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Zonation in Tourmaline from Granitic Pegmatites & the Occurrence of Tetrahedrally Coordinated Aluminum and Boron in Tourmaline

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Zonation in Tourmaline from Granitic Pegmatites & the Occurrence of Tetrahedrally Coordinated Aluminum and Boron in Tourmaline ZONATION IN TOURMALINE FROM GRANITIC PEGMATITES & THE OCCURRENCE OF TETRAHEDRALLY COORDINATED ALUMINUM AND BORON IN TOURMALINE by Aaron J. Lussier A Thesis submitted to the Faculty of Graduate Studies of The University of Manitoba in partial fulfilment of the requirements of the degree of DOCTOR OF PHILOSOPHY Department of Geological Sciences University of Manitoba Winnipeg Copyright © 2011 by Aaron J. Lussier ABSTRACT [1] Four specimens of zoned tourmaline from granitic pegmatites are characterised in detail, each having unusual compositional and/or morphologic features: (1) a crystal from Black Rapids Glacier, Alaska, showing a central pink zone of elbaite mantled by a thin rim of green liddicoatite; (2) a large (~25 cm) slab of Madagascar liddicoatite cut along (001) showing complex patterns of oscillatory zoning; and (3) a wheatsheaf and (4) a mushroom elbaite from Mogok, Myanmar, both showing extensive bifurcation of fibrous crystals originating from a central core crystal, and showing pronounced discontinuous colour zoning. Crystal chemistry and crystal structure of these samples are characterised by SREF, EMPA, and 11B and 27Al MAS NMR and Mössbauer spectroscopies. For each sample, compositional change, as a function of crystal growth, is characterised by EMPA traverses, and the total chemical variation is reduced to a series of linear substitution mechanisms. Of particular interest are substitutions accommodating the variation in [4]B: (1) TB + YAl ↔ TSi + Y(Fe, Mn)2+, where T Y T Y transition metals are present, and (2) B2 + Al ↔ Si2 + Li, where transition metals are absent. Integration of all data sets delineates constraints on melt evolution and crystal growth mechanisms. [2] Uncertainty has surrounded the occurrence of [4]Al and [4]B at the T-site in tourmaline, because B is difficult to quantify by EMPA and Al is typically assigned to the octahedral Y- and Z-sites. Although both [4]Al and [4]B have been shown to occur in natural tourmalines, it is not currently known how common these substituents are. Using 11B and 27Al MAS NMR spectroscopy, the presence of i [4]B and [4]Al is determined in fifty inclusion-free tourmalines of low transition- metal content with compositions corresponding to five different species. Chemical shifts of [4]B and [3]B in 11B spectra, and [4]Al and [6]Al in 27Al spectra, are well-resolved, allowing detection of very small (< ~0.1 apfu) amounts of T-site constituents. Results show that contents of 0.0 < [4]B, [4]Al < 0.5 apfu are common in tourmalines containing low amounts of paramagnetic species, and that all combinations of Si, Al and B occur in natural tourmalines. ii ACKNOWLEDGEMENTS I extend my most sincere gratitude to my advisor, Dr. Frank C. Hawthorne for granting me the opportunity to participate in the research that I have so- enjoyed, and for sharing his enthusiasm and insight into all things mineralogic and crystallographic. I would also like to express my appreciation to the members of my advisory committee: Drs. Norman M. Halden, Scott Kroeker, Elena Sokolova, and Mario Bieringer for their insightful comments over the past years; and to Dr. Lee A. Groat for agreeing to act as external examiner. I am very grateful to the members of the technical, research and support staff in the Department of Geological Sciences: Mr. M. A. Copper, Mr. N. Ball, Dr. Y. Abdu, Dr. P. Yang, Dr. R. Shidu, Mr. R. Chapman, Mr. S. Meijia, Dr. M. Schindler, Ms. D. Danyluk, Ms. Brenda Miller. I am particularly grateful to Mr. M. Cooper and Dr. M. Schindler for the many helpful conversations over the past years, and to Sasha Herwig for assistance with data X-ray data collection. I also thank C. Francis at the Mineralogical Museum at Harvard University for donating the Madagascar liddicoatite. I appreciate the collaborative support received from the MAS NMR lab in the Department of Chemistry at the University of Manitoba: Drs. S. Kroeker, P. M. Aguiar, and V. K. Michaelis. I also wish to thank Drs. R. C. Ewing and J. Zhang at the University of Michigan for access to, and assistance with, the TEM. I acknowledge financial support to me from: (1) the Natural Sciences and Engineering Council of Canada in the form of a PGS-D; (2) the University of Manitoba in the form of a Graduate Fellowship Award; and (3) The Province of Manitoba in the form of Manitoba Graduate Fellowship. I express great thanks to my wife, Kathryn Sexton, my mother, Eileen Lussier, and my father, Mark Lussier for their understanding, support, and patience over the years. iii For Kathy & Mom & Dad iv TABLE OF CONTENTS Abstract ………………………..………………………………………………… i Acknowledgements ………….