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Title The identification and quantitation of complex polycyclic aromatic hydrocarbon mixtures in environmental samples using comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry
Publication Date
Date Available
Date Accessioned
Degree PhD
Discipline/Department Chemistry
Degree Level doctoral
University/Publisher Oregon State University
Abstract Polycyclic aromatic hydrocarbons (PAHs) are ubiquitous contaminants and are mostly products of the incomplete combustion of organic material. PAHs are often found in environmental samples as a complex mixture of isomers. In addition, the same sources that produce complex PAH mixtures also produce other poorly characterized mixtures of organic compounds, commonly referred to as an unresolved complex mixture (UCM), that act as matrix interferences in the chromatographic analysis of samples. Conventional one-dimensional chromatographic techniques, such as gas chromatography coupled to mass spectrometry (GC/MS), are not sufficient for the analysis and quantitation of complex PAH mixtures present in environmental samples due to the high degree of overlap in compound vapor pressures, boiling points, and mass spectral fragmentation patterns. Therefore, the separation and quantitation of complex mixtures of individual PAH compounds in environmental samples requires high chromatographic resolution. Comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC×GC/ToF-MS) was used for this study. GC×GC/ToF-MS uses two different gas chromatographic columns, with different separation mechanisms, for the analysis of complex environmental samples. In theory, the peak capacity in GC×GC/ToF-MS is equivalent to the product of the individual peak capacities of each column used. However, in practice, this is rarely obtained because of the existing correlation between the two GC columns used. This dissertation is a compilation of three studies related to analytical method development for the identification and quantitation of complex PAH mixtures (including parent-PAHs, alkyl-PAHs, oxy-PAHs, nitro-PAHs, thio-PAHs, chloro-PAHs, bromo-PAHs and PAHs with molecular weight higher than 300 Da) that may be present in environmental samples using novel column combinations in GC×GC/ToF-MS. The use of a liquid crystal column (LC-50) in the first dimension, followed by a nano-stationary phase column (NSP-35) in the second dimension, was evaluated for the separation of a standard PAH mixture containing 97 different PAHs. Two standard reference materials purchased from NIST (NIST SRM1650b – Diesel Particulate Matter and NIST SRM1975 – Diesel Extract) were used, after extraction and cleanup, for method validation and comparison between the commonly used non-polar × polar column combination and the LC-50 × NSP-35 column combination with high orthogonality. As part of the method validation, an aliquot of NIST SRM1975 (Diesel extract), without sample cleanup was also analyzed for PAHs, showing that the LC-50 × NSP-35 column combination was accurate (with an average absolute percent difference of approximately 30%) for the identification and quantitation of complex PAH mixtures in environmental samples, with reduced sample preparation prior to analysis. In addition, the LC-50 × NSP-35 column combination was used for the analysis of PAHs sorbed to polystyrene pellets deployed in an urban bay area as passive water…
Subjects/Keywords PAHs; Polycyclic aromatic hydrocarbons
Contributors Simonich, Staci L. (advisor); Field, Jennifer (committee member)
Language en
Country of Publication us
Record ID handle:1957/35901
Repository oregonstate
Date Indexed 2017-03-17
Grantor Oregon State University
Issued Date 2012-12-14 00:00:00
Note [] Graduation date: 2013; [] Access restricted to the OSU Community at author's request from Dec. 27, 2012 - June 27, 2013; [peerreview] no; [embargopolicy] OSU Users;

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…ACKNOWLEDGEMENTS I would like to express sincere thanks to my major professor, Dr. Staci Simonich at Oregon State University and Dr. Eunha Hoh at San Diego State University, for their constant guidance and support during the entire research and…

…learning process. I would also like to recognize all the graduate committee members: Dr. Fred Prahl, Dr. Vince Remcho, Dr. Kim Anderson and Dr. Jennifer Field, for their assistance during my graduate career at Oregon State University. My fellow laboratory…

…thanks to all my friends from the Association of Latin American Students (ALAS) at Oregon State University, where I learned the most important lessons throughout this four years: friendship, support, solidarity and sense of community. Finally, I…

…would like to thank my family for all of their support and love, probably the most important things any person needs. CONTRIBUTION OF AUTHORS For all the following studies, Dr. Staci Massey Simonich from Oregon State University and Dr. Eunha Hoh from…

…the Graduate School of Public Health at San Diego State University. (Chapter 2, 3, 4) Jill Schrlau from the Environmental and Molecular Toxicology Department at Oregon State University assisted in the pressurized liquid extraction and solid…

…Combinations in GCGC/ToF-MS Carlos Manzano1, Eunha Hoh2 and Staci L. Massey Simonich1,3,* 1 Department of Chemistry, Oregon State University, Corvallis, Oregon 2 Graduate School of Public Health, San Diego State University, San Diego, California 3…

…Department of Environmental and Molecular Toxicology, Oregon State University, Corvallis, Oregon Environ. Sci. Technol., 2012, 46 (14), pp 7677–7684 DOI: 10.1021/es301790h Publication Date (Web): July 6, 2012 Copyright © 2012 American…