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Radioanalytical Multi-Elemental Analysis: New Methodology and Archaeometric Applications

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Radioanalytical Multi-Elemental Analysis: New Methodology and Archaeometric Applications RADIOANALYTICAL MULTI-ELEMENTAL ANALYSIS: NEW METHODOLOGY AND ARCHAEOMETRIC APPLICATIONS ________________________________________________________________ A Dissertation presented to the Faculty of the Graduate Committee University of Missouri-Columbia In Partial Fulfillment of the Requirements for the Degree Doctor of Philosophy by Magen E. Coleman Dr. J. David Robertson, Dissertation Supervisor MAY 2010 © Copyright by Magen E. Coleman, 2010 All Rights Reserved The undersigned, appointed by the dean of the Graduate School, have examined the dissertation entitled: RADIOANALYTICAL MULTI-ELEMENTAL ANALYSIS: NEW METHODOLOGY AND ARCHAEOMETRIC APPLICATIONS Presented by Magen E. Coleman, a candidate for the degree of Doctor of Philosophy, and hereby certify that, in their opinion, it is worthy of acceptance. ____________________________________ Dr. J. David Robertson ____________________________________ Dr. Michael Glasscock ____________________________________ Dr. Silvia S. Jurisson ____________________________________ Dr. C. Michael Greenlief For my parents who always supported me no matter what I wanted to do; For my professors who believed that I could accomplish great things; For my friends, fellow graduate students, who helped me survive with my sanity (relatively) intact; And for Beau, who was always there to help, support, listen, and just love me. ACKNOWLEDGEMENTS First and foremost, I would like to thank my advisor, Dr. J. David Robertson. He took a chance on a student with no background in radiochemistry and challenged me to never accept mediocrity in my research. Without his patience and support, I would not have been able to achieve what I have: a Ph.D. in chemistry and a postdoctoral position at a national lab. His support of interdisciplinary research is remarkable and his teaching style is always inspiring. Secondly, I would like to thank Dr. Michael Glascock for introducing me to the field of archaeometry. He showed me a way to combine two of my greatest interests, history and chemistry, into one research project. His support was most helpful during my pursuit of this degree. I would also like to thank my other committee members, Dr. Silvia Jurisson and Dr. C. Michael Greenlief, for their time and patience these past four years. Dr. Jurisson helped me gain a firm understanding of the basics of radiochemistry in her course and helped me greatly when it came to being a teaching assistant for that class for the first time. Dr. Greenlief helped me gain a greater understanding of spectroscopy and its applications in his analytical courses. In addition to my committee members, there were many who helped me during the course of my research to gain a greater understanding of all of its aspects. First, I would like to thank Dr. John Simpson. He helped me better understand multivariate statistics and all the information I could get out of it. I would also like to thank Dr. Jeffrey Ferguson (MURR) and Dr. Stanley Ambrose (University of Illinois) for allowing me to not only work on the Kenyan obsidian samples, but also to go to Kenya and ii participate in the sample collection. That was truly a once-in-a-lifetime experience. I would also like to thank Dr. James Harrell of the University of Toledo for supplying the Egyptian limestone samples. Dr. Ellery Frahm of the University of Minnesota-Twin Cities performed electron microprobe analysis on several Mesoamerican obsidian samples for me and also helped me gain a better understanding of the analysis technique. The Archaeometry Group at MURR, both past and present members, provided a lot of help and support when working in the lab, especially for sample preparation and the actual analysis of the samples. The Robertson research group in the Chemistry Department was a constant source of support during these four years. It is truly inspiring to work with so many amazing chemists. Lastly I would like to thank the Chemistry Department and the National Science Foundation for the financial support needed in order to complete these studies. iii Table of Contents Acknowledgments ii List of Figures viii List of Tables xi Abstract xii Chapter 1: Multi-elemental Analysis and Archaeometry 1 1.1 Introduction 1 1.2 X-ray fluorescence 3 1.2.1 XRF instruments 6 1.2.2 Basic principles of XRF analysis 7 1.2.3 XRF analysis at MURR 13 1.3 Neutron activation analysis 14 1.3.1 A brief overview of NAA 15 1.3.2 Types of NAA 16 1.3.3 Basic principles of NAA 18 1.3.4 Gamma spectroscopy and quantitative analysis 21 1.3.5 Potential interferences 23 1.3.6 NAA at MURR 25 1.4 Comparison of XRF and NAA 29 Chapter 1 References 31 Chapter 2: Statistical Methods