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Synthesis and Characterization of Strontium Fluorapatite

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Synthesis and Characterization of Strontium Fluorapatite UNLV Retrospective Theses & Dissertations 1-1-2005 Synthesis and characterization of strontium fluorapatite Chirantha Prageeth Rodrigo University of Nevada, Las Vegas Follow this and additional works at: https://digitalscholarship.unlv.edu/rtds Repository Citation Rodrigo, Chirantha Prageeth, "Synthesis and characterization of strontium fluorapatite" (2005). UNLV Retrospective Theses & Dissertations. 1813. http://dx.doi.org/10.25669/mwff-o6ha This Thesis is protected by copyright and/or related rights. It has been brought to you by Digital Scholarship@UNLV with permission from the rights-holder(s). You are free to use this Thesis in any way that is permitted by the copyright and related rights legislation that applies to your use. For other uses you need to obtain permission from the rights-holder(s) directly, unless additional rights are indicated by a Creative Commons license in the record and/ or on the work itself. This Thesis has been accepted for inclusion in UNLV Retrospective Theses & Dissertations by an authorized administrator of Digital Scholarship@UNLV. For more information, please contact [email protected]. SYNTHESIS AND CHARACTERIZATION OF STRONTIUM FLUORAPATITE by Chirantha Prageeth Rodrigo Bachelor of Science University of Colombo, Sri Lanka 2001 A thesis submitted in partial fulfillment of the requirements for the Master of Science Degree in Chemistry Department of Chemistry College of Sciences Graduate College University of Nevada, Las Vegas August 2005 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. UMI Number: 1428601 INFORMATION TO USERS The quality of this reproduction is dependent upon the quality of the copy submitted. Broken or indistinct print, colored or poor quality illustrations and photographs, print bleed-through, substandard margins, and improper alignment can adversely affect reproduction. In the unlikely event that the author did not send a complete manuscript and there are missing pages, these will be noted. Also, if unauthorized copyright material had to be removed, a note will indicate the deletion. UMI UMI Microform 1428601 Copyright 2005 by ProQuest Information and Learning Company. All rights reserved. This microform edition is protected against unauthorized copying under Title 17, United States Code. ProQuest Information and Learning Company 300 North Zeeb Road P.O. Box 1346 Ann Arbor, Ml 48106-1346 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Thesis Approval The Graduate College University of Nevada, Las Vegas th June 9 ■ 20 05 The Thesis prepared by CHIRANTHA PRAGEETH RODRIGO Entitled SYNTHESIS AND CHARACTERIZATION OF STRONTIUM FLUORAPATITE is approved in partial fulfillment of the requirements for the degree of MASTER OF SCIENCE Examination Committee Chair Dean of the Graduate College Examination Committee Member Examination Committee Member r i ^ L L h r O _________________ _ Graduate College Faculty Representative 11 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. ABSTRACT Synthesis and Characterization of Strontium Fluorapatite by Chirantha Prageeth Rodrigo Dr. Dennis W. Lindle, Examination Committee Chair Professor of Chemistry University of Nevada, Las Vegas Proliferation of nuclear waste is a major environmental issue we all face this century. Long lived radioactive isotopes such as ^^Sr contained in spent nuclear fuel have been causing major problems during the disposal stage of the nuclear fuel cycle. Disposal of radioactive isotopes requires a suitable confinement host material in order to dispose of them in a safe and appropriate repository. In this thesis I describe how to synthesize and characterize the mineral fluorapatite as a host material for Sr. Fluorapatite is a naturally occurring mineral with the unit cell formula of Caio(P 0 4 )6 p 2 . This mineral possesses a stable hexagonal crystal structure and has the natural ability to accommodate foreign cations in its structure. Pure fluorapatite and varying amounts of strontium-bearing fluorapatite were synthesized by using wet chemical synthesis methods. Products of the synthesis were confirmed by using x-ray powder diffraction analysis. Increasing lattice dimensions were observed with increasing strontium concentration. The hydroxyl stretching band in the 111 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. infrared spectra further established the formation of fluorapatite in all synthetic products. It was observed that the strontium substitutions at the Ca sites have influenced the hydroxyl stretching frequency of strontium containing fluorapatite samples. The stretching and bending modes of the phosphate groups have also been slightly affected by Sr^"^ insertion but have not changed the basic fluorapatite structure. SEM images of the annealed fluorapatite samples also verify the formation of hexagonal crystals. IV Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. TABLE OF CONTENTS ABSTRACT..................................................................................................................................iii LIST OF FIGURES....................................................................................................................vii LIST OF TABLES................................................................................................... ix ACKNOWLEDGEMENTS.........................................................................................................x CHAPTER 1 INTRODUCTION.................................................................................................1 1.1 Introduction to nuclear waste ....................................................................................1 1.2 Waste form materials ................................................................................................ 2 1.3 Fluorapatite Mineral ...................................................................................................3 1.4 Review on methods of apatite synthesis .................................................................8 1.5 Electronic structure of fluorapatite ..........................................................................8 1. 6 Research goals ......................................................................................................... 11 1.7 References ................................................................................................................. 13 CHAPTER 2 EXPERIMENTAL...............................................................................................15 2.1 Introduction .................................................................................... 15 2.2 Synthesis of fluorapatite .........................................................................................15 2.3 Characterization of fluorapatite samples ............................................................. 20 2.4 References .................................................................................................................22 CHAPTER 3 RESULTS AND DISCUSSION....................................................................... 23 3.1 Introduction...............................................................................................................23 3.2 Synthesis of apatite and X-ray diffraction studies ..............................................23 3.3 FT-IR spectroscopy ................................................................................................. 30 3.4 Raman scattering spectroscopy ..............................................................................39 3.5 Scanning electron microscopic studies .................................................................42 3.6 References .................................................................................................................49 CHAPTER 4 CONCLUSIONS................................................................................................ 50 APPENDIX I POWDER XRD DATA.................................................................................... 52 APPENDIX II FTIR SPECTRAL DATA ................. 56 APPENDIX III RAMAN SCATTERING SPECTRA.......................................................... 59 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. VITA............................................................................................................................................. 63 VI Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. LIST OF FIGURES 1.1 Computer generated unit cell of fluorapatite with PowderCell 2.4v software ......... 5 1.2 Three dimensional view of the two Ca sites .................................................................. 5 1.3 (a) Natural fluorapatite (b) natural rock sample from Siberia (c) synthetic fluorapatite fi*om Russia ...................................................................................................6 1.4 Infrared spectra of Hydroxyl stretching region of the apatite compounds .............. 10 2.1 UNEV Fluorapatite synthesis apparatus .......................................................................17 2.2 Synthetic fluorapatite from KRI institute, Russia ........................................................19 3.1 X-ray powder diffraction patterns
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