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The Crystal Chemistry of Gorceixite, Grandidierite, and Traskite with The

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The Crystal Chemistry of Gorceixite, Grandidierite, and Traskite with The THE CRYSTAL CHEMISTRY OF GORCEIXITE, GRANDIDIERITE, AND TRASKITE by TASHIA JAYNE DZIKOWSKI B.Sc, The University of Manitoba, 2004 A THESIS SUBMITTED IN PARTIAL FULFILLMENT OF THE REQUIREMENTS FOR THE DEGREE OF MASTER OF SCIENCE in THE FACULTY OF GRADUATE STUDIES ^Geological Sciences^ THE UNIVERSITY OF BRITISH COLUMBIA August 2006 © Tashia Jayne Dzikowski, 2006 ABSTRACT This thesis reinvestigates the crystal structures of gorceixite and traskite, and the geometric effects of vFe2+ for vMg substitution on the crystal structures of the grandidierite- ominelite series. All data was measured using using MoKa radiation on an automated Bruker X8 single-crystal diffractometer with a SMART APEX CCD (charge coupled device) detector. The crystal structure of gorcexite (BaAl3(P030,OH)2(OH6), a 7.0538(3), c 17.2746(6) A, V 744.4(2) A3, space group R 3m, Z=3, has been refined to an R] index of 2.3% based on 253 unique reflections. The results indicate that this specimen has rhombohedral rather than monoclinic Cm symmetry as was previously reported for the species. The crystal-structure refinement shows that the atomic arrangement of gorceixite is similar to that of other members of the plumbogummite group. The chemical compositions and crystal structures of seven members of the grandidierite- 2+ 2+ 2+ ominelite (MgAl3BSi09-Fe Al3BSi09) series withX- (Fe + Mn + Zn)/(Fe + Mn + Zn + Mg) ranging from 0.00 to 0.52 were studied to determine the geometric effects of Fe substitution for Mg on the crystal structures. Regression equations derived from single-crystal X-ray diffraction data show that b increases by 0.18 for the range X= 0-1. The crystal structure refinements show that the most significant changes involve the (Mg,Fe )05 polyhedron, which increases in volume by 0.36 A3 (5.0%), largely as a result of expansion of the MgFe-05, -02, and -06 (x2) bond distances, which increase by 0.09 (4.4%), 0.06, and 0.04 A, respectively. Numerous space groups were tried in an attempt to solve and refine the crystal structure 2+ of the traskite (Ba9Fe 2Ti2(Si03)i2(F,Cl,OH)6-6H20. The most successful was P3\m, with a 17.863(3), c 12.298(3) A, and Z = 3. The Rm = 5.3% and R{ = 5.3% values indicate that the data are good and that the model is close to being correct; however, split Ba, O, and CI sites indicate that there are missing symmetry elements within the structure. Attempts to refine the structure in P6/mmm, which contains the supposed missing symmetry elements, were unsuccessful. ii TABLE OF CONTENTS ABSTRACT ii TABLE OF CONTENTS ; iii LIST OF TABLES. v LIST OF FIGURES vi ACKNOWLEDGEMENTS vii 1.0 INTRODUCTION 1 2.0 GORCEIXITE 2 2.1 Introduction 2 2.2 Experimental 4 2.3 Results 7 2.4 Discussion 17 3.0 GRANDIDIERITE 18 3.1 Introduction 18 3.2 Background 18 3.3 Experimental 22 3.4 Results 27 3.4.1 Electron microprobe analyses 27 3.4.2 Unit cell parameters 40 3.4.3 Bond distances 40 3.4.4 Bond angles 44 3.4.5 Polyhedral edges 48 3.4.6 Polyhedral volumes and distortion parameters 52 3.4.7 Summary 52 iii 3.5 Discussion 54 3.5.1 Unit-cell parameters 54 3.5.2 Geometric effects 55 3.5.3 Effect of other substituents 57 3.5.4 Ionic radius of vFe2+ 58 3.5.6 Conclusion: vFe in minerals 58 4.0 TRASKITE 60 4.1 Introduction 60 4.2 Experimental 60 4.3 Results and Discussion 62 REFERENCES 72 APPENDIX A.l Commonly used symbols and terms 80 iv LIST OF TABLES 2.1 Electron-microprobe composition of the gorceixite single-crystal used in this study.... 5 2.2 Gorceixite: Data collection and structure refinement information 8 3.3 Atom parameters for gorceixite 9 3.4 Selected interatomic distances (A) and angles (°) for gorceixite 10 3.5 Bond valence analysis of gorceixite 13 3.6 Sample information for grandidierite and ominelite 23 3.7 Average electron-microprobe compositions of grandidierite and ominelite crystals used in the single-crystal X-ray diffraction study 25 3.8 Data measurement and refinement information for grandidierite and ominelite 28 3.9 Atomic parameters for grandidierite and ominelite 29 3.10 Atomic displacement parameters for grandidierite and ominelite 31 3.11 Interatomic distances (A) and angles (°) for grandidierite and ominelite 34 3.12 Polyhedral edges (A) for grandidierite and ominelite 37 3.13 Polyhedral volumes and distortion parameters for grandidierite and ominelite 39 4.1 Electron microprobe analyses of traskite 63 4.2 Attempted space