Sample Preparation for Trace Element Analysis

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ISBN: 9780444511010 | 0444511016
Cover: Hardcover
Copyright: 12/16/2003

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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.

Contributors to Vol XLI

Volumes in the Series

xiii

Series Editor's Preface

xiiii

Preface

xliv

Acronyms

xlvi

Chapter 1. Sampling and sample preservation for trace element analysis

(22)

Byron Kratochvil

1.1 Introduction

(1)

1.2 Preliminary considerations

(1)

1.2.1 Sampling variability

(1)

1.2.2 Sampling strategies

(1)

1.2.3 Uncertainties in sampling

(1)

1.3 Types of samples

(2)

1.3.1 Judgment samples

(1)

1.3.2 Random samples

(1)

1.3.3 Systematic samples

(1)

1.3.4 Subsamples

(1)

1.3.5 Composite samples

(1)

1.4 Planning the sampling operation

(3)

1.4.1 Defining goals

(1)

1.4.2 Sampling plans

(2)

1.5 Statistical sampling

(6)

1.5.1 Introduction

(1)

1.5.2 Minimum number of increments

(1)

1.5.3 Minimum size of increments in well-mixed particulate populations

(1)

1.5.4 Sample increment size in segregated populations

(1)

1.5.5 From where should increments be taken?

(1)

1.5.6 Model-based sampling

(1)

1.5.7 Balancing economic factors and purpose of data collection against sample quality

(1)

1.6 Sample handling and preservation during collection, transport, and storage

(3)

1.6.1 Handling and storage of samples

(2)

1.6.2 Sampling equipment

(1)

1.6.3 Sample containers

(1)

1.7 Quality assurance in sampling [24,25]

(1)

1.7.1 Overall objectives

(1)

1.7.2 Quality control

(1)

1.7.3 Quality assessment

(1)

1.8 Glossary

(2)

References

(1)

Selected bibliography

(2)

Chapter 2. Sources of analyte contamination and loss during the analytical process

(24)

Gunter Knapp and Peter Schramel

2.1 Introduction

(1)

2.2 Contamination

(5)

2.2.1 Materials

(3)

2.2.2 Reagents

(1)

2.2.3 Airborne particles

(1)

2.3 Losses

(5)

2.4 Sampling

(1)

2.5 Storage

(2)

2.6 Drying and homogenisation

(2)

2.7 Dilution, dissolution and digestion

(2)

2.8 Separation and preconcentration

(1)

2.9 Element measurement

(1)

References

(5)

Chapter 3. Calibration approaches for trace element determination

(46)

Douglas C. Baxter and Ilia Rodushkin

3.1 Introduction

(1)

3.2 Basic assumptions and some terminology

(1)

3.3 Selection of the calibration approach

(3)

3.4 Statistical evaluation of recovery data

(3)

3.5 Linear regression

(12)

3.5.1 Ordinary linear regression

(3)

3.5.2 Weighted linear regression

(5)

3.5.3 Linear regression for data with uncertainties in both variables

(3)

3.6 External calibration

(7)

3.6.1 Estimating uncertainty

(2)

3.6.2 Optimizing precision

(2)

3.6.3 Accounting for non-constant sensitivity

(2)

3.7 Method of standard additions

(5)

3.7.1 Estimating uncertainty

(1)

3.7.2 Optimizing precision

(2)

3.7.3 Accounting for non-constant sensitivity

(1)

3.8 Internal standardization

(2)

3.8.1 Estimating uncertainty

(1)

3.8.2 Optimizing precision

(1)

3.9 Isotope dilution

(9)

3.9.1 Mass discrimination and detector dead time

(1)

3.9.2 Estimating uncertainty

(2)

3.9.3 Optimizing precision

(2)

Acknowledgements

(1)

References

(3)

Chapter 4. Stated references for ensuring traceability of trace element analysis

(24)

Philippe Quevauviller

4.1 Introduction

(1)

4.2 Meaning of traceability for chemical measurements

(2)

4.3 SI units

(1)

