Sample Preparation for Trace Element Analysis
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Table of contents
- Cover
- Contentsxv
- Contributors to Vol XLIvi
- Volumes in the Seriesxiii
- Series Editor’s Prefacexliii
- Prefacexliv
- Acronymsxlvi
- Chapter 1. Sampling and sample preservation for trace element analysis1
- 1.1 Introduction1
- 1.2 Preliminary considerations2
- 1.3 Types of samples3
- 1.4 Planning the sampling operation5
- 1.5 Statistical sampling8
- 1.6 Sample handling and preservation during collection, transport, and storage14
- 1.7 Quality assurance in sampling [24,25]17
- 1.8 Glossary18
- References20
- Selected bibliography21
- Chapter 2. Sources of analyte contamination and loss during the analytical process23
- 2.1 Introduction23
- 2.2 Contamination24
- 2.3 Losses29
- 2.4 Sampling34
- 2.5 Storage35
- 2.6 Drying and homogenisation37
- 2.7 Dilution, dissolution and digestion39
- 2.8 Separation and preconcentration41
- 2.9 Element measurement42
- References42
- Chapter 3. Calibration approaches for trace element determination47
- 3.1 Introduction47
- 3.2 Basic assumptions and some terminology48
- 3.3 Selection of the calibration approach49
- 3.4 Statistical evaluation of recovery data52
- 3.5 Linear regression55
- 3.6 External calibration67
- 3.7 Method of standard additions74
- 3.8 Internal standardization79
- 3.9 Isotope dilution81
- Acknowledgements90
- References90
- Chapter 4. Stated references for ensuring traceability of trace element analysis93
- 4.1 Introduction93
- 4.2 Meaning of traceability for chemical measurements94
- 4.3 SI units96
- 4.4 Documented standards96
- 4.5 Reference methods97
- 4.6 Reference materials99
- 4.7 Specimen banking105
- 4.8 Proficiency testing105
- 4.9 Real-case achievement of traceability of trace element analysis106
- 4.10 Conclusions113
- References114
- Chapter 5. Detection methods for the quantitation of trace elements117
- 5.1 Introduction117
- 5.2 Classical methods117
- 5.3 Flame spectrometry118
- 5.4 Electrothermal AAS135
- 5.5 Inductively coupled plasma-atomic emission spectrometry142
- 5.6 Inductively coupled plasma-mass spectrometry152
- 5.7 Atomic Fluorescence spectrometry160
- 5.8 Other atomic absorption, emission and Fluorescence methods of detection164
- 5.9 Secondary ion mass spectrometry165
- 5.10 Glow discharge mass spectrometry171
- 5.11 X-ray Fluorescence spectrometry176
- 5.12 UV/Visible spectrophotometric and chemiluminescence techniques179
- 5.13 Electrochemical methods183
- References186
- SECTION - 1: DIGESTION AND EXTRACTION APPROACHES192
- Chapter 6. Wet digestion methods193
- 6.1 Introduction and brief history193
- 6.2 Nomenclature194
- 6.3 Bibliography194
- 6.4 Reagents and vessel materials for wet digestion procedures195
- 6.5 Wet acid digestion (decomposition and dissolution) procedures199
- 6.6 Conclusions and future trends224
- References228
- Chapter 7. Dry ashing235
- 7.1 General considerations235
- 7.2 Why dry ashing?238
- 7.3 Oxidation process and dissolution of the residue240
- 7.4 Methodology244
- 7.5 Particular cases of arsenic and selenium248
- 7.6 Conclusions253
- References254
- Chapter 8. Microwave based extraction257
- 8.1 Introduction257
- 8.2 Brief history of industrial microwave devices257
- 8.3 Microwave theory258
- 8.4 Microwave laboratory equipment263
- 8.5 Vessels270
- 8.6 Control systems275
- 8.7 Methodology281
- 8.8 Sample types285
- 8.9 Advanced applications297
- 8.10 Conclusions298
- Acknowledgements299
- References299
- Chapter 9. Fusion and fluxes301
- 9.1 Introduction301
- 9.2 Fusion in lithium borates301
- 9.3 The key to successful fusion beads305
- 9.4 Application to trace element analysis308
- 9.5 Features of fusion for trace elements309
- References310
- Chapter 10. Supercritical fluid extraction313
- 10.1 Properties of supercritical fluids313
- 10.2 Instrumentation316
- 10.3 SFE of trace elements318
- 10.4 Organometallic compounds332
- 10.5 Conclusion339
- References340
- Chapter 11. Accelerated solvent extraction of organometallic and inorganic compounds343
- 11.1 Accelerated solvent extraction as a sample preparation technique343
- References352
- Chapter 12. Sonication as a sample preparation method for elemental analysis353
- 12.1 Introduction353
