Final Examination Committee, we certify that we have read this dissertation and agree that it may be presented for final defense. // s /,\77 8 • S k " L \\cr\% Final approval and acceptance of this dissertation is contingent on the candidate's adequate performance and defense thereof at the final oral examination. STATEMENT BY AUTHOR This dissertation has been submitted in partial fulfillment of requirements for an advanced degree at The University of Arizona and is deposited in the University Library to be made available to bor­ rowers under rules of the Library. Brief quotations from this dissertation are allowable without special permission, provided that accurate acknowledgment of source is made. Requests for permission for extended quotation from or re­ production of this manuscript in whole or in part may be granted by the head of the major department or the Dean of the Graduate College when in his judgment the proposed use of the material is in the in­ terests of scholarship. In all other instances, however, permission must be obtained from the author. SIGNED: ACKNOWLEDGMENTS I wish to thank Drs, Austin Long, Michael Burke and Mrs. Judy Modeleski for their guidance and knowledge so generously shared with me during my analyses of atmospheric particulate matter * Dr. Paul Damon and Professor Terah Smiley inspired me in a broader sense to carry out this work. I am grateful to Dr. Millard Seeley and Dr. Edgar J. McCullough for continued enlightenment concerning the "real world" during my stay at The University of Arizona. Special thanks go to Drs. Eric Bandurski, John Zumberge, and Mr. Michael Engel for their invaluable assistance in both the collection of mass speptra and the keeping of Murphy1s Laws to a minimum in rela­ tion to the instrumentation. Drs. Tiche Novakov, Leonard Newman, James Friend, Bruce Appel, James Lodge, and particularly Jarvis Moyers and A. Clyde Hill served as examples to me during my doctoral experience of the kind of atmospheric scientist I aspired to become. Dr. Bartholomew Nagy provided the original suggestions which led to this study. Without our numerous discussions and his tireless efforts on my behalf, this work would not have been possible. The continued teaching, encouragement, and homiletics of Dr. George Claus, Dr. Richard Shorthill, Mr. James Randazzo and especially Mr. Alfred Kunen were essential for the completion of this exercise in understanding. TABLE OF CONTENTS. Page LIST OF ILLUSTRATIONS......... vi LIST OF TABLES .......... ............. ..... viii ABSTRACT ........................... ix 1. INTRODUCTION............. 1 1.1. Atmospheric Particulate Pollutants . ........... 1 1.2. Insoluble Carbonaceous Material in Atmospheric Partiples ........... 3 1.3. Composition of Insoluble Carbonaceous Material ....... ..... ^ 2. • SIGNIFICANCE OF ORGANIC ANALYSIS OF INSOLUBLE CARBONACEOUS MATERIAL .............. 8 2.1. Atmospheric Particulate Formation, Growth and Reactions . .................... 8 2.2. Flame and Combustion Studies . .................. H 2.3. Health Implications of Insoluble Carbonaceous Material ..... .... 13 2.4. Natural Haze, Control Strategies, and Climatic Studies ............... 1^ 2.5. Particulate Pollutant Source Identification ...... 18 2.5.1. Source Determination Methods ......... 18 2.5.2. Trace Element Concentrations and Pattern Recognition Techniques ...... 18 2.5.3. Limitations of Use of Extractable Organic Matter for Source Determination .............. 18 2.6. Rationale and Goals of the Present Investigation ........ .... 21 3. EXPERIMENTAL METHODS .................... 25 3.1. Sample Collection Procedures ............. 25 3.2. Solvent Extraction Procedures ............ 25 3.3. Pyrolysis, Gas Chromatography, Mass Spectrometry ................ 27 3.3.1. Contribution of Methods ........... 27 3.3.2. High Vacuum Pyrolysis/Gas Chromatography/ Mass■Spectrometry (HVB/GC/MS) ...... 86 iv V TABLE OF CONTENTS— Continued Page 3.3.3. Pyrolysis/Gas Chromatography/Mass Spec­ trometry/Data System (P/GC/MS/DS) .... 39 4. RESULTS ........ ..................... 42 4.1. Interpretation of Data ................ 42 4.2. High Vacuum Pyrolysis/Gas Chromatography/ Mass Spectrometry Analyses ............ 44 4.3. Pyrolysis/Gas Chromatography/Mass Spectrometry/Data System Analysis ........ 70 5. DISCUSSION ......................... 74 5.1. Pyrolysis Products of Natural Organic Compounds .................... 74 5.2. Pyrolysis Products of Insoluble Carbonaceous Material .............. 81 5.3. Significance of the Results of This Investigation .................. 93 6 . SUMMARY ........... .. , . 98 REFERENCES ......................... 101 LIST OF ILLUSTRATIONS Figure Page 1. High Vacuum Pyrolysis Unit . ............. 37 2. 600°C Pyrolysis Products of a Blank Glass Fiber Filter, First Run ........ 45 3. 600°G Pyrolysis Products of a Blank Glass Fiber Filter, Second Run ......... 46 4. 600°C Pyrolysis Products of Pre-cleaned Blank Glass Fiber Filter ........... ......... 48 5. 600°C Pyrolysis Products with No Sample (Blank) Procedure .......... 49 6 . 150°C Pyrolysis Products of Tucson Urban Atmospheric Particulates .... ................. 51 7. 300°C Pyrolysis Products of Tucson Urban Atmospheric Particulates ..... .... 52 8. 450°C Pyrolysis Products of Tucson Urban Atmospheric Particulates ......... ....... 54 9. 600°C Pyrolysis Products of Tucson Urban Atmospheric Particulates ‘ . 55 , 10. 150°C Pyrolysis Products of Tucson Residential Atmospheric Particulates .............. 57 11. 300°C Pyrolysis Products of Tucson Residential Atmospheric Particulates ....... ........... 58 12. 450°C Pyrolysis Products of Tucson Residential Atmospheric Particulates ...... ....... ., 59 13. 600oC Pyrolysis Products of Tucson Residential Atmospheric Particulates .............. 50 14. 300°C Pyrolysis Products of Salt Lake City Urban Atmospheric Particulates . ............. 52 vi vii LIST OF ILLUSTRATIONS— Continued Figure Page 15. 450°C Pyrolysis Products of Salt Lake City Urban Atmospheric Particulates, First Run ....... 63 16. 450°C Pyrolysis Products of Salt Lake City Urban Atmospheric Particulates, Second Run ..... 64 17. 300°C Pyrolysis Products of Pennsylvania Resi­ dential Airport Atmospheric Particulates . 66 18. 450°C Pyrolysis Products of Pennsylvania Resi­ dential Airport Atmospheric Particulates ......... 67 19. 300°C Pyrolysis Products of Wyoming Coke Plant Atmospheric Particulates .............. 68 20. 450°C Pyrolysis Products of Wyoming Coke Plant Atmospheric Particulates ....... ....... 69 o 21. 450 C Pyrolysis Products of Indoor Office Atmospheric Particulates .............. ' 71 22. 450°C Pyrolysis Products of Riverside Atmospheric Particulates .................... 72 LIST OF TABLES Table Page 1. Sample Collection Locations and Conditions . 26 2. Representative Pyrolysis Studies 31 3. Pyrolysis/Gas Chromatography Conditions . ......... 41 4. Cyclic Compounds Identified in Auto Exhaust and by HVP/GC/MS of Atmospheric Particulates ........ 86 5. Species Not Previously Found in Ambient Samples ..... 91 viii ABSTRACT Pyrolysis/gas chromatography/mass spectrometric analysis techniques were employed for the identification of the individual components of the insoluble carbonaceous fraction of atmospheric par­ ticulate matter. Samples were collected from seven stations repre­ senting widely different environments„ This first attempt to employ the techniques mentioned for this hitherto undefined polymer-like portion of atmospheric particles resulted in the identification of over 175 compounds. Some of the individual components making up the polymer-like'matter are known toxic substances and/or cocarcinogens. It was shown that this method can be successfully applied towards the clarification of the structure of the insoluble organic matter. This fraction represents the, most stable organic portion of the atmospheric particulates, since it most likely does not undergo chemical changes from the point of origin to its collection and arrival in the lab­ oratory; for this reason it is highly suitable
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