………………………………………………… iii Dedication …………………….………………………………………………… iv Table of Contents …………….………………………………………………… v List of Tables …………………..………………………………………………… xv List of Figures ………….…….………………………………………………… xvii CHAPTER 1 INTRODUCTION 1.1 Tourmaline: towards a robust petrogenetic tool. …………………… 1 1.2 General formula and crystal structure ……………………………… 2 1.2.1 Space-group symmetry …………………………………….. 6 1.3 Tourmaline nomenclature and classification ……………………… 6 1.3.1 Tourmaline groups …………………………….…………… 7 1.3.2 Tourmaline species …………………………….…………… 9 1.3.3 Tourmaline classification …………………………………… 9 1.4 Selected physical properties of tourmaline ……………………… 16 1.4.1 Crystal form and habit …………………………………… 16 1.5 Selected optical properties of tourmaline ………………………… 17 1.5.1 Colour and colour zoning …………………..…………… 18 1.5.2 Important causes of colour …………………………… 19 v 1.6 Solid solutions in tourmaline ………………………………………… 20 1.7 Contribution of this work …………………………………………… 20 1.7.1 Review of tourmaline crystal chemistry ……………………. 20 1.7.2 Crystal chemistry of the T-site ……………………………… 21 1.7.3 Compositional zoning in tourmalines from granitic pegmatites …………………………….…………… 22 1.7.4 Note about publications ……………………………………… 23 CHAPTER 2 CRYSTAL CHEMISTRY OF CRYSTAL STRUCTURE 2.1 Introduction ………………………………….……………………… 24 2.2 Site populations and polyhedron geometry ……………………..… 25 2.2.1 The Z-site ………………………..………………………..… 26 2.2.1.1 Variation in <Y,Z-Φ> .......................………………… 29 2.2.1.2 Variation in <Z-Φ> …...................................………… 30 2.2.2 The Y-site ………………………………………………………. 34 2.2.2.1 Variation in <Y-Φ> …................................................… 35 2.2.2.2 Cation disorder between Y- and Z-octahedra ………… 40 2.2.2.3 Y-site vacancies ……………………………………….… 43 2.2.3 The T-site …………………………………………………….… 44 2.2.3.1 Variation in <T-O> …………….................................… 45 2.2.3.2. Fe3+ and the T-site …………………………………….. 47 2.2.4 The X-site ……………………………………………………..… 48 vi 2.2.4.1 Variation in <X-O> …………………………..…………… 48 2.2.5 The B-site …………………………………………………… 51 2.2.6 The O(1)-site ………………………………………..………... 51 2.2.6.1 The occurrence of F at O(1) ………………………….… 52 2.2.7 The O(3)-site ………………………………….………………… 53 2.3 Implications of short-range order around the O(1)-site ..………… 53 2.3.1 Bond-valence requirements at the O(1) site ………………………………………………..… 54 2.3.2 The stability of short-range clusters ………..……………… 54 2.3.1 O2- at the W-site: a cause of Y-Z disorder in tourmaline ………………………………………… 55 2.4 Short-range order around the O(3)-site ……………………… 56 CHAPTER 3 PHYSICAL DESCRIPTION OF TOURMALINE SAMPLES OF THIS WORK 3.1 Introduction ……………………………………………………………… 58 3.2 Oscillatory zoned liddicoatite from the Anjanabonoina Pegmatite, Madagascar …………………………………………………………… 58 3.2.1 Sample description ………………………………..………..… 58 3.2.2 Provenance ……………………………………….…………… 62 3.3 Mushroom and wheatsheaf tourmalines from Mogok, Myanmar ……………………………………………….. 63 3.3.1 Mushroom tourmaline: sample description ……..………… 63 vii 3.3.2 Wheatsheaf tourmaline: sample description …………..… 68 3.3.3 Provenance ………………………………………………..… 71 3.3 Elbaite-liddicoatite from Black Rapids Glacier, Alaska ………….… 72 3.3.1 Sample description ………………………………………… 72 3.3.2 Provenance ……………………………………………………. 72 CHAPTER 4 EXPERIMENTAL METHODS 4.1 Single-crystal X-ray diffraction ……………………………………….. 74 4.1.1 Collection of X-ray intensity data using a serial detector ………………………………………………… 74 4.1.2 Collection of X-ray intensity data using a CCD area detector ………………………………………..… 75 4.2 Crystal structure refinement …………………………………………. 75 4.3 Electron microprobe analysis ……………………………………… 77 4.3.1 EMP analysis of crystals used in singe-crystal, X-ray diffraction experiments ………………... 77 4.3.2 EMP analyses of NMR samples………………………………… 78 4.3.3 Compositional variation as a function of distance ……..… 78 4.4 27Al and 11B Magic Angle Spinning Nuclear Magnetic Resonance Spectroscopy ……………………………………………………..…… 79 4.4.1 High field 11B and 27Al MAS NMR spectra ………….…… 80 4.5 Mössbauer spectroscopy ……………………………………………… 80 viii 4.6 Calculation of structural formulae ……………………………….…… 81 4.7 Transmission electron microscopy …………………………….…… 82 4.8 Optical Mineralogy ……………………………………………..…… 82 CHAPTER 5 TETRAHEDRALLY COORDINATED Al AND B IN TOURMALINE: RESULTS OF A 11B AND 27Al MAS NMR STUDY 5.1 Introduction …………………………………………………………… 84 5.2 Detection of [4]B and [4]Al by conventional analysis …………..…… 85 5.2.1 Electron microprobe …………………………………….…… 85 5.2.2 Site-scattering REFinement (SREF) ………………………. 86 5.3 Previous work by MAS NMR ……………………………….…… 88 5.4 Samples ………………………………………………………..……… 89 5.5 11B MAS NMR …………………………………………….……… 93 5.6 27Al MAS NMR ………………………………………………………… 99 5.7 [4]Al in tourmaline …………………………………………………… 99 5.8 [6]Al in tourmaline ………………………………………….……… 103 5.9 The effect of paramagnetic constituents …………………..………… 104 5.10 The occurrence of tetrahedrally-coordinated constituents in
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