Introduction to Environmental Analysis

Series Preface xiii

Preface xv

Acronyms, Abbreviations and Symbols xix

About the Author xxiii

1 Introduction 1

1.1 The Environment 1

1.2 Reasons for Concern 2

1.2.1 Today’s World 4

1.2.2 Past and Current Crimes 4

1.3 Pollution 4

1.4 The Necessity of Chemical Analysis 8

2 Transport of Pollutants in the Environment and Approaches to their Analysis 11

2.1 Introduction 11

2.2 Sources, Dispersal, Reconcentration and Degradation 12

2.3 Transport and Reconcentration of Neutral Organic Compounds 15

2.3.1 Bioconcentration 16

2.3.2 Accumulation in Sediments 17

2.3.3 Biomagnification 18

2.3.4 Degradation 19

2.4 Transport and Reconcentration of Metal Ions 20

2.4.1 Solubilization 22

2.4.2 Deposition in Sediments 22

2.4.3 Uptake by Organisms 22

2.5 What is a Safe Level? 23

2.6 Sampling and Sample Variability 24

2.6.1 Representative Samples 24

2.6.2 Sample Storage 25

2.6.3 Critical Paths and Critical Groups 26

2.7 General Approach to Analysis 26

2.8 The Choice of Laboratory or Field Analysis 28

2.9 Quality Assurance 30

2.9.1 Finding a Suitable Method 32

2.9.2 Laboratory Standards 33

3 Water Analysis – Major Constituents 35

3.1 Introduction 35

3.2 Sampling 41

3.3 Measurement of Water Quality 46

3.3.1 Suspended Solids 46

3.3.2 Dissolved Oxygen and Oxygen Demand 47

3.3.3 Total Organic Carbon 54

3.3.4 pH, Acidity and Alkalinity 55

3.3.5 Water Hardness 57

3.3.6 Electrical Conductivity 59

3.4 Techniques for the Analysis of Common Ions 61

3.4.1 Ultraviolet and Visible Spectrometry 61

3.4.2 Emission Spectrometry (Flame Photometry) 68

3.4.3 Ion Chromatography 69

3.4.4 Examples of the Use of Other Techniques 73

4 Water Analysis – Trace Pollutants 77

4.1 Introduction 77

4.2 Organic Trace Pollutants 78

4.2.1 Guidelines for Storage of Samples and their Subsequent Analysis 80

4.2.2 Extraction Techniques for Chromatographic Analysis 81

4.2.3 Gas Chromatography 88

4.2.4 Liquid Chromatography 101

4.2.5 Immunoassay 105

4.2.6 Spectrometric Methods 110

4.3 Metal Ions 112

4.3.1 Storage of Samples for Metal Ion Analysis 112

4.3.2 Pretreatment 113

4.3.3 Atomic Spectrometry 114

4.3.4 Visible Spectrometry 124

4.3.5 Anodic Stripping Voltammetry 125

4.3.6 Liquid Chromatography 128

4.3.7 Metal Speciation: A Comparison of Techniques 131

5 Analysis of Land, Solids and Waste 135

5.1 Introduction 135

5.2 Common Problem Areas in the Analysis of Solids 138

5.2.1 Sampling 138

5.2.2 Pretreatment 139

5.2.3 Extraction of the Analyte 140

5.2.4 Sample Clean-up 140

5.2.5 Analytical Determination 141

5.2.6 Quality Assurance and Quality Control 141

5.3 Specific Considerations for the Analysis of Biological Samples 142

5.3.1 Sampling and Storage of Plant Material 142

5.3.2 Pretreatment 142

5.3.3 Extraction Techniques for Organic Contaminants 144

5.3.4 Ashing and Dissolution Techniques for Trace Metals 145

5.3.5 Analysis of Animal Tissues 146

5.4 Specific Considerations for the Analysis of Soils 146

5.4.1 Sampling and Storage 146

5.4.2 Pretreatment 148

5.4.3 Extraction of Organic Contaminants 148

5.4.4 Extraction of Available Ions 149

5.4.5 Dissolution Techniques for the Determination of Total Metal Concentrations in Soil 150

5.4.6 Determination of pH 150

5.5 Specific Considerations for the Analysis of Contaminated Land 151

5.5.1 Steps in the Investigation of Contaminated Land 152

5.5.2 Sampling, Sample Storage and Pretreatment 154

5.6 Specific Considerations for the Analyses Involved in Waste and its Disposal by Landfill 156

5.6.1 Types of Waste and their Disposal 156

5.6.2 Sampling and Storage 158

5.6.3 Pretreatment of Solids and Liquids with a High Solid Content 160

5.6.4 Analysis of Leachate 161

5.6.5 Introduction to Gaseous Emissions 164

5.7 Specific Considerations for the Analysis of Sediments and Sewage Sludge 165

5.7.1 Sampling and Storage 165

5.7.2 Pretreatment 165

5.7.3 Extraction Techniques for Organic Contaminants 167

5.7.4 Dissolution Techniques for Trace Metals 167

5.7.5 Analysis of Sewage Sludge 168

5.8 New Extraction and Dissolution Techniques 168

5.8.1 Automated Soxhlet 169

5.8.2 Accelerated Solvent Extraction 169

5.8.3 Microwave Digestion and Microwave-Assisted Extraction 169

5.8.4 Sonication 170

5.8.5 Supercritical Fluid Extraction 170

5.8.6 Comparison of the Techniques 172

6 Atmospheric Analysis – Gases 175

6.1 Introduction 175

6.1.1 A Note on Units 181

6.2 Determination of Time-Weighted Average Concentrations 183

6.2.1 Absorption Trains 183

6.2.2 Solid Adsorbents 186

6.2.3 Diffusion (or Palmes) Tubes 189

6.3 Determination of Instantaneous Concentrations 191

6.3.1 Direct-Reading Instruments 191

6.3.2 Gas Detector Tubes 199

6.3.3 Gas Chromatography and Mass Spectrometry 201

6.3.4 Monitoring Networks and Real-Time Monitoring 205

6.3.5 Remote Sensing and other Advanced Techniques 206

7 Atmospheric Analysis – Particulates 213

7.1 Introduction 213

7.2 Sampling Methods 216

7.2.1 High-Volume Samplers 216

7.2.2 Personal Samplers 217

7.2.3 Cascade Impactors 218

7.2.4 Further Considerations for Organic Compounds 219

7.2.5 Sampling Particulates in Flowing Gas Streams 220

7.2.6 PM 10 Sampling 222

7.2.7 Sampling of Acid Deposition 224

7.3 Analytical Methods Involving Sample Dissolution 225

7.3.1 Metals 225

7.3.2 Organic Compounds 226

7.4 Direct Analysis of Solids 227

7.4.1 X-Ray Fluorescence 227

7.4.2 X-Ray Emission 229

7.4.3 Neutron Activation Analysis 230

7.4.4 Infrared Spectrometry 230

7.4.5 Methods for Asbestos Analysis 230

8 Ultra-Trace Analysis 233

8.1 Introduction 233

8.1.1 What Groups of Compounds are We Discussing? 234

8.2 Analytical Methods 236

8.2.1 General Considerations 236

8.2.2 Factors Affecting Detection Sensitivity 237

8.2.3 Mass Spectrometric Detection 239

8.2.4 Quantification 245

8.2.5 Quality Control 246

8.3 A Typical Analytical Scheme 246

8.3.1 Pretreatment 248

8.3.2 Gas Chromatography 250

Responses to Self-Assessment Questions 253

Bibliography 273

Glossary of Terms 279

Units of Measurement and Physical Constants 285

Periodic Table 291

Index 293