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Aqueous Α-Lipoic Acid Solutions for Removal of Arsenic and Mercury from Materials Used for Museum Artifacts

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Aqueous Α-Lipoic Acid Solutions for Removal of Arsenic and Mercury from Materials Used for Museum Artifacts Aqueous alpha-lipoic acid solutions for removal of arsenic and mercury from materials used for museum artifacts Item Type text; Electronic Dissertation Authors Cross, Peggi Publisher The University of Arizona. Rights Copyright © is held by the author. Digital access to this material is made possible by the University Libraries, University of Arizona. Further transmission, reproduction or presentation (such as public display or performance) of protected items is prohibited except with permission of the author. Download date 25/09/2021 22:18:37 Link to Item http://hdl.handle.net/10150/195574 AQUEOUS -LIPOIC ACID SOLUTIONS FOR REMOVAL OF ARSENIC AND MERCURY FROM MATERIALS USED FOR MUSEUM ARTIFACTS by Peggi S. Cross _________________________________ Copyright © Peggi S. Cross 2007 A Dissertation Submitted to the Faculty of the DEPARTMENT OF MATERIALS SCIENCE AND ENGINEERING In Partial Fulfillment of the Requirements For the degree of DOCTOR OF PHILOSOPHY In the Graduate College THE UNIVERSITY OF ARIZONA 2007 2 THE UNIVERSITY OF ARIZONA GRADUATE COLLEGE As members of the Dissertation Committee, we certify that we have read the dissertation prepared by Peggi S. Cross entitled Aqueous -Lipoic Acid Solutions for Removal of Arsenic and Mercury from Materials used for Museum Artifacts and recommend that it be accepted as fulfilling the dissertation requirement for the Degree of Doctor of Philosophy. __________________________________________________Date: 4-12-2007 Mark Riley __________________________________________________Date: 4-12-2007 David Lynch __________________________________________________Date: 4-12-2007 Nancy Odegaard __________________________________________________Date: 4-12-2007 Wendell Ela Final approval and acceptance of this dissertation is contingent upon the candidate’s submission of the final copies of the dissertation to the Graduate College. I hereby certify that I have read this dissertation prepared under my direction and recommend that it be accepted as fulfilling the dissertation requirement. __________________________________________________Date: 4-12-2007 Dissertation Director: Mark Riley 3 STATEMENT BY AUTHOR This dissertation has been submitted in partial fulfillment of requirements for an advanced degree at the University of Arizona and is deposited in the University Library to be made available to borrowers under rules of the Library. Brief quotations from this dissertation are allowable without special permission, provided that accurate acknowledgement of source is made. Requests for permission for extended quotation from or reproduction of this manuscript in whole or part may be granted by the copyright holder. SIGNED: Peggi S. Cross 4 ACKNOWLEDGEMENTS The work described in this dissertation was supported by a grant from the National Park Service and the National Center for Preservation Technology and Training. Its contents are solely the responsibility of the author and do not necessarily represent the official position or policies of the National Park Service or the National Center for Preservation Technology and Training. The author would like to thank Dr. Nancy Odegaard, Dr. Werner Zimmt, Dr. Mark Riley, Dr. Wendell Ela and Dr. David Lynch all of the University of Arizona for their support throughout the project as well as the following individuals who have provided inspiration and encouragement: my parents Cheri Cross-Bushnell, Ellis K. Cross and Asa Bushnell; Dr. Eric Betterton of the University of Arizona; and Dr. Timberly Roane of the University of Colorado. 5 DEDICATION This work is dedicated to the Native American people and to: James Patrick Marsh Jr. (May 18, 1961 – June 20, 2004) who left us at a very young age due to cancer from an unknown cause. My work is the translation of my sorrow. Of the many known carcinogens, arsenic is the one I decided to go after. I gave it my best shot, James. Bless you and all the beings who have suffered or are suffering. 