- 12.2 Methodological considerations354
- 12.3 Historical background357
- 12.4 Applications„sonication and sample preparation358
- 12.5 Summary366
- References366
- Chapter 13. Solid phase microextraction as a tool for trace element determination371
- 13.1 Introduction371
- 13.2 General description of solid phase microextraction373
- 13.3 Solid phase microextraction: step-by-step method development375
- 13.4 Solid phase microextraction for speciation analysis380
- 13.5 Solid phase microextraction as an investigative tool388
- 13.6 Limitations of solid phase microextraction388
- 13.7 Isotope dilution calibration in combination with solid phase microextraction389
- References390
- Chapter 14. Solid-phase extraction393
- 14.1 Introduction393
- 14.2 Theory393
- 14.3 Step-by-step method development guide410
- 14.4 Applications of SPE to the determination of some trace elements439
- 14.5 Conclusion450
- References451
- Chapter 15. Chelation solvent extraction for separation of metal ions459
- 15.1 Introduction459
- 15.2 Theoretical considerations460
- 15.3 Adsorption of metal ions using chelating resins474
- 15.4 Application of chelation to sample preparation for trace metal analysis477
- References492
- Chapter 16. Cryogenic trapping for speciation analysis495
- 16.1 Introduction495
- 16.2 Definition of volatile species502
- 16.3 Physico-chemical principles and processes associated with cryofocusing504
- 16.4 Analytical constraints509
- 16.5 Sample preservation and stability517
- 16.6 Instrumentation for cryogenic trapping and selected applications520
- References529
- Chapter 17. Biotrapping as an alternative to metal preconcentration and speciation533
- 17.1 Introduction533
- 17.2 General characteristics of biological substrates535
- 17.3 Uptake mechanisms538
- 17.4 Working procedures541
- 17.5 Applications546
- 17.6 Conclusions557
- References557
- Chapter 18 Membrane extraction559
- 18.1 Introduction559
- 18.2 Membrane extraction techniques559
- 18.3 Chemical principles for metal extraction566
- 18.4 Properties of membrane extraction566
- 18.5 Experimental set-up570
- Acknowledgements574
- References574
- Chapter 19. Derivatization and vapor generation methods for trace element analysis and speciation577
- 19.1 Introduction577
- 19.2 Theory578
- 19.3 Method development583
- 19.4 Applications585
- Acknowledgements590
- References590
- Chapter 20. Laser ablation sampling593
- 20.1 Introduction593
- 20.2 Experimental system594
- 20.3 Ablation detection systems599
- 20.4 Calibration601
- 20.5 Fractionation603
- 20.6 Conclusion604
- Acknowledgements606
- References606
- Chapter 21. Flow injection techniques for sample pretreatment611
- 21.1 Introduction611
- 21.2 FI liquid–liquid extraction systems615
- 21.3 FI solid phase extraction systems626
- 21.4 FI vapor generation systems635
- 21.5 FI gas diffusion systems641
- 21.6 FI on-line sample digestion643
- References646
- Chapter 22. Automation of sample preparation649
- 22.1 Introduction649
- 22.2 Automation of liquid sample preparation653
- 22.3 Automation of solid sample preparation659
- 22.4 Robotics660
- 22.5 Advantages and disadvantages of automation of sample preparation676
- 22.6 Future prospects677
- References678
- SECTION - 2: MATRICES682
- Chapter 23. Sample preparation for crude oil, petroleum products and polymers683
- 23.1 Introduction683
- 23.2 Sample preparation techniques and instrumentation693
- 23.3 Cleanliness and quality assurance713
- Acknowledgements718
- References719
- Chapter 24. Sample preparation of geological samples, soils and sediments723
- 24.1 Introduction723
- 24.2 Sample preparation723
- 24.3 Choice of approach728
- 24.4 Methods that do not require any sample digestion„ in situ methods of analysis730
- 24.5 Methods based on solid samples733
- 24.6 Dissolution methods based on acid attack735
- 24.7 Decomposition by molten salt fusion750
- 24.8 Pre-concentration and separation procedures753
- 24.9 Sequential extractions and dissolutions755
- 24.10 Summary and conclusions758
- References758
- Chapter 25. Sample preparation for food analysis765
- 25.1 Introduction765
- 25.2 Literature766
- 25.3 Pretreatment768
- 25.4 Classification of sample treatment methods770
- 25.5 Compilation of sample treatment methods for foods770
