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Development of New Binding Phases for Speciation Measurements of Trace Metals with the Diffusive Gradients in Thin Films Technique

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Development of New Binding Phases for Speciation Measurements of Trace Metals with the Diffusive Gradients in Thin Films Technique Development of New Binding Phases for Speciation Measurements of Trace Metals with the Diffusive Gradients in Thin Films Technique Author Li, Weijia Published 2004 Thesis Type Thesis (PhD Doctorate) School School of Environmental and Applied Science DOI https://doi.org/10.25904/1912/2018 Copyright Statement The author owns the copyright in this thesis, unless stated otherwise. Downloaded from http://hdl.handle.net/10072/367741 Griffith Research Online https://research-repository.griffith.edu.au Development of New Binding Phases for Speciation Measurements of Trace Metals with the Diffusive Gradients in Thin Films Technique A thesis submitted in fulfilment of the requirements for the Degree of Doctor of Philosophy By WEIJIA LI School of Environmental and Applied Sciences Faculty of Environmental Sciences Griffith University Australia March 2004 CERTIFICATE OF ORIGINALITY I hereby declare that this submission is my own work and to the best of my knowledge it contains no materials previously published or written by another person, nor material which to a substantial extent has been accepted for the award of any other degree or diploma at Griffith University or any other educational institution, except where due acknowledgement is made in the thesis. Any contribution made to the research by others, with whom I have worked at Griffith University or elsewhere, is explicitly acknowledged in the thesis. I also declare that the intellectual content of this thesis is the product of my own work, except to the extent that assistance from others in the project’s design and conception or in style, presentation and linguistic expression is acknowledged. (signed)………………………. i ACKNOWLEDGEMENTS I wish to take this special opportunity to thank my supervisors, Dr. Huijun Zhao, Dr. Peter Teasdale and Dr. Richard John, for their support, patience and assistance through out the course of my period as a Ph.D. student. Thanks for invaluable ideas and guidance from Dr. Huijun Zhao. I wish to express my gratitude to School of Environmental and Applied Sciences, Griffith University, Australia for providing me with scholarship to undertake this project. Many thanks must also be given to head of the school, Clyde Wild, for his support; school secretary, Carmel Wild, for her English corrections of my thesis, and many other staff members in the School of Environmental and Applied Sciences for their help. I also thank to my research group, especially, Dr. Shangqing Zhang, Mr. Dianlu Jiang, Mr. Calvin Gladman, Miss Kylie Catterall, and Miss Kristy Morris, who have helped me in various ways. Thanks to staff members in the Chemistry Department, School of Molecular & Microbiological Sciences, University of Queensland for their help and assistance. I am deeply grateful my mother and father for their support and encouragement during the course of this study. Finally, I wish to thank my wife, Yali Qu, and my daughter, Mandy Li, for their great understanding, patience and assistance at any time. ii LIST OF PUBLICATIONS [1-7] [1] Li, W.; Teasdale, P. R.; Zhang, S.; John, R.; Zhao, H. Application of a Poly(4- styrenesulfonate) Liquid Binding Layer for Measurement of Cu2+ and Cd2+ with the Diffusive Gradients in Thin-Films Technique, Analytical Chemistry, 2003, 75, 2578-2583. [2] Li, W.; Zhao, H.; Teasdale, P. R.; John, R.; Zhang, S. Synthesis and characterisation of a polyacrylamide-polyacrylic acid copolymer hydrogel for environmental analysis of Cu and Cd, Reactive and Functional Polymers, 2002, 52, 31-41. [3] Li, W.; Zhao, H.; Teasdale, P. R.; John, R. Preparation and characterization of a poly(acrylamidoglycolic acid-co-acrylamide) hydrogel for selective binding of Cu2+ and application to diffusive gradients in thin films measurements, Polymer, 2002, 43, 4803-4809. [4] Li, W.; Zhao, H.; Teasdale, P. R.; John, R.; Zhang, S. Application of a cellulose phosphate ion exchange membrane as a binding phase in the diffusive gradients in thin films technique for measurement of trace metals, Analytica Chimica Acta, 2002, 464, 331-339. [5] Li, W.; Zhao, H.; Teasdale, P. R.; John, R. Application of new solid membrane diffusive layer/liquid binding phase DGT technique for environmental speciation, Environ. Sci. Technol., 2003, Submitted. [6] Li, W.; Zhao, H.; Teasdale, P. R.; John, R. Development of a new generation DGT technique using a solid membrane diffusive layer with a liquid binding phase, Analytica Chimica Acta, 2003, Submitted. iii [7] Li, W.; Zhao, H.; Teasdale, P. R.; John, R. Evaluation of new binding phases developed for use in diffusive gradients in thin films technique, Environ. Sci. Technol., 2003, Submitted. iv Table of Contents Certification………………………………………………………………………………...i Acknowledgement………………………………………………………………………….ii List of Publications………………………………………………………………………..iii Table of Contents…………………………………………………………………………..v Nomenclature……………………………………………...