Extraction Techniques for Environmental Analysis

John R. Dean is Professor of Analytical and Environmental Sciences at Northumbria University in the United Kingdom. His research is focused on investigating organic and inorganic pollutants in the environment using a range of analytical techniques.

• Preface xvAbout the Author xviiAcknowledgements xixSection A Initial Considerations 11 The Analytical Approach 31.1 Introduction 31.2 Environmental Organic Compounds of Concern 41.3 Essentials of Practical Work 121.4 Health and Safety 151.5 Considerations for Data Presentation 211.5.1 Useful Tips on Presenting Data in Tables 211.5.2 Useful Tips on Presenting Data in Graphical Form 211.6 Use and Determination of Significant Figures 211.7 Units 231.8 Calibration and Quantitative Analysis 241.9 Terminology in Quantitative Analysis 241.10 Preparing Solutions for Quantitative Work 251.11 Calibration Graphs 271.12 The Internal Standard 281.13 Limits of Detection/Quantitation 291.14 Dilution or Concentration Factors 311.15 Quality Assurance 321.16 Use of Certified Reference Materials 331.17 Applications 34Further Reading 39Section B Sampling 412 Sampling and Storage 432.1 Introduction 432.2 Sampling Strategy 442.3 Types of Aqueous Matrices 452.4 Types of Soil Matrices 462.5 Physicochemical Properties of Water and Solid Environmental Matrices 492.5.1 Aqueous (Water) Samples 492.5.2 Solid (Soil) Samples 502.6 Sampling Soil (and/or Sediment) 522.7 Sampling Water 572.8 Sampling Air 592.9 Sampling and Analytical Operations Interrelationships and Terminology 602.9.1 Sampling Operations 602.9.2 Analytical Operations 612.10 Storage of Samples 632.10.1 Choice of Storage Container for Liquid Samples 632.10.2 Cleaning of Storage Container for Liquid Samples 642.11 Preservation Techniques for Liquid Samples 652.12 Preservation Techniques for Solid Samples 662.13 Preservation Techniques for Gaseous Samples 662.14 Applications 66Reference 72Section C Extraction of Aqueous Samples 733 Classical Approaches for Aqueous Extraction 753.1 Introduction 753.2 Liquid–Liquid Extraction 753.2.1 Theory of LLE 763.2.2 Selection of Solvents 773.2.3 Solvent Extraction 783.2.4 Problems with the LLE process and Their Remedies 813.3 Liquid Microextraction Techniques 813.3.1 Single-Drop Microextraction (SDME) 813.3.2 Dispersive Liquid–Liquid Microextraction (DLLME) 823.4 Purge and Trap 843.5 Headspace Extraction 843.5.1 Procedure for Static Headspace Sampling 863.5.2 Procedure for Dynamic Headspace Sampling 873.6 Application 884 Solid-Phase Extraction 914.1 Introduction 914.2 Types of SPE Sorbent 934.2.1 Multimodal and Mixed-Phase Extractions 944.2.2 Molecularly Imprinted Polymers (MIPs) 944.3 SPE Formats and Apparatus 974.4 Method of SPE Operation 1004.5 Solvent Selection 1034.6 Factors Affecting SPE 1044.7 Selected Methods of Analysis for SPE 1044.7.1 Application of Reversed-Phase SPE 1044.7.2 Application of Normal-Phase SPE 1064.7.3 Application of Ion Exchange SPE 1074.7.4 Application of Mixed-Mode SPE 1084.8 Automation and Online SPE 1084.9 Applications 1104.10 Summary 117References 1185 Solid-Phase MicroExtraction 1195.1 Introduction 1195.2 Theoretical Considerations for SPME 1195.3 Practical Considerations for SPME 1225.3.1 SPME Agitation Methods 1235.3.2 Other SPME Operating Considerations 1245.4 Application of SPME 1245.5 Summary 130Reference 1306 In-Tube Extraction 1316.1 Introduction 1316.2 Microextraction in a Packed Syringe (MEPS) 1336.2.1 Procedure for MEPS 1336.2.2 Main Issues in MEPS 1346.3 In-Tube Extraction (ITEX) 1356.3.1 Procedure for ITEX-DHS 1356.4 Application of ITEX-DHS 1366.5 Summary 1397 Stir-Bar Sorptive Extraction 1417.1 Introduction 1417.2 Theoretical Considerations for SBSE 1417.3 Practical Issues for SBSE 1437.3.1 Main Issues in SBSE 1437.4 Application of SBSE 1447.5 Summary 1448 Membrane Extraction 1458.1 Introduction 1458.2 Theoretical Considerations for Membrane Extraction 1468.2.1 Mass Transfer Coefficient Model 1478.2.2 Chemical Reaction Kinetic Model 1488.3 Passive Sampling Devices 1498.4 Application of Passive Sampling Using Chemcatcher® 1548.5 Summary 155Reference 