- 25.6 Specific cases: methods, elements, matrices839
- 25.7 Examples of specific, recommended sample treatment procedures843
- 25.8 Closing remarks846
- References847
- Chapter 26. The determination of trace elements in water857
- 26.1 Direct methods of determination857
- 26.2 Preconcentration techniques„multielement860
- 26.3 Preconcentration„individual elements865
- 26.4 Determination of trace elements as volatile species865
- 26.5 Mercury879
- 26.6 Luminescence880
- 26.7 Voltammetry885
- 26.8 Total-Reflection X-Ray Fluorescence spectrometry891
- 26.9 Conclusions894
- References894
- Chapter 27. Aerosol sampling and sample preparation for elemental analysis903
- 27.1 Introduction903
- 27.2 Sampling of aerosols906
- 27.3 Sequential extraction schemes for aerosol samples924
- 27.4 Discussion930
- Acknowledgements931
- General terms used in sampling931
- References932
- Chapter 28. Sample preparation for industrial waste analysis935
- 28.1 Types of industrial waste935
- 28.2 Safety considerations for industrial waste analysis936
- 28.3 Sample characteristics and industrial waste sampling936
- 28.4 Digestions938
- 28.5 Leach procedures950
- 28.6 Certified reference materials957
- 28.7 Summary and future developments957
- 28.8 Useful World Wide Websites960
- Acknowledgements961
- References961
- Chapter 29. Sample preparation for semiconductor materials965
- 29.1 Introduction965
- 29.2 Contamination control969
- 29.3 Sample preparation976
- 29.4 Conclusion986
- References986
- SECTION - 3: TRACE ELEMENT SPECIATION989
- Chapter 30. Sampling and sample treatment in the analysis of organotin compounds in environmental sa991
- 30.1 Introduction991
- 30.2 Critical steps in organotin analysis994
- 30.3 Improving the quality of organotin measurements in Europe1005
- 30.4 Detailed procedure for the GC–MS determination of organotin compounds in environmental sample1017
- Acknowledgements1020
- References1021
- Chapter 31. Sample preparation for arsenic speciation1027
- 31.1 Introduction1027
- 31.2 Occurrence and distribution of arsenic in the environment1028
- 31.3 Stability of arsenic compounds1033
- 31.4 Extraction of arsenic compounds from environmental samples1038
- 31.5 Conclusions1041
- References1041
- Chapter 32. Sample preparation for speciation of selenium1045
- 32.1 Why selenium speciation?1045
- 32.2 General sample preparation1045
- 32.3 Mammals1046
- 32.4 Fish/birds1050
- 32.5 Plants1051
- 32.6 Microorganisms1055
- 32.7 Environmental1055
- References1059
- Chapter 33. Sample preparation for mercury speciation1063
- 33.1 Introduction1063
- 33.2 Aqueous solution chemistry of methylmercury1063
- 33.3 Sample collection, preservation and storage1065
- 33.4 Sample preparation1069
- 33.5 Quality control1075
- Acknowledgements1079
- References1079
- Chapter 34. Sample preparation for speciation of lead1081
- 34.1 Introduction1081
- 34.2 Toxicity of organolead compounds1083
- 34.3 The history of leaded gasoline1085
- 34.4 Properties of organolead compounds1088
- 34.5 Synthesis of organolead compounds1090
- 34.6 The biogeochemical cycle of lead1092
- 34.7 Analytical techniques for speciation analysis of organolead compounds1092
- References1111
- Chapter 35. Sample preparation for chromium speciation1115
- 35.1 The element and its reactivity1115
- 35.2 The presence of Cr in nature and industrial processes1117
- 35.3 Chemical species of Cr present in real samples1118
- 35.4 Analytical methodologies available for determination of Cr1120
- 35.5 Analytical methodologies for Cr speciation in water1120
- 35.6 Analytical methodologies for Cr speciation in biological fluids1136
- 35.7 Analytical methodologies for speciation of Cr in solid samples1145
- 35.8 Final considerations1157
- References1158
- Chapter 36. Sample preparation for metal-based drugs1173
- 36.1 Introduction1173
- 36.2 Platinum-based drugs1173
- 36.3 Gold-based drugs1180
- 36.4 Mercury1181
- 36.5 Vanadium1181
- 36.6 Lead1182
- 36.7 Conclusions1182
- References1182
- Chapter 37. Sample preparation for speciation analysis for metallobiomolecules1185
- 37.1 Introduction1185
- 37.2 Elemental species in biological systems. metallobiomolecules1186
- 37.3 Tailoring sample preparation: definition of the analyte moiety1188
