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Reynolds-B-1981-Phd-Thesis.Pdf -1- GEOCHEMICAL STUDIES ON HEAVY METALS IN WATERS AND SEDIMENTS IN MINSTERLEY BROOK, SHROPSHIRE AND THE RIVER ECCLESBOURNE, DERBYSHIRE by Brian Reynolds A Thesis presented for the degree of Doctor of Philosophy in the University of London Department of Geology Imperial College of Science and Technology London SW7. September 1981 Abstract The dispersion patterns downstream, from localised sources for Cu, Pb, Zn, Cd, Fe, Mn, Ca, and Mg, in river sediment, "dissolved" water ( < .45 pn) and suspended particulate phases have been described for two river systems contaminated by historic mining. To determine the extent of seasonal variation in the levels of metal in each phase, metal concentrations and water pH were monitored at 10 to 12 sites in each river at two monthly intervals for a year. The effects of river flow, and the relationships between metals within the three phases were investigated to identify the factors con- trolling metal dispersion and transport. The role of pH, the relationship of metal concentration to sediment grain size and the ratio of residual to non-residual metals in the sediments were also studied. Specific sources for metals within each catchment were identified, and these included mine adit drainage, collapse and run-off from mine waste and contaminated bank material and effluent discharge. -3- Acknowledqements I should like to thank my supervisor, Dr. I. Thorntonp for his help and encouragement throughout the project, Dr. L. Thorne for his guidance and advice, the staff of the Applied Geochemistry Research Group for the provision of laboratory facilities and assistance with the analytical work, and NERC for financial support. I should also like to acknowledge Dr. A. Marples, Dr. S. Mancey and Miss A. Vernon for their help at various times during the work. My particular thanks go to Dr. D. Moss of ITE, Bangor, for much time and energy spent in assistance with the statistics and computing and to ITE for making time and facilities available. I should like to record my sincere thanks to my wife Rachel, for her continued patient support and encouragement and for typing the first draft, and finally my thanks to Mrs. J. Lander for typing the final copy. -4- CONTENTS PAGE Title 1 Abstract 2 Acknowledgements 3 Contents 4 List of Figures 10 List of Tables 13 CHAPTER 1 Introduction 18 1.1 Metalliferous Mining as a Source of _ft Heavy Metals in River Waters 1.2 Toxic Effects of Heavy Metals and Limits 9f. to Water Quality 1.3 Regional Geochemical Data and Water ^ Quality CHAPTER 2 Literature Review 31 2.1 Amounts of Heavy Metals in Waters 31 2.1.1 Seasonal Variations in Metal Concentrations 31 in Water 2.1.2 Effects of Stream Discharge on Metal Concentrations 34 2.2 Sampling River Water 38 2.2.1 Selection of Sample Sites 39 2.2.2 Sampling Devices and Sample Storage 40 2.3 Filtration of Water Samples 45 2.3.1 Types of Filters 47 2.3.2 Contamination and Adsorption by Filters 50 -5- CONTENTS PAGE 2.4 Analysis of Filtrate 51 2.4.1 Chelation - Solvent Extraction 52 2.4.2 Chelating - Ion Exchange Resins 55 2.4.3 Evaporation 57 2.4.4 Co-Precipitation - 58 2.5 Analysis of Suspended Particulates 59 2.6 Forms of Metals in Solution 61 2.6.1 Classification of Metal Species 61 2.6.2 Chemical Modelling 63 2.6.3 Direct Measurement of Metal Species 65 2.6.4 Dissolved Inorganic Species 68 2.6.5 Metal-Organic Species 71 2.7 Levels of Heavy Metals in Stream Sediments 75 2.7.1 Seasonal Variations in Metal Concentrations 7 D in Sediments 2.7.2 Mode of Occurrence of Heavy Metals in Stream Sediments 80 2.8 Chemical Analysis of Stream Sediments 81 2.8.1 Partial Extraction Methods 81 2.8.2 Total Attacks 86 2.8.3 Intermediate Acid Attacks 87 2.9 Particle Size Fractionation of Stream 87 Sediments 2.10 Water-Sediment Interactions 90 2.10.1 Oxidation and Reduction Reactions 90 2.10.2 Interactions with Clays 92 2.10.3 Interactions with Iron and Manganese Oxides 94 2.10.4 Interactions with Organic Matter 97 -6- CONTENTS PAGE 2.10.5 Re-mobilisation of Heavy Metals from ^q^ Sediments 2.11 Water-Suspended Sediment Interactions 102 CHAPTER 3 Description of Field Areas 105 3.1 The Minsterley Brook - Rea Brook Catchment 105 3.1.1 General Description 105 3.1.2 Solid Geology of the Minsterley - Rea Brook 109 Catchment 3.1.3 Pleistocene and Recent Deposits in the Minsterley - Rea Brook Catchments 3.1.4 History of Metalliferous and Coal Mining 118 in West Shropshire 3.1.5 Description of Mine Drainage I24 3.1.6 Description of Mine Dumps at Gravels 125 3.2 The River Ecclesbourne Catchment 127 3.2.1 General Description 127 3.2.2 Geology of the Wirksworth Area 131 3.2.3 Geology of the Ecclesbourne Valley 134 3.2.4 Mineralisation and Mining 137 3.2.5 Mine Drainage and Lead Smelting 138 3.3 The Rowberrow Bottom Catchment 139 3.3.1 General Description 139 3.3.2 Geology of the Area Surrounding Rowberrow ^4^ Bottom 3.3.3 Outline History of Mining in the Shipham ^45 Orefield 3.3.4 Sources of Contamination in Rowberrow Bottom 147 -7- CONTENTS • PAGE CHAPTER 4 Geochemical Reconnaissance 149 4. 