of Data Analysis and Their Application to Provenance 32 Studies 2.1 Introduction 32 2.2 Statistics in archaeometry 32 2.3 Standardization of data 35 2.4 Multivariate statistics 36 2.4.1 Variance, covariance, and correlation 37 2.4.2 Distance measurements and clustering methods 38 iv 2.4.3 Principal component analysis 46 2.5 Conclusion 55 Chapter 2 References 56 Chapter 3: Sourcing Egyptian Limestone 57 3.1 Introduction 57 3.1.1 The geology of limestone 58 3.1.2 Limestone sourcing studies 59 3.1.3 The current project 62 3.2 Methodology 62 3.3 Statistical results and interpretation 63 3.3.1 The BNL samples 63 3.3.2 Samples from Dr. Harrell 71 3.4 Conclusions and future work 81 Chapter 3 References 82 Chapter 4: Sourcing Obsidian from Kenya Using Neutron Activation Analysis 83 4.1 Introduction 83 4.1.1 Obsidian: a brief overview 83 4.1.1.1 Formation of obsidian 84 4.1.1.2 Composition of obsidian 84 4.1.2 African obsidian and anthropological implications 86 4.1.3 Current project 89 4.2 Experimental methods 89 4.3 PCA results 92 4.4 Characterizing geological source groups using elemental bivariate plots 96 4.5 Conclusions 108 Chapter 4 References 109 v Chapter 5: A New Epithermal Neutron Activation Analysis Method for Titanium and 110 Barium Analysis in Obsidian 5.1 Introduction 110 5.1.1 The challenge 110 5.2 Development of the new methodology 113 5.2.1 Titanium 114 5.2.2 Barium 117 5.3 Initial Experiments 118 5.3.1 Standards and samples 118 5.3.2 Irradiation, decay, and counting procedures 119 5.3.3 Gamma spectra and determination of precision and limits of detection 119 5.3.3.1 Titanium results 121 5.3.3.2 Barium results 124 5.4 Other elements of interest 125 5.4.1 Arsenic analysis 126 5.4.1.1 Neutron capture of arsenic 126 5.4.1.2 Is the peak really due to arsenic? 127 5.4.1.3 Arsenic results 130 5.4.2 Bromine analysis 131 5.4.2.1 Neutron capture reactions of bromine 132 5.4.2.2 Br-82 decay test 133 5.4.2.3 Bromine results 134 5.5 Comparison of results from ENAA and X-ray methods 135 5.5.1 Results from the Mesoamerican obsidian samples 136 5.5.2 Results from the African obsidian samples 137 5.6 Future work and conclusions 139 5.6.1 Analysis of arsenic in biological samples 140 5.6.2 An alternative method for standard INAA procedures 140 5.6.3 Conclusions 142 Chapter 5 References 143 vi List of Appendices 144 Appendix 1 - Limestone quarry information for the BNL Egyptian limestone 145 samples Appendix 2 - Concentration data from NAA for limestone from Egypt (BNL 147 samples) Appendix 3 - Limestone source information for the Harrell Egyptian limestone 157 samples Appendix 4 - Concentration data from NAA for limestone from Egypt (Harrell 159 samples) Appendix 5 - Geographical data for African obsidian samples from Kenya 169 Appendix 6 - Concentration data from NAA for obsidian from Kenya 182 Appendix 7 - Results of concentration calculations for the standards analyzed for 230 both the standard INAA procedure and the new ENAA procedure for titanium. Appendix 8 - Results of concentration calculations for the standards analyzed for 231 both the standard INAA procedure and the new ENAA procedure for barium. Appendix 9 - Results of concentration calculations for the standards analyzed for 232 the new ENAA procedure for arsenic after both a 7-day and 5-day decay. Vita 233 vii List of Figures Figure 1.1: Illustration of X-ray fluorescence 4 Figure 1.2: Electronic transitions in the atom for characteristic X-ray lines 9 Figure 1.3: XRF spectrum of obsidian 13 Figure 1.4: Neutron Activation Analysis 15 Figure 1.5: Gamma spectrum acquired from NIST SRM 278 (obsidian) 21 Figure 2.1: City-block distance 39 Figure 2.2: Euclidean Distance 40 Figure 2.3: Dendrogram of the standardized sample data set (Table 2.1) using 43 average linkage Figure 2.4: Dendrogram of the standardized sample data set (Table 2.1) using 44 Ward’s linkage Figure 2.5(A): Scree plot from PCA results of the standardized sample data set 49 (Table 2.1): Eigenvalues vs. PCs Figure 2.5(B): Scree plot from PCA results of the standardized sample data set 50 (Table 2.1): % Variance vs. PCs Figure 2.6: Loadings plot from PCA results of the standardized sample data set 51 (Table 2.1) Figure 2.7: Loadings vector plot from PCA results of the standardized sample data 52 set (Table 2.1) Figure 2.8: Scores plot from PCA results of the standardized sample data set (Table 53 2.1) Figure 2.9: Plot of scores and loadings vectors from PCA results of the standardized 54 sample data set (Table 2.1) Figure 3.1: Map of sampled quarry locations in Egypt (BNL samples) 64 Figure 3.2: Dendrogram resulting from hierarchical cluster analysis of Egyptian 65 limestone samples (BNL samples) Figure 3.3a: Loadings bar plot for Egyptian limestone samples (BNL samples) 68 Figure 3.3b: Loadings bar plot for Egyptian limestone samples (BNL samples) 68 Figure 3.4: Plot of PC2 vs.
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