- 37.4 Homogenization and analyte recovery using unreactive buffers1188
- 37.5 Analyte recovery through partial degradation of sample matrix1190
- 37.6 Fractionation of metal species according to the molecular weight prior to analytical chromatogr1193
- 37.7 Multidimensional LC clean-up procedures prior to characterization of metal species by electrosp1195
- 37.8 Sample preparation prior to speciation analysis of biological fluids1196
- 37.9 Sample preparation prior to speciation analysis in solid matrices1200
- 37.10 Sources of error1205
- References1206
- Chapter 38. Sample preparation for the analysis of volatile metals species1211
- 38.1 Introduction1211
- 38.2 Species of interest1212
- 38.3 Characterization of gas samples1216
- 38.4 Sample preparation strategies1216
- 38.5 Specific procedures1222
- 38.6 Problems and future studies1229
- References1230
- Chapter 39. Sequential extraction1233
- 39.1 Sequential extraction procedures: a special case of sample dissolution1233
- 39.2 Types, uses and limitations of SEPs1235
- 39.3 Sample pre-treatment for SEPs1246
- 39.4 Application of other extraction techniques to SEPs1250
- 39.5 Quality control for SEPs1252
- References1253
- Index1257
Following the collection of a sample, every analytical chemist will agree that its subsequent preservation and processing are of paramount importance. The availability of high performance analytical instrumentation has not diminished this need for careful selection of appropriate pretreatment methodologies, intelligently designed to synergistically elicit optimum function from these powerful measurement tools.
Sample Preparation for Trace Element Analysis is a modern, comprehensive treatise, providing an account of the state-of-the art on the subject matter. The book has been conceived and designed to satisfy the varied needs of the practicing analytical chemist. It is a multi-author work, reflecting the diverse expertise arising from its highly qualified contributors.
The first five chapters deal with general issues related to the determination of trace metals in varied matrices, such as sampling, contamination control, reference materials, calibration and detection techniques. The second part of the book deals with extraction and sampling technologies (totaling 15 chapters), providing theoretical and practical hints for the users on how to perform specific extractions. Subsequent chapters overview seven major representative matrices and the sample preparation involved in their characterization. This portion of the book is heavily based on the preceding chapters dealing with extraction technologies. The last ten chapters are dedicated to sample preparation for trace element speciation.
- First title to provide comprehensive sample preparation information, dealing specifically with the analysis of samples for trace elements.
- The 39 chapters are authored by international leaders of their fields.
Sample Preparation for Trace Element Analysis is a modern, comprehensive treatise, providing an account of the state-of-the art on the subject matter. The book has been conceived and designed to satisfy the varied needs of the practicing analytical chemist. It is a multi-author work, reflecting the diverse expertise arising from its highly qualified contributors.
The first five chapters deal with general issues related to the determination of trace metals in varied matrices, such as sampling, contamination control, reference materials, calibration and detection techniques. The second part of the book deals with extraction and sampling technologies (totaling 15 chapters), providing theoretical and practical hints for the users on how to perform specific extractions. Subsequent chapters overview seven major representative matrices and the sample preparation involved in their characterization. This portion of the book is heavily based on the preceding chapters dealing with extraction technologies. The last ten chapters are dedicated to sample preparation for trace element speciation.
- First title to provide comprehensive sample preparation information, dealing specifically with the analysis of samples for trace elements.
- The 39 chapters are authored by international leaders of their fields.