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Chemical Analysis of Contaminated Land

De
312 pages
This book provides a unique source of reference on the chemical analysis of potentially contaminated land. It assists in specifying appropriate analyses, relevant strategies for carrying out analyses, and methods of interpreting results within the new risk-based legislative framework for contaminated land. It addresses all aspects of the analysis, from delivery of the samples to the laboratory to the presentation of the results to the clients. Emphasis is placed on concentrated, tabular data, wherever possible. Problems of analysis are highlighted and solutions are proposed. Asbestos is covered in detail in the chapter on inorganic parameters, and a chapter is included on the new techniques of ecotoxicity measurement.

Directed equally at the analytical chemist and the environmental scientist or engineer responsible for commissioning analyses of potentially contaminated soil or water samples, the book is written in a way that will prove helpful to both new and experienced practitioners. As such, it is one of the first volumes to bridge the gap between the customer and the supplier.

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Contents
Contributors Preface
1
2
3
The risk assessor as the customer K. CLIVE THOMPSON and C. PAUL NATHANAIL
1.1 Analysis issues 1.2 Definition of analysis 1.3 Quality issues in contaminated land analysis 1.3.1 Background 1.3.2 ISO 17025 1.3.3 The six valid analytical measurement (VAM) principles 1.3.4 MCERTS 1.4 Sampling point frequency considerations 1.5 Sample pretreatment issues 1.6 Analysis method requirements 1.7 Measurement uncertainty 1.8 Proficiency schemes 1.9 New areas of analysis 1.9.1 Organic carbon 1.9.2 Partition coefficients (Kd values) 1.9.3 Bioavailability and bioaccessibility Note References Publications relevant to the CLR R&D programme
The requirements of the analytical method DAVID WESTWOOD
2.1 Need for fully documented and properly validated methods 2.2 Current regimes 2.3 How to validate international, national and individual laboratory methods 2.4 Quality control – quality assurance 2.5 Prescribed method versus minimum performance characteristics approach 2.6 Proficiency testing for contaminated soil analysis 2.7 Reference materials References
Initial sample preparation MARK ALLEN
3.1 3.2
Introduction An overview of initial sample preparation
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1
1 5 5 5 6 7 8 10 12 14 15 17 18 18 19 19 20 20 22
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23 25 25 29 29 30 32 32
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34 35
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4
5
CONTENTS
3.2.1 Receipt of samples by the laboratory 3.2.2 Prepreparation 3.2.3 Coarse comminution 3.2.4 Sieving for preparation purposes 3.2.5 Homogenisation 3.2.6 Subsampling 3.2.7 Fine comminution 3.2.8 Finishing 3.2.9 Comminution of vegetation 3.3 Processes and problems 3.3.1 Contamination from preparation equipment 3.3.2 Crosscontamination 3.3.3 Subsampling bias 3.3.4 Subsampling bias caused by sieving operations 3.3.5 Loss of fine particulates, volatile and labile components 3.4 Quality control 3.5 Good laboratory practice in initial sample preparation 3.5.1 Health and safety 3.5.2 Provisional protocols References
Metal analysis PATRICK THOMAS
4.1 Introduction 4.2 General discussion 4.2.1 Overview of digestion methods 4.2.2 Dry ashing 4.2.3 Wet digestion 4.2.4 Heating devices 4.3 Overview of instrumental methods of analysis 4.3.1 What is atomic absorption? 4.3.2 Flame atomic absorption spectrometry 4.3.3 Graphite furnace atomic absorption spectrometry 4.3.4 Hydride generation atomic absorption and fluorescence methods 4.3.5 Cold vapour atomic absorption and fluorescence methods for mercury 4.4 What is atomic emission spectrometry? 4.4.1 Inductively coupled plasma atomic emission spectrometry 4.5 What is inductively coupled plasma mass spectrometry? 4.6 How to select the proper technique? 4.7 Overview of trace element speciation References
Analysis of inorganic parameters GEORGE E. RAYMENT, ROSS SADLER, ANDREW CRAIG, BARRY NOLLER and BARRY CHISWELL
5.1 5.2
Introduction Electrical conductivity 5.2.1 Soil:water extract 5.2.2 EC measurement and reporting
36 36 39 44 44 45 47 48 49 51 51 53 54 57 57 58 59 60 61 62
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64 65 67 68 68 70 72 72 74 76 78 80 81 81 85 89 91 95
