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Characterization of Tributyl Degradation Using FTIR-ATR Spectroscopy and Carbon Stable Isotope Ratio Mass Spectrometry April Renae Gillens Clemson University

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Characterization of Tributyl Degradation Using FTIR-ATR Spectroscopy and Carbon Stable Isotope Ratio Mass Spectrometry April Renae Gillens Clemson University Clemson University TigerPrints All Dissertations Dissertations 8-2016 Characterization of Tributyl Degradation Using FTIR-ATR Spectroscopy and Carbon Stable Isotope Ratio Mass Spectrometry April Renae Gillens Clemson University Follow this and additional works at: https://tigerprints.clemson.edu/all_dissertations Recommended Citation Gillens, April Renae, "Characterization of Tributyl Degradation Using FTIR-ATR Spectroscopy and Carbon Stable Isotope Ratio Mass Spectrometry" (2016). All Dissertations. 1733. https://tigerprints.clemson.edu/all_dissertations/1733 This Dissertation is brought to you for free and open access by the Dissertations at TigerPrints. It has been accepted for inclusion in All Dissertations by an authorized administrator of TigerPrints. For more information, please contact [email protected]. CHARACTERIZATION OF TRIBUTYL PHOSPHATE DEGRADATION USING FTIR-ATR SPECTROSCOPY AND CARBON STABLE ISOTOPE RATIO MASS SPECTROMETRY A Dissertation Presented to the Graduate School of Clemson University In Partial Fulfillment of the Requirements for the Degree Doctor of Philosophy Environmental Engineering and Earth Sciences by April Renae Gillens August 2016 Accepted by: Dr. Brian A. Powell, Committee Chair Dr. Cindy Lee Dr. Julianna Fessenden-Rahn Dr. Lindsay Shuller-Nickles Dr. Michael J. Singleton i ABSTRACT Tributyl phosphate (TBP) is used as an extractant in the Plutonium and Uranium Reduction Extraction (PUREX) process, as well as the Aqueous Chloride Process for Plutonium (Pu) recovery. These processes use nitric acid and hydrochloric acid, respectively. After nuclear reprocessing, TBP may be degraded in the Alkaline Hydrolysis Process using >12.5 M NaOH at 120-130 oC. TBP degrades to dibutyl phosphate (DBP), monobutyl phosphate (MBP), butanol, and phosphoric acid during hydrolysis. The goal of this dissertation is to use carbon stable isotopes to determine if there is a unique signature in TBP associated with nuclear reprocessing and solvent disposal. Acid hydrolysis experiments were performed for a three month period to determine if a fractionation in the carbon stable isotope of TBP exists over time. Alkaline hydrolysis experiments were also performed to simulate the solvent disposal process used to degrade TBP. Theoretical calculations predicting the carbon and oxygen stable isotope fractionations through use of ab initio methodology were performed and compared with experimental values. In addition, this work developed a semi-quantitative tool to determine the extent of TBP degradation as it is exposed to nitric acid and sodium hydroxide. The semi-quantitative tool involved the quantification of peak intensity ratios using FTIR-ATR spectroscopy. Another component of this work included solid phase extraction (SPE) to separate TBP and DBP from aqueous media. It was found that the extent of fractionation predicted by theory aligns well with the experimental results. The carbon stable isotope measurements in TBP revealed that a heavy shift occurs in reactions of TBP with nitric acid, hydrochloric acid, and sodium hydroxide. The largest ii shift of 8.3 per mil was seen when TBP was reacted with 9 M HCl at 75 oC. There was a 4 per mil difference between the carbon stable isotope value of TBP in 9 M HCl and 8 M o HNO3 at 75 C. It is suspected that this difference would merge over time. Hydrolysis o experiments conducted in 4 M HCl and 4 M HNO3 at temperature ≤ 50 C for three months showed no significant fractionation. However, only a small fraction of TBP was degraded within this short time-frame. The degradation of TBP in 12.5 M NaOH was near completion but less than a 2 per mil fractionation was measured. It is possible that this process does not give a significant fractionation due to its degradation mechanism. The FTIR-ATR peak intensity ratio for the alkaline hydrolysis system yields a close approximation of the extent of TBP degradation relative to the amount quantified by gas chromatography. This dissertation gives valuable insight on the characterization of carbon stable isotopes and the FTIR-ATR analysis of TBP that is helpful to the nuclear forensics community. iii DEDICATION To my beloved Uncle, the late Curtis Edward Gillens and to my children. iv ACKNOWLEDGMENTS Thank you, Toti Larson, for teaching me the ropes of this research. I can honestly say that the content herein revolves around what I have learned from and with you during my time as a Post Baccalaureate at the Los Alamos National Laboratory (June 2010— July 2011). Thank you for being patient with me and helping me to believe that I too can be a scientist. Thank