155Section D Extraction of Solid Samples 1579 Classical Approaches for Extraction of Solid Samples 1599.1 Introduction 1599.2 Theory of Liquid–Solid Extraction 1599.3 Soxhlet Extraction 1629.3.1 Experimental 1639.4 Soxtec Extraction 1649.5 Ultrasonic Extraction 1659.5.1 Experimental 1669.6 Shake Flask Extraction 1679.6.1 Experimental 1679.7 Application 168Reference 17010 Pressurized Liquid Extraction 17110.1 Introduction 17110.2 Theoretical Considerations Relating to the Extraction Process 17110.2.1 Solubility and Mass Transfer Effects 17210.2.2 Disruption of Surface Equilibrium (By Temperature and Pressure) 17310.3 Instrumentation for PLE 17310.4 A Typical Procedure for PLE 17510.5 In Situ Clean-Up or Selective PLE 17910.6 Method Development for PLE 18110.6.1 Pre-Extraction Considerations 18110.6.2 Packing the Extraction Vessel 18110.7 Applications of PLE 18210.8 Summary 204References 20411 Microwave-Assisted Extraction 20511.1 Introduction 20511.2 Theoretical Considerations for MAE 20511.2.1 Selecting an Organic Solvent for MAE 20711.2.2 Heating Methods 20811.2.3 Calibration of a Microwave Instrument 20911.3 Instrumentation for MAE 21011.4 A Typical Procedure for MAE 21111.5 Applications of MAE 21211.6 Summary 217References 21712 Matrix Solid-Phase Dispersion 21912.1 Introduction 21912.2 Practical Considerations for MSPD 21912.3 Optimization of MSPD 22012.4 Application of MSPD 22112.5 Summary 22813 Supercritical Fluid Extraction 22913.1 Introduction 22913.2 Theoretical Considerations for SFE 23013.3 Supercritical CO2 23113.4 Instrumentation for SFE 23113.5 A Typical Procedure for SFE 23213.6 Application of SFE 23613.7 Summary 238References 238Section E Extraction of Gaseous Samples 23914 Air Sampling 24114.1 Introduction 24114.2 Techniques Used for Air Sampling 24214.2.1 Whole Air Collection 24214.2.2 Enrichment Onto Solid Sorbents 24314.2.2.1 Active Methods 24314.2.2.2 Passive Methods 24314.3 Thermal Desorption 24414.4 Workplace Exposure Limits 24914.5 Biological Monitoring 24914.6 Particulate Matter 25014.7 Application of Air Sampling 25114.8 Summary 252References 252Section F Post-Extraction 25315 Pre-Concentration and Associated Sample Extract Procedures 25515.1 Introduction 25515.2 Solvent Evaporation Techniques 25515.2.1 Needle Evaporation 25615.2.2 Automated Evaporator (TurboVap) 25615.2.3 Rotary Evaporation 25615.2.4 Kuderna–Danish Evaporative Concentration 25815.2.5 Automated Evaporative Concentration System 25815.3 Post-Extract Evaporation 26015.4 Sample Extract Clean-Up Procedures 26015.4.1 Column Chromatography 26015.4.1.1 Partition Chromatography 26115.4.1.2 Gel Permeation Chromatography 26115.4.1.3 Ion-Exchange Chromatography 26115.4.2 Acid–Alkaline Partition 26215.4.3 Acetonitrile–Hexane Partition 26215.4.4 Sulphur Clean-Up 26215.4.5 Alkaline Decomposition 26215.5 Derivatization for Gas Chromatography 26215.6 Application of Pre-Concentration for Analysis 264References 26416 Instrumental Techniques for Environmental Organic Analysis 26516.1 Introduction 26516.2 Theory of Chromatography 26516.3 Chromatography Detectors: The Essentials 27116.4 Gas Chromatography 27216.4.1 Choice of Gas for GC 27316.4.2 Sample Introduction in GC 27416.4.3 The GC Oven 27516.4.4 The GC Column 27716.4.5 GC Detectors 27916.4.6 Compound Derivatization for GC 28316.5 High-Performance Liquid Chromatography 28416.5.1 The Mobile Phase in HPLC 28416.5.2 Sample Introduction in HPLC 28516.5.3 The HPLC Column 28616.5.4 Detectors for HPLC 28816.6 Other Techniques for Environmental Organic Analysis 29216.6.1 Infrared Spectroscopy 29216.6.2 Nuclear Magnetic Resonance Spectrometry 29316.6.3 Portable Techniques for Field Measurements 29316.7 Applications of Chromatography in Environmental Analysis 29416.8 Summary 300Further Readings 300Section G Post-Analysis: Decision- Making 30117 Environmental Problem Solving 30317.1 Introduction 303References 327Section H Historical Context 32918 A History of Extraction Techniques and Chromatographic Analysis 33118.1 Introduction 33118.2 Application 339References 345Appendices 347SI units and Physical Constants 357Index 361

Select Guide Rating