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Mirecki Phd.Pdf .. AMINOSTRATIGRAPHY, GEOCHRONOLOGY AND GEOCHEMISTRY OF FOSSILS FROM LATE CENOZOIC MARINE UNITS IN SOUTHEASTERN VIRGINIA By June Elizabeth Mirecki A dissertation submitted to the Faculty of the University of Delaware in partial fulfillment of the requirements for the degree of Doctor of Philosophy in Geology June 1990 N AMINOSTRATIGRAPHY, GEOCHRONOLOGY AND GEOCHEMISTRY OF FOSSILS FROM LATE CENOZOIC MARINE UNITS IN SOUTHEASTERN VIRGINIA By June Elizabeth Mirecki Approved: _ Billy P. Glass, Ph.D. Chairman of the Department of Geology Approved:, -:-- _ Carol E. Hoffecker, Ph.D. Acting Associate Provost for Graduate Studies b AMINOSTRATIGRAPHY, GEOCHRONOLOGY AND GEOCHEMISTRY OF FOSSILS FROM LATE CENOZOIC MARINE UNITS IN SOUTHEASTERN VIRGINIA '. By June Elizabeth Mirecki I certify that I have read this dissertation and that in my opinion it meets the academic and professional standard required by the University as a dissertation for the degree of Doctor of Philosophy. Signed: _ John F. Wehmiller, Ph.D. Professor in charge of dissertation I certify that I have read this dissertation and that in my opinion it meets the academic and professional standard required by the University as a dissertation for the degree of Doctor of Philosophy. Signed: _ Billy P. Glass, Ph.D. Chairman of the Department of Geology and member of dissertation committee I certify that I have read this dissertation and that in my opinion it meets the academic and professional standard required by the University as a dissertation for the degree of Doctor of Philosophy. Signed: - _ Dr. Peter B. Leavens, Ph.D. Member of dissertation committee I certify that I have read this dissertation and that in my opinion it meets the academic and professional stpndard required by the University as a dissertation for the degree of Doctor of Philosophy. Signed: _ Dr. Noreen Tuross, Ph.D. Member of dissertation committee I certify that I have read this dissertation and that in my opinion it meets the academic and professional standard required by the University as a dissertation for the degree of Doctor of Philosophy. Signed: _ Dr. Harold White, Ph.D. • Member of dissertation committee t • TABLE OF CONTENTS List of Tables." , . List of Figures " "" ". CHAPTER 1: INTRODUCTION AND STATEMENT OF PURPOSE .. CHAPTER 2: ANALYTICAL METHODS I: SEPARATION AND QUANTIFICATION OF AMINO ACiDS . 2.1: Sample Preparation . 2.2: System Description . 2.2.1: A Note on Reagent and Laboratory Glassware Quality . 2.3: Calculation of Amino Acid Concentration " .. CHAPTER 3: EVALUATION OF AMINO ACID DATA . 3.1: Introduction and Structure of Chapter . 3.2: Chromatographic Criteria . 3.3: Precision of ILC Molluscan Shell Powder Analyses . 3.3.1: Precision of Amino Acid Concentrations From ILC-B Molluscan Shell Powders .. 3.3.2: Precision of Amino Acid Fractions From ILC-B Molluscan Shell Powders .. 3.3.3: Precision of Free/Total Amino Acid Values From ILC-B Molluscan Shell Powders . 3.3.4: Precision of ALLOIISO Values From ILC-B Molluscan Shell Powders .. 3.3.5: Accuracy of ALLO/ISO Values from ILC-B Molluscan Shell . Powders .. 3.4: Precision of Fossil Sample Analyses .. 3.4.1: Comparison of Fossil Sample and ILC Standard Data Run Concurrently . CHAPTER 4: ANALYTICAL METHODS II: ATOMIC ABSORPTIQN SPECTROMETRY, X-RAY DIFFRACTION, SCANNING ELECTRON MICROSCOPY AND WEIGHT GAIN/LOSS EXPERIMENTS .. 