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99 99 101 101
5.3
5.4
5.5
5.6
5.7
5.8
5.9
CONTENTS
pH 5.3.1 pH of 1:5 soil/water suspension (pH ) w 5.3.2 pH of 1:5 soil/0.01 M calcium chloride extract (pH ) c 5.3.3 pH of 1:5 soil/1 M potassium chloride extract (pH ) K 5.3.4 pH of sodium fluoride suspension (pH ) F 5.3.5 pH of hydrogen peroxide extract (pH ) HO 5.3.5.1 Procedure 5.3.6ΔpH Redox potential 5.4.1 Summary 5.4.2 Capacity factor (Poise) 5.4.3 Usefulness of pe 5.4.4 Measurement of soil redox and electrodes Water soluble chloride 5.5.1 Chloride – 1:5 soil/water extract, ion chromatography (chemical suppression of eluent conductivity) Water soluble boron 5.6.1 Hot water extractable soil B Sulfur 5.7.1 Total sulfur – Xray fluorescence 5.7.1.1 Preparation of standard pellets 5.7.1.2 Preparation of soil pellets 5.7.1.3 Analysis 5.7.2 Pyrite and other iron disulfides and acid volatile sulfides (chromium reducible sulfur) 5.7.2.1 Procedure 5.7.2.2 Calculation of the chromium reducible sulfur content 5.7.3 Water extractable sulfur – ICPAES 5.7.4 Water extractable sulfatesulfur – ion chromatography (chemical suppression of eluent conductivity) Cyanides, thiocyanates and cyanates 5.8.1 Cyanides 5.8.2 Thiocyanates 5.8.3 Cyanates 5.8.4 Standard digestion procedures and free cyanide 5.8.5 Speciation techniques for metallocyanide complexes 5.8.5.1 Ion chromatography 5.8.5.2 Atomic absorption spectrometry 5.8.5.3 Capillary zone electrophoresis 5.8.6 Determination of other cyanide compounds in soil Asbestos 5.9.1 Introduction – the asbestos minerals and their uses 5.9.2 The health effects of asbestos 5.9.3 Common building materials and products that contained asbestos 5.9.4 Common asbestos containing materials that may be found in contaminated land sites 5.9.5 Encountering asbestos containing materials during a site investigation or redevelopment 5.9.6 The packaging of suspected asbestos containing materials for transportation to a testing laboratory 5.9.7 Choosing a suitable testing laboratory 5.9.8 Analysis of suspect asbestos containing materials
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101 102 102 102 103 103 103 103 104 104 104 104 105 106
107 107 107 108 109 109 109 109
110 111 111 112
112 112 112 115 115 116 117 117 118 118 118 119 119 120 120
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123 124 124
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CONTENTS
5.9.9 Achievable laboratory detection limits and interpretation of results 5.9.9.1 Bulk materials 5.9.9.2 Soil materials Abbreviations Notes References
Petroleum hydrocarbons and polyaromatic hydrocarbons JIM FARRELLJONES
6.1
6.2 6.3
6.4
Introduction 6.1.1 Chemical characteristics 6.1.2 Architecture of organic molecules 6.1.3 Aromatics 6.1.4 Chemical composition of petroleum 6.1.4.1 Product characteristics 6.1.4.2 Gasoline (called petrol in the UK) 6.1.4.3 Aviation gasoline 6.1.4.4 Jet fuels 6.1.4.5 Kerosene – domestic heating fuel 6.1.4.6 Diesel fuel 6.1.4.7 Fuel oils 6.1.4.8 Lubricating oils Environmental fate of petroleum products Factors influencing the analytical process 6.3.1 Collection and preservation 6.3.2 Sample extraction 6.3.2.1 Soxhlet 6.3.2.2 Manual shake 6.3.2.3 Accelerated solvent extraction 6.3.2.4 Microwave 6.3.2.5 Thermal extraction and static headspace 6.3.2.6 Purge and trap (dynamic headspace) 6.3.3 Concentration of sample extract 6.3.3.1 Sorbant/cryogenic trapping 6.3.3.2 Snyder column 6.3.3.3 KudernaDanish concentrator (KD concentrator) 6.3.3.4 Nitrogen evaporation 6.3.3.5 Vacuum 6.3.4 Cleanup of sample 6.3.4.1 Removal of nonpetroleum species 6.3.4.2 Isolation of particular species 6.3.4.3 Concentration of particular analytes 6.3.5 Measurement 6.3.5.1 Total petroleum hydrocarbons (TPH) 6.3.5.2 Petroleum group type analysis (not suitable for risk estimation) 6.3.5.3 Individual compound analysis Total petroleum hydrocarbons: a detailed method review 6.4.1 Gas chromatography 6.4.1.1 Gasoline range organics (GRO) 6.4.1.2 Diesel range organics 6.4.1.3 Total petroleum hydrocarbons
126 126 126 127 127 128
132
132 132 133 133 133 136 136 137 137 137 139 139 139 139 141 141 141 142 143 143 143 144 144 145 145 145 146 146 146 146 146 146 147 148 148 148 148 148 149 154 154 156
7
CONTENTS
