Sample Handling and Trace Analysis of Pollutants (eBook)

Front Cover 1
Sample Handling and Trace Analysis of Pollutants: Techniques, Applications and Quality Assurance 4
Copyright Page 5
CONTENTS 6
Preface 12
PART I: FIELD SAMPLING TECHNIQUES AND SAMPLE PREPARATION 14
CHAPTER 1. SAMPLE HANDLING STRATEGIES FOR THE ANALYSIS OF ORGANIC COMPOUNDS IN ENVIRONMENTAL WATER SAMPLES 16
1.1 Introduction 17
1.2 Liquid–liquid extraction procedures 19
1.3 Supported liquid membrane extraction procedures 22
1.4 Solid-phase extraction 23
1.5 Clean-up of samples 54
1.6 On-line coupling of SPE to LC 59
1.7 Conclusion and further developments 77
References 78
CHAPTER 2. SEPARATION, CLEAN-UP AND RECOVERIES OF PERSISTENT TRACE ORGANIC CONTAMINANTS FROM SOILS, SEDIMENT AND BIOLOGICAL MATRICES 86
2.1 Introduction 86
2.2 Sample preservation and storage 88
2.3 Recoveries 91
2.4 Extraction 93
2.5 Clean-up and group separation 107
2.6 Group separation and multi-residue schemes 115
2.7 Confirmatory methods 119
2.8 Quality assurance and interlaboratory studies 120
2.9 Hyphenated techniques 120
2.10 Health and safety 121
References 122
CHAPTER 3. APPLICATIONS OF MICROWAVE-ASSISTED EXTRACTION IN ENVIRONMENTAL ANALYSIS 128
3.1 Sample preparation techniques in environmental analysis 128
3.2 Fundamentals of MAE 130
3.3 Instrumentation 134
3.4 Applications of microwave-assisted extraction 138
3.5 Future directions 164
References 164
CHAPTER 4. SAMPLE HANDLING AND ANALYSIS OF PESTICIDES AND THEIR TRANSFORMATION PRODUCTS IN WATER MATRICES BY LIQUID CHROMATOGRAPHIC TECHNIQUES 168
4.1 Introduction 168
4.2 Sample handling (extraction and clean-up) 172
4.3 LC determination of pesticides (except MS detection) 194
4.4 LC-MS 205
4.5 Conclusions 215
Acknowledgements 216
References 216
PART II: APPLICATION AREAS 222
CHAPTER 5. ENVIRONMENTAL APPLICATIONS OF GAS CHROMATOGRAPHY-ATOMIC EMISSION DETECTION 224
5.1 Introduction 224
5.2 Instrumentation 225
5.3 Applications 227
5.4 Conclusion 249
References 249
CHAPTER 6. METHODS FOR THE DETERMINATION AND EVALUATION OF CHLORINATED BIPHENYLS (CBs) IN ENVIRONMENTAL MATRICES 252
6.1 Introduction 253
6.2 Sources of PCBs 255
6.3 Compound selection 256
6.4 Matrix extraction 259
6.5 Clean-up 268
6.6 Group separation 271
6.7 LC-GC combinations 273
6.8 Analytical chromatography 276
6.9 Detection 280
6.10 Quality assurance 285
6.11 Data interpretation 288
References 291
CHAPTER 7. IMMUNOASSAYS FOR ENVIRONMENTAL ANALYSIS 300
7.1 Introduction 302
7.2 Types of immunoassays 304
7.3 Antibodies 317
7.4 Hapten design 321
7.5 Conjugation procedures using proteins or enzymes 326
7.6. Immunoassay features 331
7.7 Matrix effect 335
7.8 Validation studies 342
7.9 Conclusions and future developments 343
Acknowledgements 344
References 344
CHAPTER 8. COUPLED-COLUMN LC (LC/LC) IN ENVIRONMENTAL TRACE ANALYSIS OF POLAR PESTICIDES 354
8.1 Introduction 354
8.2 Coupled-column liquid chromatography (LC/LC) 355
8.3 LC/LC-UV 358
8.4 LC/LC with selective detection 378
8.5 Systematic method-development 382
8.6 Conclusions 388
Acknowledgements 388
References 388
CHAPTER 9. LIQUID CHROMATOGRAPHIC AND BIORECOGNITION TECHNIQUES FOR THE DETERMINATION OF PHENOLS AND THEIR SUBSTITUTED DERIVATIVES IN WATER SAMPLES 392
9.1 Introduction 392
9.2 Sampling strategies for water analysis using membrane-based analysis 394
9.3 Separation techniques and detection principles for the determination of phenols 397
9.4 Solid phase extraction methodology 403
9.5 CLC-biosensor detection 406
9.6 Biosensor developments 410
9.7 Immuno-based bio-recognition for the analysis of other pesticides 418
References 423
CHAPTER 10. HPLC METHODS FOR THE DETERMINATION OF MYCOTOXINS AND PHYTOTOXINS 426
10.1 Introduction 426
10.2 Mycotoxins 427
10.3 Phycotoxins 445
References 461
CHAPTER 11. DETERMINATION OF RADIONUCLIDES IN ENVIRONMENTAL SAMPLES 470
11.1 Introduction 471
11.2 Radioactive nuclides in nature 471
11.3 Technologically modified exposure to natural radiation 476
11.4 Pathways and samples of interest 481
11.5 Collection and preparation of samples 484
