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Pyrene Availability As Determined by the Interactions of Natural Organic Matter with the Soil Mineral Matrix

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Pyrene Availability As Determined by the Interactions of Natural Organic Matter with the Soil Mineral Matrix PYRENE AVAILABILITY AS DETERMINED BY THE INTERACTIONS OF NATURAL ORGANIC MATTER WITH THE SOIL MINERAL MATRIX Denise Marie Brown A dissertation submitted to the faculty of the University of North Carolina at Chapel Hill in partial fulfillment of the requirements for the degree of Doctor of Philosophy in the Department of Environmental Sciences and Engineering, School of Public Health. Chapel Hill 2006 Approved by: Advisor: Professor Frederic K. Pfaender Reader: Professor Michael D. Aitken Reader: Professor Marc J. Alperin Reader: Professor Russell F. Christman Reader: Professor Steven C. Whalen © 2006 Denise Marie Brown ALL RIGHTS RESERVED ii ABSTRACT DENISE MARIE BROWN: Pyrene Availability as Determined by the Interactions of Natural Organic Matter with the Soil Mineral Matrix. (Under the direction of Professor Frederic K. Pfaender) Soil organic matter (SOM), especially humic substances and biological material, profoundly affect polyaromatic hydrocarbon (PAH) movement, toxicity, and degradation when assessing acceptable end points for in situ remediation practices. The complex, inter- dependent relationship between soil chemical and physical attributes makes determining absolute PAH fate, transport, and availability a formidable task. This research attempted to correlate the impact known SOM components have on pyrene sorption as related to sorbent loading and type and mineral phase aggregation. The objective was achieved by generating a synthetic soil, composed of mineral matter, humic acid (HA), and peptidoglycan (PG), and comparing this matrix to freshly contaminated and aged natural soils, using pyrene as the representative hydrophobic organic contaminant. In contrast to HA, a larger concentration of PG sorbed to both mineral phases (hematite and montmorillonite clay); thus, promoting further particle aggregation, and effectually resulting in greater pyrene sorption as evidenced by HPLC and fluorescence microscopy. The greater the concentration and number of constituents introduced into the synthetic matrix, culminating in a HA+PG mixture loaded onto clay, the greater the resulting pyrene sorption and similarity to spiked natural soils, both in chemical and physical attributes. The final result was a compiled fluorescence map visually detailing pyrene iii location and percentage sorbed in relation to PG, HA, and the mineral phases for natural and synthetic soils, where the biological constituent held a significant influence over pyrene compared to that by the humic substances. In summary, the type and concentration of SOM constituents, specifically humic substances and biological material, sorbed to a mineral phase significantly impact soil physical and chemical characteristics, and therefore, should be accounted for when determining pyrene fate, transport, and availability within contaminated soil systems. Potentially, when these observations are combined with fluorescence microscopy, consultants could determine the most effective remediation technology to target specific locations, such as pore spaces, or strong sorptive entities, such as PG, and achieve acceptable end-points. iv This dissertation is dedicated to those that supported me the most…. To my parents, Robert and Sandy Brown, who taught me to persevere and strive for the best. To my brother and sister-in-law, Darren and Angela Brown, who always knew when to ask “Aren’t you done yet?” Finally, to my nephew, Austin, who always inspires me. Finally, to my husband, Jeff Zborowski, who was kind enough to go to Iraq for seven months and leave me alone to finish this monstrosity, but also the one to make me smile through the frustration and love me through the tears. Thank you. v ACKNOWLEDGEMENTS This research was supported by the Superfund Hazardous Substances Basic Research Program grant (5P42ES05948). For use of their scientific instruments, I thank Professor Marc Alperin (TOC), Professor Mike Aitken (HPLC), Dr. Wallace Ambrose (SEM), and Dr. Robert Bagnell (CLSM). For their valuable assistance, I acknowledge Dr. Robert Schoonhoven (image analysis and compilation), Dr. Chad Roper (flow cell and HPLC method), Tom Long and Joanna Park (HPLC method), and Dr. Glenn Walters (evaporation station). For brainstorming, support, and therapeutic complaint sessions, I deeply thank Julie Swanson, Sabrina Powell, Kate Lindsay, Dr. David Singleton, Michelle Sullivan, and Maiysha Jones. Finally, for their research guidance, I also thank my committee, Professors Fred Pfaender (my advisor), Mike Aitken, Marc Alperin, Russ Christman, and Steve Whalen. Thank you. vi TABLE OF CONTENTS LIST OF TABLES ....………………………………………………………………………....xii LIST OF FIGURES .....