6.4.2 Infrared spectroscopy (IR) TPH 6.4.3 Gravimetric TPH methods 6.4.4 Immunoassay TPH methods 6.5 Petroleum group type analysis (detailed review) 6.5.1 Thin layer chromatography (Iatroscan™ method) 6.5.2 Speciated group type TPH 6.6 Individual compound analysis 6.7 Polyaromatic hydrocarbons (PAHs) 6.7.1 Structure 6.7.2 Sources 6.7.3 Carcinogenic nature 6.7.4 Methods of analysis 6.7.4.1 Screening test kits 6.7.4.2 Gravimetric 6.7.4.3 Thin layer chromatography (TLC) 6.7.4.4 High pressure liquid chromatography (HPLC) 6.7.4.5 Gas chromatography–flame ionisation detector (GC–FID) 6.7.4.6 Gas chromatography–mass spectrometry (GC–MS) Abbreviations Glossary of terms Bibliography Editors’ note
Volatile organic compounds SUE OWEN and PETER WHITTLE
7.1 Introduction 7.2 Presence of VOCs in soil 7.3 Sampling and subsampling 7.3.1 Artefacts 7.4 Methods of analysis 7.4.1 Methanol extraction 7.4.2 Headspace 7.4.3 Purge and trap 7.4.4 Direct aqueous injection 7.5 Chromatography 7.5.1 Capillary columns 7.6 Detectors and quantitation 7.6.1 Mass spectrometric detection (MS) 7.6.2 Flame ionisation detector (FID) 7.6.3 Electron capture detector (ECD) 7.6.4 Electrolytic conductivity detector (ELCD) 7.6.5 Photoionisation detector (PID) 7.6.6 Standards and quantitation 7.7 Screening techniques 7.7.1 Qualitative analysis 7.7.2 Semiquantitative analysis 7.8 Specific groupings References Commonly used groupings for analysing VOC samples
ix
159 160 160 160 161 161 163 163 163 163 164 166 166 166 166 168 168 168 168 169 175 176
177
177 177 178 180 180 180 181 181 181 182 182 182 182 183 183 183 184 184 185 185 185 185 186 186
x
8
9
CONTENTS
Nonhalogenated organic compounds including semivolatile organic compounds (SVOCs) JOOP HARMSEN and PAUL FRINTROP
8.1 Introduction 8.2 Extraction 8.2.1 Presence of organic compounds in soil 8.2.1.1 Soxhlet 8.2.1.2 Shaking (agitation) procedure 8.2.1.3 Pressurised fluid extraction (PFE) 8.2.1.4 Super critical fluid extraction (SFE) 8.2.2 Pretreatment in relation to extraction 8.3 Screening or quantitative determination 8.3.1 Group parameters 8.4 The bioavailable fraction 8.5 Detection, identification and quantification 8.5.1 Detection 8.5.2 Identification 8.5.3 Quantification 8.6 Examples 8.6.1 Group parameters for organohalogens 8.6.2 Phthalates 8.6.3 Organotin compounds 8.6.4 More polar herbicides and pesticides 8.6.5 Phenols References
Leaching tests LESLIE HEASMAN
9.1 Introduction 9.2 The value of leaching tests in land contamination 9.3 The primary factors which control leaching 9.3.1 The leaching mechanism 9.3.2 The chemistry of the contaminants of concern 9.3.3 The pH and redox potential of the environment in which the material is present 9.3.4 The nature of the leachant 9.3.5 Physical, chemical or biological changes in the material over time 9.4 Available leaching tests 9.4.1 Types of leaching tests 9.4.2 Basic characterisation tests 9.4.3 Compliance tests 9.4.4 Verification tests 9.4.5 Reviews of available tests 9.5 Quality assurance and quality control 9.6 Selection of a leaching test 9.7 Interpretation of the results of leaching tests References
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189 189 189 192 193 194 195 195 197 198 199 201 201 202 204 205 205 207 209 211 213 214
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216 217 217 218 219
219 219 220 220 221 221 222 222 223 223 225 226 227
10
CONTENTS
Ecological assessment and toxicity screening in contaminated land analysis ANDREAS P. LOIBNER, OLIVER H.J. SZOLAR, RUDOLF BRAUN and DORIS HIRMANN
10.1 Introduction 10.1.1 Ecotoxicology 10.1.2 Ecological risk assessment 10.2 Toxicity testing 10.2.1 Level of organisation 10.2.2 Biological responses 10.2.2.1 Statistical estimation of endpoints 10.2.3 Ecotoxicity tests and bioassays 10.3 The use of bioassays for soil evaluation 10.3.1 Ecological assessment and toxicity screening 10.3.2 Selection criteria for bioassays 10.3.3 Scope of application 10.3.3.1 The role of bioassays in soil testing 10.3.3.2 Application of bioassays for toxicity screening 10.3.3.3 Application of bioassays for ecological assessments 10.3.4 Test media: solid samples and aqueous extracts 10.3.4.1 Pretreatment and storage of contaminated samples 10.3.5 Bioassays relevant for contaminated soil analysis 10.4 Conclusion Acknowledgements 10.5 Bioassays Abbreviations References
Appendix 1 Appendix 2 Appendix 3 Index
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229 229 230 232 233 234 236 237 238 242 243 244 245 246 247 249 251 251 253 254 254 264 264
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