you, U.S. Department of Homeland Security Education Programs, for believing in me and influencing my career path. I am very grateful for your sponsorship in the form of the U.S. Department of Homeland Security Undergraduate Scholarship (August 2008—August 2011). It was through this scholarship that I was able to intern at the Los Alamos National Laboratory and discover my passion for nuclear forensics research. Thank you, U.S. Department of Homeland Security Nuclear Forensics Graduate Fellowship, for funding my graduate education and providing me with resources that many graduate students often do not receive. Thank you, Clemson University, for opening your doors for me to achieve the highest degree obtainable. I am honored to become the first African-American to earn a Ph.D. in Environmental Engineering and Science from Clemson University. This material is based upon work supported by the U.S. Department of Homeland Security under Grant Award Number, 2012-DN-130-NF0001-01. The views and conclusions contained in this document are those of the authors and should not be interpreted as necessarily representing the official policies, either expressed or implied, of the U.S. Department of Homeland Security. v TABLE OF CONTENTS Page TITLE PAGE .................................................................................................................... i ABSTRACT ..................................................................................................................... ii DEDICATION ................................................................................................................ iv ACKNOWLEDGMENTS ............................................................................................... v LIST OF TABLES ........................................................................................................... x LIST OF FIGURES ....................................................................................................... xii CHAPTER I. INTRODUCTION ......................................................................................... 1 Relevance of Project to DHS DNDO/NTNFC TNF ................................ 1 Purpose of the Study ................................................................................ 2 II. LITERATURE REVIEW .............................................................................. 5 Tributyl Phosphate in the PUREX Process .............................................. 5 Typical PUREX Flowsheet ...................................................................... 6 First Solvent Extraction Cycle ................................................................. 7 Second Solvent Extraction Cycle for Pu and U ....................................... 8 Inefficiency of the PUREX Process as a Function of Degradation Product Ingrowth during Reprocessing ........................................................... 8 TBP Disposal/Caustic Treatment ........................................................... 12 TBP’S Role in Pu Processing ................................................................ 14 Hydrochloric Acid Processing ............................................................... 14 TBP Degradation Mechanisms – Dealkylation versus Hydrolysis ........ 15 Acidic Hydrolysis .................................................................................. 17 Alkaline Hydrolysis ............................................................................... 20 Analytical Instrumentation and Methods for the Characterization of TBP ................................................................................................... 21 Infrared Spectroscopy and Gas Chromatography .................................. 22 Solid Phase Extraction ........................................................................... 23 Carbon Stable Isotope Ratio Mass Spectrometry .................................. 23 vi Table of Contents (Continued) Page Combining Existing Technologies ......................................................... 26 Knowledge Gaps .................................................................................... 26 III. HYPOTHESES & OBJECTIVES .. .............................................................28 Hypotheses ............................................................................................. 28 Objectives for the Theoretical Work ...................................................... 29 Objectives for the Experimental Work .................................................. 30 General Task Descriptions ..................................................................... 32 Task Interrelatedness ............................................................................. 33 Overview ................................................................................................ 34 IV. RAPID QUANTIFICATION OF TBP AND TBP DEGRADATION PRODUCT RATIOS BY FTIR-ATR ....................................................35
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