4.4 Documented standards

(1)

4.5 Reference methods

(2)

4.6 Reference materials

(6)

4.6.1 The various categories of materials and related requirements

(1)

4.6.2 Production

100

(2)

4.6.3 Methods used for material characterisation or certification

102

(1)

4.6.4 Use of reference materials

102

(1)

4.6.5 Traceability of reference materials

103

(2)

4.7 Specimen banking

105

(1)

4.8 Proficiency testing

105

(1)

4.9 Real-case achievement of traceability of trace element analysis

106

(7)

4.9.1 Total trace element determinations

106

(2)

4.9.2 Operationally defined trace element determinations

108

(2)

4.9.3 Determinations of chemical forms of elements

110

(3)

4.10 Conclusions

113

(1)

References

114

(3)

Chapter 5. Detection methods for the quantitation of trace elements

117

(76)

Les Ebdon, Andrew S. Fisher, Maria Betti and Maurice Leroy

5.1 Introduction

117

(1)

5.2 Classical methods

117

(1)

5.3 Flame spectrometry

118

(17)

5.3.1 Introduction

118

(1)

5.3.2 Theory

118

(1)

5.3.3 Instrumentation

119

(2)

5.3.4 Interferences and background correction techniques

121

(2)

5.3.5 Conventional nebulisation

123

(4)

5.3.6 Alternative methods of sample introduction

127

(8)

5.4 Electrothermal AAS

135

(7)

5.4.1 Introduction

135

(1)

5.4.2 Conventional ET-AAS

136

(3)

5.4.3 Multi-element ET-AAS

139

(1)

5.4.4 Chemical vapour generation-ET-AAS

140

(1)

5.4.5 Speciation

141

(1)

5.5 Inductively coupled plasma-atomic emission spectrometry

142

(10)

5.5.1 Introduction

142

(1)

5.5.2 Theory and interferences

142

(1)

5.5.3 Instrumentation

143

(9)

5.5.4 Figures of merit

152

(1)

5.6 Inductively coupled plasma-mass spectrometry

152

(8)

5.6.1 Introduction

152

(1)

5.6.2 Theory

153

(1)

5.6.3 Instrumentation

154

(2)

5.6.4 Different types of analysis

156

(1)

5.6.5 Interferences

156

(2)

5.6.6 Sample introduction techniques

158

(2)

5.6.7 Figures of merit

160

(1)

5.7 Atomic fluorescence spectrometry

160

(4)

5.7.1 Introduction

160

(2)

5.7.2 Theory

162

(1)

5.7.3 Instrumentation

162

(1)

5.7.4 Sample introduction

163

(1)

5.7.5 Interferences

163

(1)

5.7.6 Figures of merit

163

(1)

5.8 Other atomic absorption, emission and fluorescence methods of detection

164

(1)

5.8.1 Microwave induced plasma

164

(1)

5.8.2 Direct current plasma

165

(1)

5.9 Secondary ion mass spectrometry

165

(6)

5.9.1 Introduction

165

(2)

5.9.2 Practical principles

167

(1)

5.9.3 Sensitivity and quantification

168

(3)

5.10 Glow discharge mass spectrometry

171

(5)

5.10.1 Introduction

171

(2)

5.10.2 Glow discharge processes

173

(2)

5.10.3 Applications to trace element analysis

175

(1)

5.11 X-ray fluorescence spectrometry

176

(3)

5.11.1 Introduction

176

(1)

5.11.2 Instrumentation

177

(1)

5.11.3 Matrix effects

177

(1)

5.11.4 Quantitative and trace analysis

178

(1)

5.12 UV/Visible spectrophotometric and chemiluminescence techniques

179

(4)

5.12.1 UV/Visible spectrophotometric techniques

179

(2)

5.12.2 Molecular fluorescence and chemiluminescence detection

181

(2)

5.13 Electrochemical methods

183

(3)

5.13.1 Differential pulse anodic stripping voltammetry

183

(1)

