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The Role of Sulfur in the Preservation of Isoprenoid Hydrocarbons in Sedimentary Materials of the Washington Continental Margin

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The Role of Sulfur in the Preservation of Isoprenoid Hydrocarbons in Sedimentary Materials of the Washington Continental Margin AN ABSTRACT OF THE THESIS OF Luis Antonio Pinto Alvarez for the degree of Doctor of Philosophy_ in Oceanographypresented on September 23. 1993 Title: The Role of Sulfur in the Preservation of Isoprenoid Hydrocarbons in Sedimentary Materials of the Washington Continental Margin. Redacted for privacy Abstract approved: Fredrick G. Prahi A systematic study of highly branched isoprenoids (HBI) was carried outin suspended particulate material (SPM) and Washington coastal sediments todetermine their origin and fate. SPM collected at 10 m depth was filtered throughNitex membranes.C25HBI were found only in the 1.2-40 .tm range over the shelf. The particle size fractionation of SPM shows different enrichment for HEH, a common hydrocarbon in phytoplankton, and the sum ofC25HBI in the finer fractions suggesting these hydrocarbons do not share a common source. The distribution ofC25andC30HBI correlates with the chlorophyll maxima suggesting an upper-water microbial source associated with phytoplankton biomass. It has been hypothesized that sulfur addition into specific biomarkers occurs during the early stages of diagenesis. Incorporation of the HBI into a refractory geomacromolecule via a sulfur linkage or formation of HBI-thiophenes are notevident in the sedimentary lipids. HBI show a rapid decrease in concentration with depth inboth midshelf and slope sediments suggesting that biodegradation is the major pathwayfor their disappearance in Washington coastal sediments. Sediment cores from a midshelf and slope locations show the existenceof suboxic/anaerobic conditions within the first 5 cm in the sediments. Elementalsulfur distribution in the midshelf appears to be controlled by bioturbation. On the slope,its profile indicates a quasi steady state regime. Phytane and phytenes (ZPhy) are the major products of Raney nickel desulfurization in both midshelf and slope sediments. Spinach and a strain ofEm iliana huxleyitreated with Raney nickel showed strikinglysimilarpatternstothe desulfurization products of sedimentary lipids. The amount ofPhy in the slope decreases abruptly by a factor of 6 in the top 2 cm and gradually increases with depth. These results are interpreted as phytyl coming from two sources: (1) chlorophyll-a and (2) S-bound to geomacromolecules. Partial released of phytyl moieties from chlorophyll- a warrants a reevaluation of Raney nickel as a selective desulfurizing agentbefore its application for paleoenvironmental reconstruction. Reducing micro-environments appear to exist within the bioturbated zone in shelf sediments. However, there is no clear evidence for phytyl moieties S-linked to macromolecules within the mixed layer. Results obtained during this study indicate that sulfur incorporation to biomarkers, although present, does not represent a significant mechanism for the preservation of organic carbon in normal marine sediments. The Role of Sulfur in the Preservation of Isoprenoid Hydrocarbons in Sedimentary Materials of the Washington Continental Margin by Luis Antonio Pinto Alvarez A THESIS submitted to Oregon State University in partial fulfillment of the requirements for the degree of Doctor of Philosophy Completed September 1993 Commencement June 1994 Redacted for privacy Associate Professor of Oceanography in charge of major Redacted for privacy Dean ofCollege of Oceanography Redacted for privacy Dean of Gradu School Date thesis is presentedSeptember 23. 1993 Typed by Luis Antonio Pinto Alvarez ACKNOWLEDGEMENTS The completion of my graduate studies at O.S.U. would have not been possible without the involvement of many people at different times and in different ways. I thank Dr. Fredrick Prahl for providing the financial support and guidance in the development of this research. I acknowledge his skills as a scientist and his willingness to listen and to give poignant criticism during the experimental and writing stages of this study. I also thank Drs. Bob Collier, Chih-An Huh, Gary Klinkhammer, Christopher Langdon, Barry Sherr, and Bemd Simoneit, for the time they set aside to be members of my PhD committee. I thank the National Science Foundation for an award to participate in the XI Dissertation Symposium on Chemical Oceanography, Hawaii, 1993. I am especially grateful to the following people for their assistance in my research: Dr. Bernd Simoneit who provided space in his laboratory to set up the Raney nickel procedure, access to organosulfur standards, his personal library, and GCJMS facilities. Dr. Orest Kawka for helping me finding a summer job with ODP during Leg 127 to the Japan Sea, for analyzing some samples on the GCIMS and helpful discussion throughout