…………………………………………………………………… ..xiv LIST OF ABBREVIATIONS .…………………………………………………………… xviii Chapter 1. INTRODUCTION AND OBJECTIVES ………………………………………............ ….1 1.1 Introduction …………………………………………………………………......... ….1 1.2 Objectives ………………………………………………………………………… ….3 2. LITERATURE REVIEW ….……………………………………………………………….7 2.1 Soil Chemical Structure .....…………………………………………………......... .…7 2.1.1 Soil Organic Matter (SOM) ...……………………………………………… ….8 2.1.1.1 Soil Organic Matter Components ………....……………………......... ...10 2.1.1.2 Dual Mode Model: Glassy versus Amorphous Carbon …………………14 2.1.2 Soil Organic Matter Sorption to Mineral Phases ..…………………….........…16 2.1.2.1 Humic Substance Sorption to Mineral Phases ...………….….…………18 2.1.2.2 Peptidoglycan Sorption to Mineral Phases ...……………………………20 2.1.3 Summary ...………………………………………………………………….…21 2.2 Soil Physical Structure …………..……………………………...………………..…22 2.2.1 Mineral Phases ……………………………………………………………...…22 vii 2.2.2 Aggregation …….………………………………...………………………... ...24 2.2.3 Pore Spaces ………….……..………………………………...…………….. ...25 2.3 Polyaromatic Hydrocarbons ...…………………………………………………… ...27 2.3.1 Dual Mode Sorption Model ………………………….…………………….. ...29 2.3.1.1 PAH Dissolution into SOM ………………………………………….. ...33 2.3.1.2 Filling SOM and Mineral Phase Holes with PAHs …..…………………35 2.4 Summary ………………………………………………………………………….…37 3. SYNTHETIC CLAY AS A SURROGATE FOR MODELING PYRENE SORPTION TO NATURAL SOIL ..………………………………………..…39 3.1 Introduction …………………………………...…………………………………..…39 3.2 Experimental Section ...…………………………………………………………...…40 3.2.1 Natural Soils ………………………………………………………………..…40 3.2.2 Synthetic Soils ……………………………………………………………...…41 3.2.3 Aqueous Phase PG and HA Analysis …………………………………………42 3.2.4 Particle Surface Area (PSA) Analysis ……………………………………...…43 3.2.5 Pyrene Application to Synthetic and Natural Soils …………………...........…44 3.2.6 Aqueous Phase Pyrene Analysis …………………………………………...…45 3.2.7 Fluorescence Microscopy …………………………………………………..…46 3.2.8 Fluorescence Intensity Analysis ……………………………………............…47 3.3 Results ..……………………………………………………………………...........…47 3.3.1 Comparison of Physical and Chemical Attributes ………………................…47 3.3.2 Particle Surface Area (PSA) Analysis ……………………………………...…48 3.3.3 Pyrene Sorption to Natural and Synthetic Soils ………………………………49 viii 3.4 Discussion …………………………………………………………………...........…51 4. IMPACT OF HUMIC ACID AND PEPTIDOGLYCAN ON THE TOTAL ORGANIC CARBON CONCENTRATION AND PARTICLE AGGREGATION OF SYNTHETIC SOIL ………………………............…54 4.1 Introduction ………………………………………………………………….........…54 4.2 Experimental Section ...……………………………………………………............…56 4.2.1 Synthetic Soils ………………………………………………………...........…57 4.2.2 Aqueous Phase PG and HA Analysis …………………………………………57 4.2.3 Particle Surface Area (PSA) Analysis ……………………………………...…57 4.2.4 Fluorescent Labeling of Peptidoglycan ……………………………….........…57 4.2.5 Fluorescence Microscopy …………………………………………………..…58 4.2.6 Image Compilation ……………………………………………………………59 4.2.7 Fluorescence Intensity Analysis ………………………………………….……61 4.3 Results ……………………………………………………………………….........…61 4.3.1 Humic Acid (HA) Sorption ………………………………………………...…61 4.3.2 Peptidoglycan (PG) Sorption ……………………………………………….…67 4.3.3 Humic Acid (HA) and Peptidoglycan (PG) Combined Sorption …………..…71 4.4 Discussion …………………………………………………………………............…76 5. INFLUENCE OF SOM COMPONENTS ON PYRENE FRESHLY SPIKED IN SYNTHETIC AND NATURAL SOILS ……………………………........…88 5.1 Introduction ………………………………………………………………….........…88 5.2 Experimental Section ...……………………………………………………............…90 5.2.1 Natural and Synthetic Soils …………………………………………...........…90 5.2.2 Pyrene Application to Synthetic and Natural Soils …………………...........…91 ix 5.2.3 Aqueous Phase Pyrene Analysis ……………………………………............…91 5.2.4 Fluorescent Labeling of Peptidoglycan ……………………………….........…91 5.2.5 Fluorescence Microscopy …………………………………………………..…92 5.2.6 Image Compilation ……………………………………………………….……92 5.2.7 Fluorescence Intensity Analysis ………………………………………………92 5.2.8 Fluorescence Histograms to Determine Pyrene-SOM Associations ….........…92 5.3 Results ……………………………………………………………………………..…95 5.3.1 Background Interference and Pyrene Sorption Tests …………………………95 5.3.2 Pyrene Sorption to HA Synthetic Soils ………………………………...........100 5.3.3 Pyrene Sorption to PG Synthetic Soils ………………………………............104 5.3.4 Pyrene Sorption to HA + PG Synthetic Soils ………………………………..107 5.3.5 Pyrene Sorption to Natural Soils …………………………………….............111 5.3.6 Pyrene Preference and “Mapping” Contaminated Soils ……………………..114 5.4 Discussion ……………………………………………………………………….....122 6. FLUORESCENCE INTENSITY AS A TECHNIQUE TO STUDY PAH CONCENTRATIONS, FATE, AND TRANSPORT WITHING SOILS ……………………………………………………………………....133 6.1 Introduction …………………………………...…………………………………....133 6.2 Experimental Section ...……………………………………………………..............135 6.2.1 Natural and Synthetic Soils ……………………………………………….....135
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