Extraction Techniques for Environmental Analysis

Explore the analytical approach to extraction techniques

In Extraction Techniques for Environmental Analysis, accomplished environmental scientist and researcher John R. Dean delivers a comprehensive discussion of the extraction techniques used for organic compounds relevant to environmental analysis. In the book, extraction techniques for aqueous, air, and solid environmental matrices are explored and case studies that highlight those techniques are included.

Readers will find in-depth treatments of specific extraction techniques suitable for adoption in their own laboratories, as well as reviews of relevant analytical techniques used for the analysis of organic compound extracts (with a focus on chromatographic separation and detection).

Extraction Techniques for Environmental Analysis also includes a chapter that extensively covers the requirements for an analytical laboratory, including health and safety standards, as well as:

• A thorough introduction to pre-sampling, as well as the extraction of aqueous samples, including the classical approach for aqueous extraction and solid phase extraction
• Comprehensive explorations of the extraction of gaseous samples, including air sampling
• Practical discussions of the extraction of solid samples, including pressurized fluid extraction and microwave-assisted extraction
• In-depth examinations of post-extraction procedures, including pre-concentration using solvent evaporation

Extraction Techniques for Environmental Analysis is a must-read resource for undergraduate students of applied chemistry, as well as postgraduates taking analytical chemistry courses or courses in related disciplines, like forensic or environmental science.

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.

