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Scandium Quantification in Selected Inorganic and Organometallic Compounds

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Scandium Quantification in Selected Inorganic and Organometallic Compounds SCANDIUM QUANTIFICATION IN SELECTED INORGANIC AND ORGANOMETALLIC COMPOUNDS by Hlengiwe Thandekile Mnculwane A thesis submitted in fulfilment of the requirements for the degree of Magister Scientiae In the Faculty of Natural & Agricultural Sciences Department of Chemistry University of the Free State Bloemfontein Supervisor: Prof. W. Purcell Co-Supervisor: Dr. J. Venter January 2016 Declaration by candidate I hereby declare that the dissertation submitted here for the degree of Master in Science at the University of the Free State is my own original work and has not been previously submitted for academic examination towards any qualification at any other University. I further declare that all the sources that I have used or quoted have been indicated and acknowledged by means of complete references. Signature...................................................... Date............................................. Hlengiwe Thandekile Mnculwane Acknowledgements I hereby wish to thank God for being with me up to thus far and each and every person who contributed, directly or indirectly, to the completion and success of this study: Firstly, I am indebted to my supervisor, Prof. W Purcell for giving me the opportunity to further my academic career by accepting me as part of the Analytical chemistry group and for the guidance and patience throughout my study. To my Co-supervisor, Dr. J. Venter, thank you so much for the review of my work and for the recommendations and suggestions which greatly improved my thesis writing. To my colleagues, Dr. M. Nete, Dr. T. Chiweshe, S. Xaba, D. Nhlapho, M. Zidge, Dr S. Kumar, G. Malefo, Q. Vilakazi and L. Ntoi, I would like to say thank you very much for being so helpful and for providing such a friendly environment that was also conducive to carry out my project, and to P. Nkoe thank you “skeem” stay cool. To all my friends, I want to thank you for the love, support and encouragement throughout my studies. I also wish to express my gratitude to my parents (Mrs T.B. Mnculwane and Mr J.J. Mnculwane), my siblings (Jabulisile, Nonhlanhla, Hlangabeza, Phendukani, Xolile and Sphephelo), and to Mnculwane family as a whole, thank you for the love and support from the onset of my studies. Special thanks to MINTEK for the financial assistance, you are highly acknowledged. Hlengiwe Thandekile Mnculwane TABLE OF CONTENTS LIST OF FIGURES ............................................................................................... .viii LIST OF TABLES ................................................................................................. .xii LIST OF ABBREVIATIONS ................................................................................. .xvii KEYWORDS ........................................................................................................ .xix Chapter 1: Motivation of the study .......................................................................... 1 1.1 Background of scandium .................................................................................. .1 1.2 Motivation of this study ..................................................................................... .7 1.3 Aim of the study ................................................................................................ .8 Chapter 2: Introduction ............................................................................................. 9 2.1 Introduction ....................................................................................................... .9 2.2 Discovery of scandium ...................................................................................... .9 2.3 Natural occurrence of scandium .................................................................... .11 2.4 Scandium production, market and beneficiation ............................................. .19 2.4.1 Scandium production ................................................................................. 19 2.4.2 Scandium market ...................................................................................... 26 2.4.2 Scandium beneficiation ............................................................................. 28 2.5 Applications and uses of scandium .................................................................. 32 2.6 Physical and chemical properties .................................................................... 35 2.6.1 Scandium crystallographic structure ......................................................... 37 2.7 Scandium chemistry ......................................................................................... 38 2.7.1 Scandium halides ...................................................................................... 39 2.7.2 Scandium oxide ......................................................................................... 40 2.7.3 Nitrate and sulphate chemistry of scandium .............................................. 41 2.7.4 Coordination chemistry .............................................................................. 41 2.8 Conclusion ....................................................................................................... 43 Chapter 3: Analytical techniques for dissolution, quantification and identification of scandium: Literature survey ................................... 44 3.1 Introduction ...................................................................................................... 44 Table of Contents 3.2 Dissolution and recovery of scandium in different scandium-bearing minerals…... ........................................................................................................... 45 3.2.1 Introduction ............................................................................................... 45 3.2.2 Conclusion ................................................................................................ 52 3.3 Analytical techniques for determination of scandium ....................................... 53 3.3.1 Introduction ............................................................................................... 53 3.3.2 Spectrophotometric techniques ................................................................. 54 3.3.2.1 Ultra Violet-Visible (UV-Vis) spectroscopy .......................................... 54 3.3.3 Inductively coupled plasma techniques ..................................................... 60 3.3.3.1 Inductively coupled plasma-optical emission spectrometry ................ 60 3.3.3.2 Inductively coupled plasma-mass spectrometry ................................. 65 3.3.4 Atomic absorption spectroscopy and neutron activation analyses ............ 68 3.3.5 Conclusion ................................................................................................ 69 3.4 Characterization of scandium complexes ........................................................ 70 3.4.1 Infrared (IR) ............................................................................................... 70 3.4.2 CHNS micro-elemental analysis ................................................................ 75 3.5 Conclusion ....................................................................................................... 76 Chapter 4: Selection of analytical techniques ...................................................... 78 4.1 Introduction ...................................................................................................... 78 4.2 Sample dissolution methods ............................................................................ 78 4.2.1 Open flask acid digestion .......................................................................... 79 4.2.2 Microwave-assisted digestion ................................................................... 81 4.2.3 Flux fusion dissolution ............................................................................... 84 4.3 Characterization techniques ............................................................................ 86 4.3.1 Infrared (IR) spectroscopy ......................................................................... 87 4.3.2 CHNS micro-analyser ................................................................................ 89 4.3.3 Melting point determination ....................................................................... 91 4.3.4 X-ray crystallography................................................................................. 92 4.4 Quantification techniques ................................................................................. 93 4.4.1 Inductively coupled plasma-optical emission spectrometry ....................... 94 4.4.1.1 Introduction ......................................................................................... 94 4.4.1.2 Instrumentation and principles of ICP-OES ........................................ 96 4.5 Separation and purification techniques .......................................................... 101 ii Table of Contents 4.5.1 Magnetic separation ................................................................................ 102 4.5.2 Solvent extraction .................................................................................... 103 4.6 Method validation ........................................................................................... 111 4.6.1 Accuracy ................................................................................................. 112 4.6.1.1 Absolute error (E) ............................................................................
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