4.1: Introduction and Structure of Chapter .. 4.2: Atomic Absorption Spectrometry Methods: Calcium, Strontium, Manganese and Iron . 4.2.1: Estimation of Dilution Error .. 4.2.2: Comments for Future Work . ...2 4 4.3: Scanning Electron Microscopy ,.. ".. " ", , ,,." .. 4.4: X-Ray Diffraction Methods . 4.5: Water Weight Gain/Loss Experiments""", .. CHAPTER 5: GEOLOGIC HISTORY OF THE PLEISTOCENE UNITS • FOUND IN THE OUTER COASTAL PLAIN OF SOUTHEASTERN ViRGINIA " " "., 5.1: Introduction " .. 5.2: Lithostratigraphy of Pleistocene Units in Southeastern Virginia (Oaks and Coch.1973) . 5.3: Reinterpretations Considering Timing and Magnitude of Sea Level Rise . 5.4: Lithostratigraphy of Related Field Sites in Virginia: Norris Bridge and Yadkin Pit. , .. 5.4.1: The Norris Bridge Locality .. 5.4.2: The Yadkin Pit Locality .. 5.5: Comparison of Stratigraphic Frameworks Applied in Southeastern Virginia . 5.5.1: Definition of Lithostratigraphic Frameworks in Southeastern Virginia .. 5.5.2: Definition of Biostratigraphic Frameworks in Southeastern Virginia . 5.5.3: Definition of an Allostratigraphic Framework in Southeastern Virginia. and Its Relationship to Aminostratigraphy . CHAPTER 6: AMINOSTRATIGRAPHY OF THE PLEISTOCENE UNITS FOUND IN THE OUTER COASTAL PLAIN OF SOUTH- EASTERN ViRGINIA "" ". 6.1: Introduction .. 6.2: Aminostratigraphy of Gomez Pit. 6.3: Aminostratigraphy of the Yadkin Pit and Norris Bridge Localities.. 6.4: Calibration of ALLOnSO Values in Southeastern Virginia .. 6.4.1: Uranium Series Ages ". 6.5: Age Estimates Using the ESR (Electron Spin Resonance) Dating MetNod " . 6.6: Age Options for Aminoiones Defined in Southeastern Virginia .. 6.6.1: Aminozone IIa . 6.6.2: Aminozone lie , . 6.6.3: Aminozone lid ,. 6.6.4: Aminozone lie . 6.7: Concluding Remarks . CHAPTER 7: AGE ESTIMATES FOR AMINOZONES DEFINED IN SOUTH­ EASTERN VIRGINIA USING THE NON-LINEAR MODEL OF ISOLEUCINE EPIMERIZATION " .. 7.1: Introduction .. • • II n (7.1: Introduction ~ 7.2: Modeling Temperature History . 7.3: The Quantitative Non-Linear Model of Isoleucine Epimerization .. 7.4: Amino Acid Epimerization Age Estimates for Aminozones IIc and lid in Southeastern Virginia .. 7.4.1: Age Estimates Using Aminozone lIa Calibrated By 70.2 ka Uranium Series Dates . 7.4.2: Age Estimates Using Aminozone Ita Calibrated By Substage 5e (120 ka) High Sea Stand .. 7.5: Summary . CHAPTER 8: DIAGENETIC MODIFICATION OF MOLLUSC SHELL: ANALYSIS OF AMINO ACID COMPOSITION, ELEMENTAL CONCENTRATIONS, MINERALOGY AND TEXTURES IN LATE CENOZOIC MOLLUSCS 8.1: Introduction . 8.2: Definition of Shell Quality . 8.2.1: Relationship Between Shell Quality and Shell Porosity: Water Weight Gain/Loss Experiments . 8.2.2: Relationship Between Shell Age ,and Shell Micro- textures: SEM Observations . 8.3: A General!zed Model of Diagenetic Hydrolysis and Epimerization . 8.4: Toward a Leaching Model for Molluscan Shell Amino Acids . 8.5: Variations in Amino Acid Composition with Condition . • 8.5.1: Gomez Pit Aminozone Ila . 8.5.2: Comparison of Amino Acid Data Between Gomez Pit IIc and Yadkin Pit Ilc . 8.5.3: Comparison of Amino Acid Data Between Norris Bridge lid and Gomez Pit lid .. 8.6: Variations in Amino Acid Composition with Time . 8.6,,;1: Changes in Amino Acid Concentrations and Their Distribution in Free and Bound States . 