Section A: Initial Considerations

1. The Analytical Approach

Learning objectives

1.0 Introduction

1.1 Environmental organic compounds of concern

1.2 Essentials of practical work

1.3 Health and safety

1.4 Considerations for data presentation

1.5 Use and determination of significant figures

1.6 Units

1.7 Calibration and quantitative analysis

1.8 Terminology in quantitative analysis

1.9 Preparing solutions for quantitative work

1.10 Calibration graphs

1.11 The internal standard

1.12 Limits of detection / quantitation

1.13 Dilution or concentration factors

1.14 Quality assurance

1.15 Use of certified reference materials

1.16 Applications

Further Reading

Section B: Sampling

2. Sampling and storage

Learning objectives

2.0 Introduction

2.1 Sampling strategy

2.2 Types of aqueous matrices

2.3 Types of soil matrices

2.4 Physicochemical properties of water and solid environmental matrices

2.4.1 Aqueous (water) samples

2.4.2 Solid (soil) samples

2.5 Sampling soil (and/or sediment)

2.6 Sampling water

2.7 Sampling air

2.8 Sampling and analytical operations inter-relationships and terminology

2.9 Storage of samples

2.9.1 Choice of storage container for liquid samples

2.9.2 Cleaning of storage container for liquid samples

2.10 Preservation techniques for liquid samples

2.11 Preservation techniques for solid samples

2.12 Preservation techniques for gaseous samples

2.13 Applications

Reference

Section C: Extraction of Aqueous Samples

3. Classical approach for aqueous extraction

Learning objectives

3.0 Introduction

3.1 Liquid-liquid extraction

3.1.1 Theory of liquid-liquid extraction

3.1.2 Selection of solvents

3.1.3 Solvent extraction

3.1.4 Problems with the liquid-liquid extraction process and their remedies

3.2 Liquid microextraction techniques

3.2.1 Single drop microextraction (SDME)

3.2.2 Dispersive liquid-liquid microextraction (DLLME)

3.3 Purge and trap

3.4 Headspace extraction

3.4.1 Procedure for static headspace sampling

3.4.2 Procedure for dynamic headspace sampling

3.5 Application

4. Solid phase extraction

Learning objectives

4.0 Introduction

4.1 Types of SPE sorbent

4.2 SPE formats and apparatus

4.3 Method of SPE operation

4.4 Solvent selection

4.5 Factors affecting SPE

4.6 Selected methods of analysis for SPE

4.6.1 Application of reversed phase SPE

4.6.2 Application of normal phase SPE

4.6.3 Application of ion exchange SPE

4.6.4 Application of mixed mode SPE

4.7 Automation and on-line SPE

4.8 Applications

4.9 Summary

References

5. Solid phase microextraction

Learning objectives

5.0 Introduction

5.1 Theoretical considerations for SPME

5.2 Practical considerations for SPME

5.2.1 SPME agitation methods

5.2.2 Other SPME operating considerations

5.3 Application of SPME

5.4 Summary

Reference

6. In-Tube extraction

Learning objectives

6.0 Introduction

6.1 Microextraction in a packed syringe (MEPS)

6.1.1 Procedure for MEPS

6.1.2 Main issues in MEPS

6.2 In-tube extraction (ITEX)

6.2.1 Procedure for ITEX-DHS

6.3 Application of ITEX-DHS

6.4 Summary

7. Stir-bar sorptive extraction

Learning objectives

7.0 Introduction

7.1 Theoretical considerations for SBSE

7.2 Practical issues for SBSE

7.2.1 Main issues in SBSE

7.3 Application of SBSE

7.4 Summary

8. Membrane extraction

Learning objectives

8.0 Introduction

8.1 Theoretical considerations for membrane extraction

8.1.1 Mass transfer coefficient model

8.1.2 Chemical reaction kinetic model

8.2 Passive sampling devices

8.3 Application of passive sampling using Chemcatcher®

8.4 Summary

Reference

Section D: Extraction of Solid Samples

9.0 Classical approaches for extraction of solid samples

Learning objectives

9.0 Introduction

9.1 Theory of liquid-solid extraction

9.2 Soxhlet extraction

9.2.1 Experimental

9.3 Soxtec extraction

9.4 Ultrasonic extraction

9.4.1 Experimental

9.5 Shake flask extraction

9.5.1 Experimental

9.6 Application

Reference

10. Pressurised liquid extraction

Learning objectives

10.0 Introduction

10.1 Theoretical considerations relating to extraction process

10.1.2 Disruption of surface equilibrium (by temperature and pressure)

10.2 Instrumentation for PLE

10.3 A typical procedure for PLE

10.4 In-situ clean-up or selective PLE

10.5 Method development for PLE

10.5.1 Pre-extraction considerations

10.5.2 Packing the extraction vessel

10.6 Applications of PLE

10.7 Summary

References

11. Microwave-assisted extraction

Learning objectives

11.0 Introduction

11.1 Theoretical considerations for MAE

11.1.1 Selecting an organic solvent for MAE

11.1.2 Heating methods

11.1.3 Calibration of a microwave instrument

11.2 Instrumentation for MAE

11.3 A typical procedure for MAE

11.4 Applications of MAE

11.5 Summary

References

12. Matrix Solid phase dispersion

Learning objectives

12.0 Introduction

12.1 Practical considerations for MSPD

12.2 Optimization of MSPD

12.3 Application of MSPD

12.4 Summary

13. Supercritical fluid extraction

Learning objectives

13.0 Introduction

13.1 Theoretical considerations for SFE

13.2 Supercritical CO2

13.3 Instrumentation for SFE

13.4 A typical procedure for SFE

13.5 Application of SFE

13.6 Summary

References

Section E: Extraction of Gaseous Samples

14. Air sampling

Learning objectives

14.0 Introduction

14.1 Techniques used for air sampling

14.1.1 whole air collection

14.1.2 Enrichment onto solid sorbents

14.2 Thermal desorption

14.3 Workplace exposure limits

14.4 Biological monitoring

14.5 Particulate matter

14.6 Application of air sampling

14.7 Summary

References

Section F: Post-extraction

15. Pre-concentration and associated sample extract procedures

Learning objectives

15.0 Introduction

15.1 Solvent evaporation techniques

15.1.1 Needle evaporation

15.1.2 Automated evaporator (Turbovap)

15.1.3 Rotary evaporation

15.1.4 Kuderna-Danish evaporative concentration

15.1.5 Automated evaporative concentration system

15.2 Post-extract evaporation

15.3 Sample extract clean-up procedures

15.3.1 Column chromatography

15.3.2 Acid-alkaline partition

15.3.3 Acetonitrile-hexane partition

15.3.4 Sulfur clean-up

15.3.5 Alkaline decomposition

15.4 Derivatization for gas chromatography

15.5 Application of pre-concentration for analysis

References

16. Instrumental Techniques for Environmental Organic Analysis

Learning objectives

16.0 Introduction

16.1 Theory of chromatography

16.2 Chromatography detectors: The essentials

16.3 Gas chromatography

16.3.1 Choice of gas for GC

16.3.2 Sample introduction in GC

16.3.3 The GC oven

16.3.4 The GC column

16.3.5 GC detectors

16.3.6 Compound derivatization for GC

16.4 High performance liquid chromatography

16.4.1 The mobile phase in HPLC

16.4.2 Sample introduction in HPLC

16.4.3 The HPLC column

16.4.4 Detectors for HPLC

16.5 Other techniques for environmental organic analysis

16.5.1 Infra-red spectroscopy

16.5.2 Nuclear magnetic resonance spectrometry

16.5.3 Portable techniques for field measurements

16.6 Applications of chromatography in environmental analysis

16.7 Summary

16.8 Further reading

References

Section G: Post-analysis: Decision making

17. Environmental problem solving

Learning objectives

17.0 Introduction

17.1 Case study 1. Defining the problem: Initial planning and considerations

17.2 Case study 2. A consideration of the whole concept of environmental analysis

17.3 Case study 3. Environmental Chemistry Escape Room

 References

Section H: Historical context

18. A history of extraction techniques and chromatographic analysis

Learning objectives

18.0 Introduction

18.1 Application

References

Appendices: Crossword puzzles to aid learning and understanding

Appendix A1: A crossword of key terms in Chapters 4 to 8: extraction techniques for aqueous samples.

Appendix A2: A crossword of key terms in Chapters 10 to 13: extraction techniques for solid samples.

Appendix A3: A crossword for key terms on instrumental techniques for environmental organic analysis.

Crossword solutions

SI units and Physical Constants

Periodic Table

Index

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