……………………………….x Abstract…………………………………………………………………………………...xii CHAPTER 1 General Introduction .............................................................................1 1.1. SIGNIFICANCE OF THIS RESEARCH...............................................................2 1.2. THE SPECIATION OF TRACE METALS IN NATURAL WATERS .................6 1.3. THE NEED FOR SPECIATION MEASUREMENTS OF TRACE METALS .....9 1.3.1. The Free-ion Activity Model ..........................................................................11 1.3.2. The Biotic Ligand Model................................................................................13 1.4. ISSUES TO CONSIDER WHEN SAMPLING AND MEASURING TRACE METAL SPECIES ..........................................................................................................16 1.4.1. Sampling Factors ...........................................................................................16 1.4.2. Measurement Factors .....................................................................................18 1.5. TECHNIQUES USED FOR IN SITU MEASUREMENT AND SPECIATION OF TRACE METALS ..........................................................................................................21 1.5.1. Diffusive Gradients in Thin Films (DGT) .....................................................23 1.6. OBJECTIVES OF THIS STUDY.........................................................................39 CHAPTER 2 Experimental and Methodology............................................................43 2.1. INTRODUCTION ..............................................................................................44 2.2. REAGENTS AND SOLUTIONS.......................................................................44 2.2.1. Chemicals and Materials.............................................................................44 2.2.2. Solutions .....................................................................................................45 2.3. PROCEDURES ..................................................................................................48 2.3.1. Preparation of Diffusive Gel.......................................................................48 2.3.2. Preparation of Chelex 100 Binding Gel......................................................49 2.3.3. Characterisation of the Structure and Composition of Binding Hydrogels 50 2.3.4. Assembling and Disassembling the Gel Based DGT Devices ...................50 2.3.5. Measurement of Diffusion Coefficient in Diffusive Layer ........................51 v 2.4. INSTRUMENTATION ......................................................................................53 2.4.1. Atomic Absorption Spectroscopy (AAS) ...................................................53 2.4.2. Measurement of Metal Concentrations in a Solution Containing PSS .......54 2.4.3. Solution pH Measurement ..........................................................................54 2.4.4. Solution Salinity Measurement...................................................................54 CHAPTER 3 Synthesis and Characterisation of a Poly(acrylamide-co-acrylic acid) Copolymer Hydrogel Based Binding Phase for the Diffusive Gradients in Thin Films (DGT) Technique ............................…………………………………………………………………………55 3.1 INTRODUCTION ..............................................................................................56 3.2 EXPERIMENTAL..............................................................................................59 3.2.1 Preparation of the Poly(acrylamide-co-acrylic acid) Copolymer Hydrogel 59 3.2.2 Characterisation of the Structure and Composition of the PAM-PAA Hydrogels....................................................................................................................59 3.2.3 Swelling Properties of the PAM-PAA Hydrogel........................................60 3.2.4 Metal Binding Properties of the PAM-PAA Hydrogel...............................60 3.2.5 Elution and Analysis of the Metal Ions ......................................................61 3.2.6 Validation of the PAM-PAA Hydrogel for Use with DGT ........................62 3.3 RESULTS AND DISCUSSION .........................................................................62 3.3.1 Preparation of the Poly(acrylamide-co-acrylic acid) Copolymer Hydrogel ... ....................................................................................................................62 3.3.2 Composition of the PAM-PAA Copolymer Hydrogel ...............................63 3.3.3 PAM-PAA Hydrogel Swelling Properties ..................................................66 3.3.4 Metal Binding Properties
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