groups and resulting Flack x parameters, and |E -1| values of traskite 66 4.3 Traskite: Data collection and structure refinement information 66 4.4 Atom parameters for traskite 67 4.5 Selected interatomic distances (A) for traskite 69 4.6 Selected interatomic angles (°) for traskite ...71 v LIST OF FIGURES 2.1 Coordination polyhedra of cations in the gorceixite structure 11 2.2 The gorceixite structure projected onto (a) (100) and (b) (001) 16 3.1 Projection of the crystal structure of grandidierite and ominelite onto (001) 20 3.2 Coordination polyhedra for the cations in the grandidierite-ominelite structure 21 3.3 (Fe2+ + Mn + Zn)/(Fe2+ + Mn + Zn + Mg) vs. (a) a, (b) b, (c) c, (d) Ffor grandidierite and ominelite 41 3.4 (Fe2+ + Mn + Zn)/(Fe2+ + Mn + Zn + Mg) vs. (a) MgFe-05a, (b) MgFe-02, (c) MgFe-06 x 2 for grandidierite and ominelite 42 3.5 (Fe2+ + Mn + Zn)/(Fe2+ + Mn + Zn + Mg) vs. (a)All-06 x 2; (b) A12-04 x 2; (c) A12-07f x 2 (squares), -05c x 2 (triangles) for grandidierite and ominelite 43 3.6 (Fe2+ + Mn + Zn)/(Fe2+ + Mn + Zn + Mg) vs. (a) Ol-MgFe-02 (squares), 06-MgFe-06b (triangles); (b) Ol-MgFe-06 x 2; (c) 02-MgFe-06 x 2 (squares), 01-MgFe-05a (triangles); and (d) 02-MgFe-05a for grandidierite and ominelite 45 3.7 (Fe2+ + Mn + Zn)/(Fe2+ + Mn + Zn + Mg) vs. (a) 06-A11-02 x 2 (squares), -02d x 2 (triangles); (b) 01-A13-05a (squares), -02i (triangles) for grandidierite and ominelite 46 3.8 (Fe2+ + Mn + Zn)/(Fe2+ + Mn + Zn + Mg) vs. (a) 04-Si-06j x 2 (squares), -Ol (triangles); (b) 06j-Si-06f (squares), -Ol x 2 (triangles) for grandidierite and ominelite 47 2+ 2+ 2+ 3.9 (Fe + Mn + Zn)/(Fe + Mn + Zn + Mg) vs. (Mg,Fe )05 polyhedral edges: (a) 02-06 x 2 (squares), 01-05a (triangles); (b) 06-05a x 2 (squares), -6b (triangles); (c) 01-02 (squares), -06 x 2 (triangles) 49 3.10 (Fe2+ + Mn + Zn)/(Fe2+ + Mn + Zn + Mg) vs. polyhedral edges: (a) A1106, 06-02d x 2; (b) A1206, 07f-04h x 2 (squares), -04 x 2 (triangles); (c) A1305, 02i-01 50 2+ 2+ 3.11 (Fe + Mn + Zn)/(Fe + Mn + Zn + Mg) vs. Si04 tetrahedral edges, 04-06 x 2 51 3.12 (Fe2+ + Mn + Zn)/(Fe2+ + Mn + Zn + Mg) vs. (a) volume of the (Mg,Fe2+)05 (squares) and A130s (triangles) polyhedra, (b) volume of the All06 (squares) and A1206 (triangles) octahedra, (c) tetrahedral angle variance for Si04 tetrahedron in grandidierite and ominelite 53 4.1 Structure of traskite projected down (001) 61 vi ACKNOWLEDGEMENTS I would like to thank Prof. Lee A. Groat for suggesting this project, always being there to listen, discussing and solving mineralogical problems with me, spending endless hours helping me write and edit, collecting data when I could not, and giving me the opportunity to move to Vancouver where I have experienced the most amazing time of my life. I would also like to thank Edward S. Grew and John A. Jambor for their contribution to my work with grandidierite and gorceixite. In addition, I would like to thank Colin Fyfe and Mati Raudsepp for serving on my committee. I would not have been able to collect electron microprobe data without the help of Mati Raudsepp nor would I have been able to collect X-ray diffraction data without the help of Anita Lam and Brian Patrick. I would also like the thank Anita and Brian for all of their help with interpreting my results. I would also like to thank Allison Brand for helping prepare and revise my manuscripts. My last two years have gone so smoothly in part because of Alex Allen's assistance with graduate affairs. I would also like to thank my dear friends Jen, Laura, Megan, Victoria, and Tanya. Your support and friendship over the years means so much to me. I would also like to thank my family for encouraging me to always do my best and to set my goals high. I would not be here without you. Support for this project was provided by NSERC operating grants to Lee A. Groat. Personal financial support was provided by a Post-Graduate Masters and a Canada Graduate Scholarship Masters NSERC as well as the University of British Columbia in the form of scholarships and teaching assistantships. vii 1.0 INTRODUCTION Here I reinvestigate the crystal structures of gorceixite and traskite, and the geometric effects of vFe2+ for vMg substitution on the crystal structures of the grandidierite-ominelite series. For data collection I used a Bruker X8 single crystal X-ray diffractometer with a SMART APEX CCD (charge coupled device) detector in the Center for Higher Order Structure Elucidation (C-HORSE) lab at the University of British Columbia. I was the first to use this instrument this instrument to examine the crystal structures of minerals.
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