5.13.2 Cathodic and adsorptive stripping voltammetry

184

(1)

5.13.3 Ion selective electrodes

185

(1)

References

186

(7)

DIGESTION AND EXTRACTION APPROACHES

Chapter 6. Wet digestion methods

193

(42)

Henryk Matusiewicz

6.1 Introduction and brief history

193

(1)

6.2 Nomenclature

194

(1)

6.3 Bibliography

194

(1)

6.4 Reagents and vessel materials for wet digestion procedures

195

(4)

6.5 Wet acid digestion (decomposition and dissolution) procedures

199

(25)

6.5.1 Open systems

199

(4)

6.5.2 Closed systems

203

(7)

6.5.3 Flow systems

210

(3)

6.5.4 Vapor-phase acid digestion (gas-phase reactions)

213

(3)

6.5.5 Efficiency of wet digestion (decomposition and dissolution) procedures

216

(3)

6.5.6 Comparison of wet digestion techniques

219

(1)

6.5.7 Digestion systems (instrumentation, equipment, automation)

220

(1)

6.5.8 Safety of acid digestions (sample acid digestion safety)

221

(3)

6.6 Conclusions and future trends

224

(4)

References

228

(7)

Chapter 7. Dry ashing

235

(22)

Michel Hoenig

7.1 General considerations

235

(3)

7.2 Why dry ashing?

238

(2)

7.3 Oxidation process and dissolution of the residue

240

(4)

7.3.1 Particular case of plant matrices

243

(1)

7.4 Methodology

244

(4)

7.4.1 Heating devices

244

(1)

7.4.2 Ashing vessels

245

(1)

7.4.3 Influence of the sample composition

246

(1)

7.4.4 Operating modes for environmental samples

246

(2)

7.5 Particular cases of arsenic and selenium

248

(5)

7.5.1 Ashing aids

250

(1)

7.5.2 What to do?

251

(2)

7.6 Conclusions

253

(1)

References

254

(3)

Chapter 8. Microwave based extraction

257

(44)

Edward E. King and David Barclay

8.1 Introduction

257

(1)

8.2 Brief history of industrial microwave devices

257

(1)

8.3 Microwave theory

258

(5)

8.4 Microwave laboratory equipment

263

(7)

8.4.1 Magnetron

264

(3)

8.4.2 Power application

267

(1)

8.4.3 Waveguide

267

(1)

8.4.4 Microwave cavity

267

(1)

8.4.5 Reflected energy

267

(1)

8.4.6 Mode stirrer and turntables

268

(1)

8.4.7 Microwave compatible materials

269

(1)

8.5 Vessels

270

(5)

8.5.1 Materials

271

(1)

8.5.2 Structural components

272

(1)

8.5.3 Safety

272

(1)

8.5.4 Closed vessels

273

(1)

8.5.5 Vent and reseal vessels

274

(1)

8.5.6 Open vessels

274

(1)

8.6 Control systems

275

(6)

8.6.1 Power/time

275

(1)

8.6.2 Pressure

275

(3)

8.6.3 Temperature

278

(2)

8.6.4 Power optimization feedback

280

(1)

8.7 Methodology

281

(4)

8.7.1 Pressurized closed vessel extractions

282

(1)

8.7.2 Atmospheric open vessel extractions

283

(2)

8.8 Sample types

285

(12)

8.8.1 Inorganic

285

(1)

8.8.2 Leaches and other partial extractions

286

(1)

8.8.3 Complete dissolutions

287

(1)

8.8.4 High-temperature extractions

288

(2)

8.8.5 Complex sequential extractions

290

(1)

8.8.6 Organic

291

(1)

8.8.7 Carbohydrates

292

(1)

8.8.8 Proteins

293

(1)

8.8.9 Fats, oils, and waxes

294

(3)

8.9 Advanced applications

297

(1)

8.9.1 Clean chemistry

297

(1)

8.9.2 Concentration/evaporation

297

(1)

8.10 Conclusions

298

(1)

Acknowledgements

299

(1)

References

299

(2)