1 Introduction 149 4. 2 Collection of Stream Sediment Samples 149 4. 3 Analysis of Stream Sediment Samples 153 4. 4 Collection of Stream Water -Samples 153 4. 5 Analysis of Stream Water Samples 156 4. 6 Sample Contamination 158 4. 7 Results and Discussion 160 4. 8 Conclusions 178 CHAPTER 5 A Comparison of Filter Types and Methods for the Determination of Heavy Metals in 180 Suspended Particulate Matter 5. 1 Introduction 180 5. 2 Experimental Methods 182 5. 2. 1 Total Digestion of Membrane Filters 182 5. 2. 2 Leaching of Heavy Metals from Filters 182 5. 3 Determination of Heavy Metals in Suspended 183 Particulates 5. 3. 1 Comparison Between the Existing Method and 183 Wet Acid Digestion 5. 3. 2 Comparison Between the Existing Method and 184 Cold Acid Leaching 5. 3. 3 Total Heavy Metals by Sample Evaporation and 186 Acid Digestion 5. 4 Results and Discussion 186 5. 5 Conclusions 201 CHAPTER 6 Experimental Procedures 203 6.1 Seasonal Stream Sediment and Water Sampling Programme -8- CONTENTS PAGE 6.1.1 Sample Collection and Pretreatment 203 6.1.2 Chemical Analysis of Seasonal Samples 205 6.1.3 Assessment of Sampling and Analytical 207 Variation in Seasonal Sediment Data 6.2 Partitioning of Heavy Metals within Stream 207 Sediments 6.2.1 Determination of Residual and Non-residual Heavy Metals in Sediments 208 6.2.2 Size Fractionation of Stream Sediments 208 6.3 Measurement of River Discharge 210 6.4 The Determination of Heavy Metals in Soils, 213 Alluvium and Mine Waste 6.4.1 Sample Collection 213 6.4.2 Chemical Analysis 215 6.5 Determination of Heavy Metals in Shallow 215 Groundwater and Mine Drainage CHAPTER 7 Analytical Results and Discussion for 2j7 Minsterley Brook and the River Ecclesbourne 7.1 Introduction 217 7.2 Heavy Metals in Alluvium, Mine Waste, Soils 218 and Effluents 7.2.1 Minsterley Brook 218 7.2.2 River Ecclesbourne 235 7.3 Patterns of Metal Dispersion 239 7.3.1 Metal Dispersion in Sediments in Minsterley 240 Brook 7.3.2 Metal Dispersion in Sediments in the River 244 Ecclesbourne 7.3.3 Variations in Minsterley Brook Sediment Data 248 7.3.4 Variations in River Ecclesbourne Sediment Data 258 -9- CONTENTS PAGE 7.3.5 Metal Dispersion in Waters in Minsterley 262 Brook 7.3.6 Metal Dispersion in Waters in the River - 269 Ecclesbourne 7.3.7 Variations in Metal Concentrations in Water 276 7.4 Seasonal Variations in Geochemical Data 296 7.4.1 Stream Sediments 296 7.4.2 Filtrable Stream Water Data 304 7.5 Relationships Between Sample Types 310 7.6 Interelement Correlations 321 7.7 Partitioning of Heavy Metals in Stream 33^ Sediments 7.8 Distribution of Metals in Relation to 345 Sediment Grainsize 7.9 Relationships Between Metal Concentrations 3^^ and River Flow 7.10 Analytical Control Data 372 CHAPTER 8 Conclusions and Recommendations for 3QQ Further Research Bibliography 394 Appendix 1 423 Appendix 2 432 Appendix 3 436 Appendix 4 444 Appendix 5 467 -10- LIST OF FIGURES PAGE FIGURE 1.1 Interim Line Printer Geochemical Map for 30 Cadmium 2.1 Types of Metal Species in Water 62 2.2 Effects of Reaction Temperature and Time on the Extraction of Cu from Sediments 85 2.3 The Relationship Between Surface Area and Trace Metal Adsorption in Sediments 89 3.1 Drainage Plan of Minsterley Brook 106 3.2 Simplified Geology of the Minsterley Brook Catchment 112 3.3 Plan of the Roman Gravels Mine Dump 126 3.4 Drainage Plan of the River Ecclesbourne 128 3.5 Simplified Geology of the River Ecclesbourne Catchment 135 3.6 Drainage Plan of Rowberrow Bottom 142 3.7 Simplified Geology of the Area Surrounding Rowberrow Bottom 143 4.1 Stream Sample Sites, Minsterley Brook 151 4.2 Stream Sample Sites, River Ecclesbourne 152 4.3 Pb in Stream Sediments - Minsterley Brook 162 4.4 Pb in Stream Water - Minsterley Brook 165 4.5 Pb Dispersion in Sediments and Water - Minsterley Brook 166 4.6 Cd Dispersion in Sediments and Water - Rowberrow Bottom 169 4.7 Zn in Stream Sediments - River Ecclesbourne 172 4.8 Zn in Stream Water - River Ecclesbourne 173 4.9 Zn Dispersion in Sediments and Water - River Ecclesbourne 174 6.1 Stream Discharge Measurement by Partial Area Method 211 -11- LIST OF FIGURES PAGE 6.2 Soil Sampling Transects across Minsterley Catchment 214 7.1 Description of Dump Borehole at Gravels Mine 221 and Profiles for Pb, Znf Cd and Fe 7.2A Pb in Soils of the Minsterley Catchment - Transect A and B 229 7.2B Pb in Soils of the Minsterley Catchment - Transect C 230 7.3 Pb in Minsterley Brook Bank Soils 232 7.4 Cd in Minsterley Brook Bank Soils 233 7.5 Downstream Distribution of Zn in River Ecclesbourne
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