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Structural Analysis of Water and Alcohol Solutions

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Structural Analysis of Water and Alcohol Solutions Structural analysis of water and alcohol solutions A thesis submitted to the Graduate School of the University of Cincinnati in partial fulfillment of the requirements for the degree of Master of Science in the Department of Materials Science of the College of Engineering and Applied Science by Kelly J. Cross B.S. Purdue University May 2007 Committee Chair: Dale W. Schaefer, Ph.D. Abstract Water-alcohol solutions have been extensively studied to correlate molecular structure to thermodynamic properties, which are known to deviate strongly from ideality. This project offers an analysis of cluster formation in ethanol-water binary solutions and an approach to identify distinctive structures within water and alcohol (W-A) solutions. Thermodynamic properties (such as enthalpy) and hydrogen bond strength can provide physical evidence of clustering within the solution. The heat of mixing was observed as a function of concentration. The concentration dependence of hydrogen bonding strength was analyzed through Infrared spectroscopy. Molecular aggregation in solution was explored experimentally with light scattering. Some of the results were consistent with published data and some results did not support data in the current literature. The calorimetry data were consistent with the published data showing a minimum at ~20 mol%. In the water rich region, we assume the hydrogen-bonded water clusters isolate individual ethanol molecules. The frequency shift observed with IR spectroscopy shows that the C-O bond strength increases with increasing ethanol concentration. Similar to the observations of D’Angelo, the frequency shift of the C-O and C-H stretching is concentration-dependent and is attributed to the transfer of electron density from the carbon of the methyl group. The observed minimum (17 mol%) in the H-OH bending absorption band frequency indicates an increase in hydrogen bond strength between water molecules in the water-rich region. ii The light scattering analysis was complex and required multiple systems to draw conclusions from the results. Two systems, ethanol in water and butoxy-ethanol in water, were studied with light scattering to observe the Rayleigh ratio (RR). The RR is proportional to the scattered light intensity. The ethanol-in-water system did not show a peak in the plot of RR as a function of concentration. However, for the butoxy-ethanol system a maximum in the RR vs. concentration occurs at ~2.5 mol%, close to the 3 mol% reported by Ito. The average scattering intensity, however, was four times less than reported by Ito and Schmitz. The major finding of the research is that the cluster nature, which is intimately related to solution properties, changes with concentration. The calorimetry and IR data suggest enhanced hydrogen bond strength of water in the water rich region that transitions to increased self association of ethanol in the alcohol rich region. iii Blank Page iv Acknowledgements First, I would like to thank The Creator and sustainer of all life. To my ancestors who paved the way for me including my father, Pastor Israel L. Cross II. Next I would like to thank my mother for being my hero and my role model. I am grateful for the support of my partner, my family, and my extended family. Thank you Drs. Marie Paretti and Holly Matusovich for teaching me technical writing. Thank you to Dr. Schaefer, Dr. Danni Wu, Dr. Naiping Hu, Dr. Stephen G. Fenimon, Dr. Carlos Co, Dr. Douglas Kohls and the Schaefer research group for their collective efforts. Lastly, thank you to OVAL for the financial support of this research. Hotep v Table of Contents Abstract .................................................................................................................................................. ii Blank Page .............................................................................................................................................. iv Acknowledgements ................................................................................................................................. v Table of Contents ................................................................................................................................... vi List of Tables and Figures .......................................................................................................................viii Chapter 1: Introduction ........................................................................................................................... 1 Motivation for Study ........................................................................................................................ 1 Chapter 2: Calorimetry and Thermodynamics .......................................................................................... 3 Chapter 2.1: Introduction .................................................................................................................... 3 Chapter 2.2: Experiment ...................................................................................................................... 6 Chapter 2.3: Results and Discussion ..................................................................................................... 8 Chapter 2.4: Conclusions ................................................................................................................... 12 Chapter 3: FT-IR ..................................................................................................................................... 13 Chapter 3.1: Introduction .................................................................................................................. 13 Chapter 3.2: Experiment .................................................................................................................... 17 Materials ....................................................................................................................................... 17 Measurements .............................................................................................................................. 17 Chapter 3.3: Results and Discussion ................................................................................................... 19 Chapter 3.4: Conclusions ................................................................................................................... 24 Chapter 4: Light Scattering .................................................................................................................... 26 Chapter 4.1- Introduction/Motivation for Study .................................................................................... 26 Chapter 4.2: Experiment .................................................................................................................... 29 Materials ....................................................................................................................................... 29 Measurements .............................................................................................................................. 29 Chapter 4.3: Results and Discussion ................................................................................................... 32 vi Water-Ethanol (W-E) ..................................................................................................................... 32 2-Butoxy-ethanol in water (BE) ...................................................................................................... 33 Chapter 4.4: Conclusions ................................................................................................................... 36 Chapter 5: Summary and Future Work................................................................................................... 37 References ............................................................................................................................................ 39 Appendices............................................................................................................................................ 41 Appendix A: Calorimetry ....................................................................................................................... 41 Calorimetry Procedure ................................................................................................................... 41 IR Spectroscopy Chapter .................................................................................................................... 42 1.3.2 Spectrum .............................................................................................................................. 42 IR Summary Tables ........................................................................................................................ 44 Light Scattering Chapter .................................................................................................................... 46 Appendix C: Static Light Scattering Procedure ....................................................................................... 46 Appendix D: Dynamic Light Scattering Procedure.................................................................................. 51 vii List of Tables and Figures Figure 1: Schematic of the ChemiSens CPA200 calorimeter [10] .............................................................. 8 Figure 2: Multiple peak-fitting example of EtOH added to water............................................................ 10 Figure 3: Excess enthalpy of mixing (∆H)
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