8.7: Sr Concentrations and Sr/Ca Values with Time, and Condition . CHAPTER NINE: SUMMARY AND FUTURE WORKS : .. REFERENCES CiTED . Appendix A: ILC Data and Experiments Appendix A.1: Total and Free ILC-B Concentration Data. Appendix A.2: Total and Free ILC-B Concentration Data Appendix A.3: Free/Total Values for ILC-B Samples Appendix A.4: Hydrolysis Experiment Data .. Iq LIST OF TABLES Table 3-1: Sample description for ILC standard molluscan shell powders..... Table 3-2: Statistical summary describing precision of ILC-B FreelTotal values for each amino acid .. Table 3-3: Comparison of mean ALLO/ISO values and standard deviations with published data .. Table 4-1: Summary of techniques used to determine diagenetic changes in molluscan shell carbonate ·. Table 4-2: Operating parameters for elemental analyses using flame atomic absorption spectrometry . Table 4-3: Statistics describing 10 analyses of the ILC-D powder to determine dilution error " ······· ··· Table 6-1: Statistics describing four aminozones found in southeastern • Virginia and the Delmarva peninsula """ " . Table 6-2: Uranium series ages obtained from fossil corals collected from localities described in the text. "" · Table 6-3: Electron spin resonance age estimates and (ALLO/ISO)TOTAL values obtained from analyses of mollusc valves collected from Gomez Pit. "" "" " "."." " "". Table 7-1: Range of (ALLO/ISO)TOTAL values and corresponding y values for each aminozone defined in Gomez Pit. Table 7-2:The range of age estimates (in ka) calculated for aminozone lie (above) and aminozone lid (below) in Gomez Pit using maximum, mean and minimum values of y1 and y2 as applied to the non-linear kinetic model of isoleucine epimerization .. Table 7-3: The range of age estimates (in ka) calculated for aminozone IIc (above) and aminozone lid (below) in Gomez Pit using maximum, mean and minimum values of y1 and y2 as applied to the non-linear kinetic model of isoleucine epimerization .. Appendix Table A.1-1: Total ILC-S Concentration data Appendix Table A.1-2: Free ILC-S Concentration data Appendix Table A.2-1: Total ILC-S Fraction data Appendix Table A.2-2: Free ILC-S Fraction data Appendix Table A.3-1: Free/Total Values for ILC-S Samples Appendix Table A.4-1: Hydrolysis Experiment Data Appendix Table A.S-1: Glassware Adsorption Data Appendix Table C.1-1: Ca, Fe, Mn and Sr concentrations (lJg/g shell) in mollusc shells Appendix Table C.2-1: R values for calcite/aragonite mixtures, obtained from X-ray diffraction Appendix Table C.3-1: Raw data from long-term weight gain/loss experiment Appendix Table C.3-2: Raw data from short-term weight gain/loss experiment Appendix Table E.1-1:, Uranium concentrations used to calculate internal dose in shell samples for ESR dating Appendix Table E.1-2: Element concentrations in sediment for each UDAMS si~e from which shells were analyzed Appendix Table F.1-1: Values of constants a and b for the kinetic equation • for isoleucine epimerization LIST OF FIGURES Fig. 1-1 : L- and 0- stereoisomers of the amino acid isoleucine . Fig. 1-2: Area of study . Fig. 2-1 : Flow chart showing laboratory analyses of a molluscan fossil. ...... Fig. 2-2: Typical chromatogram of an ILC-B total hydrolysate sample .." ....... Fig. 2-3: Sample calculation of amino acid concentration from peak area raw data .
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