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Long Term Blood Oxygenation Membranes University of Kentucky UKnowledge Theses and Dissertations--Biomedical Engineering Biomedical Engineering 2015 Long Term Blood Oxygenation Membranes Joseph V. Alexander University of Kentucky, [email protected] Right click to open a feedback form in a new tab to let us know how this document benefits ou.y Recommended Citation Alexander, Joseph V., "Long Term Blood Oxygenation Membranes" (2015). Theses and Dissertations-- Biomedical Engineering. 28. https://uknowledge.uky.edu/cbme_etds/28 This Doctoral Dissertation is brought to you for free and open access by the Biomedical Engineering at UKnowledge. It has been accepted for inclusion in Theses and Dissertations--Biomedical Engineering by an authorized administrator of UKnowledge. For more information, please contact [email protected]. STUDENT AGREEMENT: I represent that my thesis or dissertation and abstract are my original work. Proper attribution has been given to all outside sources. I understand that I am solely responsible for obtaining any needed copyright permissions. I have obtained needed written permission statement(s) from the owner(s) of each third-party copyrighted matter to be included in my work, allowing electronic distribution (if such use is not permitted by the fair use doctrine) which will be submitted to UKnowledge as Additional File. I hereby grant to The University of Kentucky and its agents the irrevocable, non-exclusive, and royalty-free license to archive and make accessible my work in whole or in part in all forms of media, now or hereafter known. I agree that the document mentioned above may be made available immediately for worldwide access unless an embargo applies. I retain all other ownership rights to the copyright of my work. I also retain the right to use in future works (such as articles or books) all or part of my work. I understand that I am free to register the copyright to my work. REVIEW, APPROVAL AND ACCEPTANCE The document mentioned above has been reviewed and accepted by the student’s advisor, on behalf of the advisory committee, and by the Director of Graduate Studies (DGS), on behalf of the program; we verify that this is the final, approved version of the student’s thesis including all changes required by the advisory committee. The undersigned agree to abide by the statements above. Joseph V. Alexander, Student Dr. Eric A Grulke, Major Professor Dr. Abhijit Patwardhan, Director of Graduate Studies LONG TERM BLOOD OXYGENATION MEMBRANES _______________________________________________ DISSERTATION _______________________________________________ A dissertation submitted in partial fulfillment of the requirements for the degree of Doctor of Philosophy in the College of Engineering at the University of Kentucky By Joseph Victor Alexander Lexington, Kentucky Co-Directors: Dr. Eric Anderson Grulke, Professor of Chemical and Materials Engineering and Dr. Joseph Bertram Zwischenberger, Professor of Surgery, Lexington, Kentucky Copyright© Joseph Victor Alexander 2014 ABSTRACT OF DISSERTATION LONG TERM BLOOD OXYGENATION MEMBRANES Hollow fiber membranes are widely used in blood oxygenators to remove carbon dioxide and add oxygen during cardiopulmonary bypass operations. These devices are now widely used off- label by physicians to perform extracorporeal blood oxygenation for patients with lung failure. Unfortunately, the hollow fiber membranes used in these devices fail prematurely due to blood plasma leakage and gas emboli formation. This project formed ultrathin (~100nm) polymer coatings on polymer hollow fiber membranes. The coatings were intended to “block” existing pores on the exterior surfaces while permitting high gas fluxes. This coating is synthesized using surface imitated control radical polymerization. The coating was durable and did not peel or degrade. Fibers modified using this coating technique did not substantially degrade the mechanical properties of the membrane. This coating technique prevented blood plasma leakage and gas emboli formation. The coating permitted blood oxygenation and carbon dioxide removal from in a mock circulation module. Coating formation on polymeric hollow fiber membranes using surface initiated controlled radical polymerization allows for the formation of membranes that have the potential for long term blood oxygenation. This coating technique would allow these long term blood membranes to be produced more inexpensively than currently existing membranes used for long term use. KEYWORDS: Hollow Fiber Membrane, Surface Initiated Polymerization, Atom Transfer Radical Polymerization, Long Term Blood Oxygenation, Extra Corporeal Membrane Oxygenation, Polymer Surface Modification ________Joseph Victor Alexander____ Student’s Signature ________________________________ Date LONG TERM BLOOD OXYGENATION MEMBRANES By Joseph Victor Alexander _________Dr. Eric A. Grulke Co-Director of Dissertation Dr. Joseph B. Zwischenberger Co-Director of Dissertation Dr. Abijit Patwardhan Director of Graduate Studies _______________________ Date To the family, friends and mentors that made this possible ACKNOWLEDGMENTS The following dissertation, while an individual work, benefited from the insights and direction of several people. First, I would like to acknowledge my gratitude to my Dissertation Co-Chairs, Dr. Eric Grulke, PhD and Dr. Joseph Zwischenberger, MD. Dr. Grulke’s ridged requirements for experimental analysis and reporting exemplify high quality scholarship. Dr. Zwischenberger’s enthusiasm, energy and openness to new ideas are an inspiration to all. I would like to sincerely thank both of these accomplished gentlemen for the freedom and independence they granted me. It has truly been a privilege to learn from both. Next, I wish to thank the complete Dissertation Committee, and outside reader, respectively: Dr. David Puleo, Dr. Thomas Dzuibla, Dr. Zhakary Hilt, Dr. Hainsworth Shin and Dr. Thomas Balk Each individual provided insights that guided and challenged my thinking, substantially improving the finished product. In addition to the technical and instrumental assistance above, I received equally important assistance from family and friends. Outside mentors provided me with the wisdom and knowledge to not only earn my PhD but to develop my learning and scientific abilities to the level at which I could independently devise and employ engineering solutions. My mother, Paula Alexander, instilled in me, from an early age, the desire and skills to obtain the Ph.D. iii Table of Contents ACKNOWLEDGMENTS iii LIST OF TABLEs viii LIST OF FIGURES ix Chapter 1 Introduction 1 Chapter 2 Background 3 2.1 Introduction 3 2.2 Blood Oxygenator Development 4 2.3 Lung Transplantation – Targets for Long Term Blood Oxygenator 5 2.3.1 Research Challenges 5 2.5 Atom Transfer Radical Polymerization 5 2.5.1 Research Challenges 6 2.6 Surface Initiated Atom Transfer Radical Polymerization 6 2.6.1 Research Challenges 7 2.7 Membrane Modifications with s-ATRP 7 2.7.1 Research Challenges 7 Chapter 3 Mechanical Strength of Hollow Fiber Membranes after Surface Functionalization 8 3.0 Abstract 8 3.1 Highlights 8 3.2 Introduction 8 3.3 Experimental 10 3.3.1 Materials 10 3.3.2 Hollow Fiber Preparation 10 3.3.3 Fiber Oxidation 10 3.3.4 Mechanical Testing 11 3.4.3 Burst Strength 13 3.3.5 Physio-Chemical Properties 16 3.4 Results and Discussion 17 3.4.1 Tensile Testing of PP HFM Exposed to Aqueous Potassium Persulfate 17 3.4.2 Ammonium Persulfate Pretreatment 21 3.4.3 Ozone Gas Pretreatment 21 3.4.4 Statistical Analysis of Tensile Testing Data from Treated Membranes 21 iv 3.4.5 Repeatability of Aqueous Treatments 31 3.4.6 X-Ray Diffraction of Polypropylene Hollow Fibers after Reaction with Functionalization Reagents 33 3.4.7 Fiber Permeation/Burst Strength 36 3.5 Conclusions 43 Chapter 4 Contamination Levels of Commercially Available Polypropylene Hollow Fiber Membranes and Effect on Surface Functionalization 44 4.0 Abstract 44 4.1 Highlights 44 4.2 Introduction 44 4.3 Experimental 45 4.3.1 Materials & Equipment 45 4.3.2 Equipment 45 4.3.3 Procedures 47 4.4 Results 49 4.4.1 HPLC chromatograms for soybean and mineral oils 49 4.4.2 Residue Extracted from Hollow Fiber Membranes 55 4.4.3 PEGMA coatings on hollow fiber membranes 57 4.4.4 Bubble point testing. 61 4.5 Discussion 61 4.6 Conclusions 62 Chapter 5 Ultrathin Polymer Films on Polymeric Hollow Fiber via Aqueous s-ATRP 63 5.0 Abstract 63 5.1 Highlights 63 5.2 Introduction 63 5.3 Materials and Methods 67 5.3.1 Materials and Equipment 67 5.3.2 S-ATRP Process 68 5.3.3 Coating Evaluation 68 5.3.4 Imaging of Hollow Fiber Membrane Samples Using Scanning Electron Microscopy 69 5.3.5 Bubble Testing of Coated HFM. 69 5.3.6 Pressure Testing of Coated HFM 71 5.3.7 Durability/Delamination Resistance of S-ATRP Coating 71 5.3.8 Porosity Determination 71 v 5.3.9 Durability of Surface Coating 72 5.4 Results and Discussion 73 5.4.1 Durability of Surface Coating 78 5.4.2 Pressure Testing of S-ATRP Formed Composite Hollow Fiber Membrane 78 5.4.3 Permeability of HFM Functionalized with S-ATRP Formed PEGMA Coating 80 5.5 Conclusions 80 Chapter 6 Modules Fabricated using Composite S-ATRP Hollow Fiber Membranes 81 6.0 Abstract 81 6.1 Highlights 81 6.2. Introduction 81 6.3 Materials and Methods 82 6.3.1 Fiber Bundle Fabrication and Cleaning 83 6.3.2 Fabrication of Hollow Fiber Membrane Module 83 6.3.3 Functionalization of fiber exterior surfaces 83 6.3.4 s-ATRP coating protocols 84 6.3.5 Fabrication of PMP Module 84 6.3.6 Gas Permeation of s-ATRP formed Composite PP HFM Module 84 6.3.7 Leak Testing
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