6 TABLE OF CONTENTS LIST OF ILLUSTRATIONS..................................................................................................8 LIST OF TABLES…………………………………………………………………………14 ABSTRACT............................................................................................................... ……...16 1. INTRODUCTION....................................................................................................... .....18 2. HYPOTHESES.................................................................................................................20 3. BACKGROUND......................................................................................................... .....22 3.1 Pesticide contamination on museum artifacts...............................................................22 3.2 Arsenic and mercury toxicity........................................................................................24 3.3 American Indian use of objects ....................................................................................25 3.4 Existing processes for the removal of arsenic and mercury.........................................27 3.5 The structure of -lipoic acid........................................................................................29 3.6 The solvency of -lipoic acid and Reduced -lipoic acid ............................................31 3.7 Photochemical Reaction of -lipoic acid……………………………………………..33 3.8 The reaction of -lipoic acid and other chemicals with arsenic……………………...35 3.9 The reaction of -lipoic acid with mercury.............................................................. ....38 3.10 Sorption/Desorption properties of materials................................................................39 4. MATERIALS AND METHODS .....................................................................................41 4.1 Preparations of solutions...............................................................................................42 4.2 Photolysis of -lipoic acid............................................................................................43 4.3 Reaction of -lipoic acid with sodium arsenite or sodium arsenate.............................45 4.3.1 Equilibrium experiments……………………………………………………….45 4.3.2 Rate of Reaction..................................................................................................45 4.3.3 Effect of stirring rate and temperature................................................................44 4.3.4 Effects of the pH on the reaction rate.................................................................47 4.4 Quantification of –SH and H2S formation and extent of reduction..............................48 4.5 Analysis of material changes and residues using ATR-FTIR.......................................49 4.6 Selectivity of binding of reduced -lipoic acid to arsenite versus anions and cations...........................................................................................................................50 4.7 Preparation of test materials and sorption/desorption studies using XRF.....................51 4.7.1 Preparation of samples.........................................................................................51 4.7.2 Adsorption of arsenic and mercury onto materials..............................................51 4.7.3 Desorption of arsenic from materials using variable stirring rates and temperature..........................................................................................................52 4.7.4 X-ray Fluorescence Spectrometer........................................................................53 4.8 Decontamination of materials........................................................................................54 4.9 Analysis of material changes and residues using ATR-FTIR……………..…………..56 4.10 Analysis of the reaction of arsenic and treatment solutions with cotton wood root using ATR-FTIR..........................................................................................................57 7 TABLE OF CONTENTS (continued) 5. RESULTS AND DISCUSSION…………………………………………….…..………58 5.1 Solubility of -lipoic Acid……………………………………………….……..….. ...58 5.1.1 Solubility of organic solvent based solutions…………………………..….….…….58 5.1.2. Effect of acid/base concentration on solubility……………………………………...60 5.1.3. Reversibility of turbidity……………………………………...…….…….…………67 5.2 Photolysis of -lipoic Acid…………………………………………….….…….…. ...68 5.2.1 Acid/base effects on reduction rate ………………………………………….….....68 5.2.2 Effect of alcohol on reduction rate………………………..……….……….….…...74 5.2.3 The effect of reduction on the pH and solubility………………………………… ..78 5.2.4 Quantification of –SH formation and extent of reduction...................................... ..81 5.2.5 Effect of different light sources………………………………………..…..…….. ..83 5.2.6 Effect of temperature on the photolysis rate……………………………...………..85 5.3 Reaction of -lipoic acid with sodium arsenite and sodium arsenate in solution….....86 5.3.1 The reaction of As(III) with reduced lipoic acid.................................................... ..87 5.3.2 Effect of lipoic acid concentration on the reaction rate.......................................... ..90 5.3.3 Reaction rate control mechanisms.......................................................................... ..92 5.3.4 Diffusion control.......................................................................................................94 5.3.5 Chemical activation...............................................................................................
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