my research. Dr. Roald Leif for his OSC data and "impromptu extended hours" talking about the "fate of the organic geochemist". Dr. Charles Miller for providing me with office space and phone facilities for so many years. Dr. Patricia Wheeler for a gift of Nitex membranes. Dr. Roy Carpenter for inviting me to participate on the 1990 cruise aboard the Wecoma. Dr. Chih-An Huh for teaching me the 210Pb and 234Th analysis. Dr. Robert Collier for allowing me to use his laboratory facility, including the AAS/graphite furnace and Chi Meredith for carrying out and teaching me the manganese and iron analyses. Margaret Sparrow for lipid extraction of the 1985 sediment core and maintenance of the CNS elemental analyzer. Kirsten Amthor for SPM data of 1988 and a gift of BT-6. Sandy Moore for the use of his analytical microbalance, helping to correct my written English and conversations regarding "the greedy megamachine". Laura for editing one of the chapters at an earlier stage. Joy Burke and Harold Sowers for going beyond their duty when I needed their help. The captain and crew of the R/V Wecoma 1985, 1988, 1990. Jorge for makingsure the final copy of my thesis reached the Graduate School. I thank the following people who provided financial support forme to stay in school: Dr. Robert Kiekel (Foreign Language Department), Dr. Jim Krueger (Department of Chemistry) and Dr. Tom Dillon (College of Oceanography) for supporting me with a Teaching Assistantship. Dr. Larry Moore and Marilyn Canfield (Department of Plant Pathology) for hiring me as a student worker to learn about apples and "Crown galls". Marilyn for friendship and support. Sarvahara and Susan for loan offers "to make Immigration happy". Drs. Marvin Durham and William Smart from the Office of International Education for their concern and help in finding solutions for us, "international students" (aka aliens) to be legal in this country. Above all, I am deeply indebted to four human beings who represent the best of friendship and through them I acknowledge all the rest of my friends. Christine, who shared with me her joy for life, sensitivity, good humor, time together when I got "sick" in Alvord desert, and "the rest of the family: Cathrina, Chris, Frank, Kyoung-Hee, Laura, and Tina". Michael, for being instrumental in resolving my visa status which allowed me to stay at OSU to pursue my PhD degree. Later, he was instrumental in my application for a postdoc in Alaska. We shared our love for music with the Peace Choir, and did not lose the hope even during that rough New Year's eve of 1990 in Albany. I also thank the support from his family. Sarvahara, for revealing an exciting world of new ideas and feelings, for our dialogues about science, Central America, "the other Evil Empire", the environment, and about personal relationships. Thank you for introducing me to Barry Lopez's writings. Sergio, "el Pelao", for our exhausting racketball encounters, the endless hours dreaming about "Blue Unicorns and the Southern Cross", and the friendship of his wonderful hosts Gail and Dave. A special place is in my heart for Alejandra, Erika, Betty & Jim Myers, and mama. Partial financial assistance came from NSF Grants OCE-87-16244, OCE-90- 00517, and OCE-92-03292. TABLE OF CONTENTS GENERAL INTRODUCTION.................................1 Transport and preservation of organic carbon in the marine environment .. 1 Incorporation of sulfur to labile organic molecules..................3 Objective of the present study................................4 Study area............................................. 5 II.EXPERIMENTAL METHODS.................................7 Sample collection........................................7 Interstitial water analysis..................................10 Elemental C,N and S analyses...............................10 Particle size separation....................................10 Lipid extraction.........................................11 Deasphalting...........................................13 Column chromatography..................................13 Recovery efficiencies.....................................13 Procedural blanks.......................................14 Raney nickel desulfurization................................14 Gas chromatographic (GC) analysis...........................14 Optimization of the GCIFPD...............................15 Standard curve for triphenylphosphine sulfide (TTPS)..............18 Elemental sulfur determination..............................21 Intercalibration of detectors and data acquisition packages...........22 Analytical precision......................................25 GC/mass spectrometry....................................27 ifi. BIOGEOCHEMISTRY OF HIGHLY BRANCHED ISOPRENOIDS IN SUSPENDED PARTICULATE MATTER OFF THE WASHINGTON COAST....................................30 Introduction...........................................30 Results...............................................34
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