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I Doctor of Philosophy Department Of. Geology, University of Sheffield THE GEOCHEMISTRY AND MINERALOGY OF COAL AND COAL-BEARING STRATA FROM THE CANNOCK COALFIELD WITH SPECIAL REFERENCE TO CHLORINE VOLUME 1 STEPHEN ALLEN CASWELL I Submitted in fulfilment of the requirements for the degree of Doctor of Philosophy Department of. Geology, University of Sheffield. January, 1983. fi SUMMARY (i) The Geochemistry and Mineralogy of Coal and Coal-Bearing Strata from the Cannock Coalfield with Specific Reference to Chlorine The project was conducted on four coals seams, the Shallow and Yard (Lower Coal Measures) from Lea Hall Colliery at Rugeley, and the Park and-Eight Feet seams from Littleton Colliery, near Cannock. Ultimate, proximate analyses and moisture contents showed them to be of high volatile bituminous 'B' coal-rank, and typical of high Cl coals. The Cl investigation showed a relationship with organic matter where ash is a dilutant, reaching c. 1% (by weight) in the coals, almost an order higher than in the associated mudrocks. It is related to the internal surface area and is thus highest in the vitrinite dominated 'bright rocks' and lowest in the 'dull coals'. Two types of Cl were identified, originating from saline ground waters, the former representing present ground water solutions trapped in the larger pores and readily water-soluble, and the latter held in organic combination within smaller or closed pores produced by Hercynian rank imposition. Varying levels of this Cl can be released by ion exchange with carbonates in leaching experiments. The mudrock and coal ash mineralogy was conducted on low temperature ashed material which suffered the side-effect of gypsum formation during oxidation. The mudrock mineralogy is dominated by detrital minerals, quartz and clays predominating. Diagenetic minerals"rarely account for 7% of the normative minerals except in localised pyrite and siderite nodules., Climate played an important role in the detrital mineralogy, the lower seam floor measures being dominated by a tropically leached suite of kaolinite and quartz. Continental movement led to increased aridity characterised by illite and chlorite which dominate the higher seams. The intraseam dirt bands are composed of very fine clays, rapidly deposited over wide areas by minor base-level changes or river (ii) bank bursts. The roof measures show least evidence of leaching and are often highest in diagenetic siderite. Ba, Sr, Rb (illite) and Zr (zircon) are predominantly detrital trace elements whilst oxyhydroxide material was-the transporting media. for the diagenetically located elements, Ni, Pb (pyrite), Co and Mn (siderite). Cu is primarily associated with organic matter. The detrital coal mineralogy reflects the fine mudrock material and is usually highest associated with the dirt bands. Diagenetic minerals dominate the ash, reaching 95% (by weight), the major component being late diagenetic cleat. A paragenetic sequence of mineralisation follows a widespread trend from sulphides, silicates to carbonates reflecting changing ground water composition. The cleat fractures represent micro- jointing produced with stress release during uplift. Its frequence decreases with bed thickness, and the brittle nature of vitrinite causes it to have the earliest formed and most abundant cleat. The strength of multimaceral lithotypes such as durain is much greater and therefore fracture least, later änd with a greater dilation. F.. _-,. ý a. ,. ýý re (iii) ACKNOWLEDGEMENTS This research project was undertaken with the financial support of a C. A. S. E. Award sponsored by the Central Electricity Generating Board (C. E. R. L., Leatherhead) and the Natural Environmental Research Council and to these establishments my appreciation is gratefully acknowledged. To the following I extend my thanks: - Dr. D. A. Spears, as my supervisor at Sheffield University, for many fruitful discussions and much encouragement; Dr. C. D. Curtis, as my temporary supervisor and for showing continued interest in my project; Dr. J. Bettelheim (external supervisor) and Dr. K. G. Saunders of the C. E. R. L., for their continued interest, help and access to C. E. R. L. data; Mr. J. H. Atkin (Chief Scientific Officer, Western Division) and Mr. R. H. Hoare (Chief Geologist, Western Division) of the N. C. B. who arranged for my underground visits and for technical information. Mr. T. Halker and Mr. K. Whitworth (N. C. B. geologists) in their help during sample collection; Mr. K. Kendal (C. E. G. B. ) for conducting ultimate and proximate analyses on my coal samples; Mr. E. Hall (Water Research Centre) for high speed centrifuging of coal samples; Dr. I. F. Holmes, in close co-operation and discussions in the Chlorine study; Dr. R. Kanaris-Sotiriou, for his help in X-ray techniques; Dr. N. J. Soper, for discussions on joint formation; Mr. V. A. Somogyi, Mr. A. Saxby and Mrs. S. M. Rhodes in helping a non-chemist in wet chemical analysis; Mr. H. Brockley, in T. E. M. microscopy and preparation; Mr. M. G. Cooper, for help and instruction in the art of cartography and the