11.6 Measurements of radioactivity 488
11.7 Conclusions 543
References 543
CHAPTER 12. DETERMINATION OF ORGANIC POLLUTANTS IN INDUSTRIAL WASTEWATER EFFLUENTS 550
12.1 General introduction 550
12.2 Sample preparation methods 553
12.3 Mass spectrometric characterization: GC–MS and LC–MS 560
12.4 Rapid biological measurements 571
12.5 Wastewater monitoring 579
12.6 Conclusions and future developments 593
Acknowledgements 593
References 594
CHAPTER 13. MINE WASTE CHARACTERIZATION 598
13.1 Mine waste 598
13.2 Sampling 600
13.3 Sample preparation 601
13.4 Physical properties 602
13.5 Chemical properties 608
13.6 Conclusions 632
Acknowledgements 632
References 632
PART III: QUALITY ASSURANCE, REFERENCE MATERIALS AND CHEMOMETRICS 636
CHAPTER 14. CERTIFIED REFERENCE MATERIALS FOR THE QUALITY CONTROL OF MEASUREMENTS IN ENVIRONMENTAL MONITORING 638
14.1 Particular aspects of environmental analysis 638
14.2 Reliability of data 639
14.3 The need for accuracy 640
14.4 How to achieve accuracy 640
14.5 Use of CRMs 645
14.6 Requirements for certified reference materials 648
14.7 CRMs for environmental monitoring 657
14.8 Conclusion 658
References 658
CHAPTER 15. STANDARD REFERENCE MATERIALS FOR THE DETERMINATION OF TRACE ORGANIC CONSTITUENTS IN ENVIRONMENTAL SAMPLES 662
15.1 Introduction 662
15.2 Modes of certification 663
15.3 Types of environmental SRMs 665
15.4 Analytical approach for the certification of natural matrix SRMs 669
15.5 Recent SRM activities 678
Acknowledgements 698
References 699
CHAPTER 16. INTERPRETATION OF ENVIRONMENTAL DATA USING CHEMOMETRICS 702
16.1 Introduction 702
16.2 Multivariate analysis of environmental data 703
16.3 Examples of application 720
References 747
PART IV: EMERGING TECHNIQUES 750
CHAPTER 17. APPLICATION OF CAPILLARY ELECTROPHORESIS IN ENVIRONMENTAL ANALYSIS 752
17.1 General introduction 753
17.2 CE techniques 755
17.3 Detection techniques in capillary electrophoresis 758
17.4 Trace enrichment in capillary electrophoresis 764
17.5 Environmental applications 775
17.6 Environmental applications of CE–MS detection 791
17.7 Conclusions and future developments 796
Acknowledgements 797
References 797
CHAPTER 18. APPLICATION OF FLUORESCENCE SPECTROSCOPIC TECHNIQUES IN THE DETERMINATION OF PAHS AND PAH METABOLITES 802
18.1 Introduction 802
18.2 Fluorescence spectroscopy 804
18.3 Applications 811
18.4 Conclusions 836
References 837
CHAPTER 19. APPLICATIONS OF LIQUID CHROMATOGRAPHY-MASS SPECTROMETRY IN ENVIRONMENTAL CHEMISTRY CHARACTERISATION AND DETERMINATION OF SURFACANTS AND THEIR METABOLITES IN WATER SAMPLES BY MODERN MASS SPECTROMETRIC TECHNIQUES
19.1 Introduction 841
19.2 Pretreatment and separation 848
19.3 FIA- and LC-MS detection of surfactants and their metabolites in standard mixtures, industrial blends, spiked and real environmental samples 850
19.4 Identification of surfactants and their metabolites by MS-MS using flow injection analysis (FIA-MS-MS) or after LC-separation (LC-MS-MS) 903
19.5 Quantification of surfactants and their metabolites by flow injection analysis (FIA) and after LC-separation in combination with MS-detection 927
19.6 Conclusions 933
References 942
CHAPTER 20. LC/MS INTERFACING SYSTEMS IN ENVIRONMENTAL ANALYSIS: APPLICATIONS TO POLAR PESTICIDES 948
20.1 Introduction 948
20.2 LC/MS interfaces 950
20.3 Applications 964
20.4 Conclusions 1005
Acknowledgements 1008
References 1008
CHAPTER 21. ORGANOMETALLIC COMPOUND DETERMINATION IN THE ENVIRONMENT BY HYPHENATED TECHNIQUES 1016
21.1 Introduction 1018
21.2 Flow injection analysis 1021
21.3 Volatilization reactions, cryogenic trapping, chromatographic separation and atomic spectrometry detection 1024
21.4 Separation by gas chromatography 1032
21.5 Separation by liquid chromatography 1052
21.6 Conclusion 1078
References 1079
CHAPTER 22. FUNDAMENTALS AND APPLICATIONS OF BIOSENSORS FOR ENVIRONMENTAL ANALYSIS 1088
22.1 Introduction 1088
22.2 Transducer technology 1090
22.3 Biorecognition principle 1100
22.4 Conclusions 1113
Acknowledgements 1114
References 1114
Subject index 1120