Appendix diagrams. Mr. G. Mulhearn, for thin section preparation; Mr. B. Piggott, for. help in photographic matters; Mr. S. T. Reynolds,. for trace element analysis and discussion in the follow-up to this work thesis; Mr. A. Sheldon (Department of Metallurgy)', for S. E. M. operation . (iv) Finally, but not least, to the secretaries who suffered from my protracted pestering during typing, without whom this thesis would not have been completed: - Miss S. Forster; Miss P. M. Mellor; Mrs. M. Townsend and Mrs. B. M. Wilson. .t'4 (V) VOLUME 1 LIST OF CONTENTS page number SUMMARY i ACKNOWLEDGEMENTS iii LIST OF CONTENTS V CHAPTER 1 INTRODUCTION 1 Sample Locations 2 Sampling Scheme 5 Coal Sample Description 6 Mudrocks 9 Mudrock Colour 11 Sample Numbering 12 Coal Analysis 14 Classification of Coal by Rank 17 Macroscopic Seam Sections and Formation Curves 18 CHAPTER 2 REGIONAL GEOLOGY - THE CANNOCK COALFIELD 21 General 21 The South Staffordshire Coalfield and its Extensions 22 Stratigraphy 23 Igneous Intrusions 31 Structure 32 CHAPTER 3 WATER-SOLUBLE ELEMENTS IN COAL AND ASSOCIATED STRATA 34 Section 1 LEACHING EXPERIMENTS 36 (vi) Page Number Preliminary Studies 36 Water-soluble Leaching Experiments 37 30-72 B. S. S. Mesh Fraction-Eight Feet Seam 37 150-200 B. S. S. Mesh Coal 40 Tema Coal 41 Seam Profiles 41 Conclusions 43 Section 2 DIFFUSION STUDY 45 Theory of Diffusion 46 Eight Feet Seam - Diffusion Experiments 48 Conclusions 52 Section 3 TEMA GROUND ANALYSIS OF WATER-SOLUBLE ELEMENTS 53 Method 53 Discussion of Seam Profiles 55 Element Distribution within Seam Profiles 57 Sodium 57 Potassium 60 Calcium 61 Magnesium 62 Bicarbonate 63 Hydrogen - ion Activity 65 Sulphate 66 Chlorine 68 CHAPTER 4 TOTAL CHLORINE 73 The Origin of Chlorine 73 Nature of Chlorine in Coal 74 Chlorine Distribution 75 Variation with Rank 75 Variation with Depth 77 (vii) Page Number Small Scale Local Variations 78 Within Seam Variations 78 Association with Coal Types 78 Mode and Time of Chlorine Introduction 79 Peat Growth 79 During Deposition 79 Diagenetic Alteration of Ground Waters 80 Total Cl Profiles, Lea Hall and Littleton Collieries 82 Discussion of Profiles 82 The Influence of very Saline Ground Waters- an overriding example. 87 Total Cl and Depth 89 Prediction of Cl Leaching Levels 89 Influence of Ground Water on Leachable Cl 90 Location of Cl in Coal 90 Time of Cl Introduction 91 Conclusions 92 CHAPTER 5 LOW TEMPERATURE ASHING 95 Apparatus 95 L. T. A. Side Effects 96 Temperature of Ashing 100 Ashing- The Colour of Mineral Matter 100 Mineral Matter Profiles 101 CHAPTER 6 MUDROCKANALYSES 102 Section 1 WHOLE ROCK GEOCHEMISTRY 102 XRF Preparation 103 Major Element Geochemistry 105 Normative Mineralogy 107 (viii) Page Number Quartz 108 Combined Silica and Alumina 111 Titania 112 Ferrous Iron 113 Ferric Iron 114 Manganese 115 Calcium 117 Magnesium 118 Sodium and Potassium 120 Phosphorous 121 Conclusions 123 Section 2 CLAY MINERAL ANALYSIS 126 Method 126 Sample Preparation 126 Pre-treatment Procedures 129 Peak Area Estimation 130 Clay Proportions 133 Clay Minerals in the Coal 134 Clay Mineral Distribution in the Mudrocks 135 Clay Mineral Variation 135 Chlorite Composition 139 Illite 141 Illite Polytypes 142 Crystallinity Index and Sharpness Ratio 143 Mixed-layer Clays 145 Kaolinite 148 Crystallinity. 149 The Significance of Kaolinite in Diagenesis 151 (ix) Page Number The Implications of the Kaolinite Content in the Floor Measures 152 Conclusions - 154 Section 3 TRACE ELEMENTS 157 Sample Preparation 157 Past Study 158' Trace Elements in Early Sulphide Diagenesis, Nodules, Cleat and Associated Strata 158 Trace Element Comparisons 159 Seam Profile Description - General 159 Trace Element Associations 160 Further Evidence on Trace Element Location 170 Summary of Trace Element Locations 171 Source of Trace Elements 171 Conclusions 175 Section 4 PHYSICAL PROPERTIES OF MUDROCKS 177 N. C. B. Cone Indenter 177 The-Influence of Mineralogy, Fabric and Organic Matter- 177 Conclusions 180 CHAPTER 7 EXCHANGEABLE CATIONS 181 Method 181 Cation Exchange - Theory 182 Clay Mineral Content and C. E. C. 184 Clay, Associationships 185 -Mineral Seam Profiles 186 Cation Ratios 189 Exchangeable Cations in Coals 191 Conclusions 191 LX) Page Number CHAPTER 8 COAL MINERALOGY AND GEOCHEMISTRY 193 The Origin of Minerals in Coal Seams 193 Inorganic Matter in Vegetation 194 Coal Mineral Matter Analysis - XRD 196 Minerals Present 196 Sulphide Group 199 Clay Group including Quartz 201 Carbonate Group 204 Other Minerals 205 Summary of Coal Minerals 206 Coal Ash Geochemistry - XRF 207 Constraints 207 Total Silica and Alumina 208 Titania 210 Total Iron 213 Calcium, Magnesium and Manganese 215 Sodium and Potassium 218 Phosphorous 220 The Relative Contributions of Detrital and Diagenetic Minerals in Coal Ash and Associated Strata 221 Conclusions 224 CHAPTER 9 CLEAT 228 Cleat origins 229 Cleat Frequency 231 Influence of Bed Thickness 232 Physical Properties of Coal Types 233 (xi) Page Number Cleat Mineralogy 234 Minerals Present 234 Between Colliery Comparisons 235 Yorkshire, Nottinghamshire, S.
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