Chapter 9. Fusion and fluxes

301

(12)

Fernand Claisse

9.1 Introduction

301

(1)

9.2 Fusion in lithium borates

301

(4)

9.2.1 General

301

(4)

9.3 The key to successful fusion beads

305

(3)

9.3.1 The concept of "neutrality"

305

(1)

9.3.2 The optimal flux and crystallization

306

(1)

9.3.3 Cracking of fused beads

307

(1)

9.3.4 Loss and retention of sulfur

308

(1)

9.4 Application to trace element analysis

308

(1)

9.4.1 Maximizing X-ray intensities

308

(1)

9.4.2 Minimizing background

309

(1)

9.5 Features of fusion for trace elements

309

(1)

References

310

(3)

Chapter 10. Supercritical fluid extraction

313

(30)

Roberto Alzaga, Sergi Diez and Josep M. Bayona

10.1 Properties of supercritical fluids

313

(3)

10.2 Instrumentation

316

(2)

10.2.1 Experimental solubility measurements

318

(1)

10.3 SFE of trace elements

318

(14)

10.3.1 Ligand solubility in SFs

326

(2)

10.3.2 Complex-SF solubility

328

(1)

10.3.3 SFE process

328

(4)

10.4 Organometallic compounds

332

(7)

10.4.1 Organotin compounds

332

(6)

10.4.2 Organomercury compounds

338

(1)

10.4.3 Organolead compounds

339

(1)

10.4.4 Arsenic compounds

339

(1)

10.5 Conclusion

339

(1)

References

340

(3)

Chapter 11. Accelerated solvent extraction of organometallic and inorganic compounds

343

(10)

John L. Ezzell

11.1 Accelerated solvent extraction as a sample preparation technique

343

(9)

11.1.1 Introduction

343

(1)

11.1.2 Basic principles of ASE operation

344

(1)

11.1.3 ASE instrumentation

345

(1)

11.1.4 ASE methods development

346

(3)

11.1.5 Application areas

349

(2)

11.1.6 Summary

351

(1)

References

352

(1)

Chapter 12. Sonication as a sample preparation method for elemental analysis

353

(18)

Kevin Ashley

12.1 Introduction

353

(1)

12.2 Methodological considerations

354

(3)

12.3 Historical background

357

(1)

12.4 Applications-sonication and sample preparation

358

(8)

12.4.1 Environmental analysis

358

(2)

12.4.2 Industrial hygiene

360

(3)

12.4.3 Biological tissues and fluids

363

(1)

12.4.4 Other applications

364

(2)

12.5 Summary

366

(1)

References

366

(5)

Chapter 13. Solid phase microextraction as a tool for trace element determination

371

(22)

Zoltán Mester and Ralph sturgeon

13.1 Introduction

371

(2)

13.2 General description of solid phase microextraction

373

(2)

13.2.1 Extraction modes

373

(2)

13.2.2 Coatings

375

(1)

13.3 Solid phase microextraction: step-by-step method development

375

(5)

13.3.1 Extraction mode selection

375

(1)

13.3.2 Fiber coating selection

376

(1)

13.3.3 Derivatization method selection

376

(1)

13.3.4 Optimization of desorption conditions

376

(1)

13.3.5 Sample volume optimization

376

(1)

13.3.6 Optimization of the extraction time

377

(1)

13.3.7 Optimization of extraction conditions

377

(1)

13.3.8 Determination of the linear dynamic range

378

(1)

13.3.9 Selection of the calibration method

378

(1)

13.3.10 Precision of the method

379

(1)

13.3.11 Automation of the method

379

(1)

13.4 Solid phase microextraction for speciation analysis

380

(8)

13.4.1 Volatile metal species-gas chromatographic determination

380

(8)

13.5 Solid phase microextraction as an investigative tool

388

(1)

13.6 Limitations of solid phase microextraction

388

(1)

13.7 Isotope dilution calibration in combination with solid phase microextraction

389

(1)

References

390

(3)

Chapter 14. Solid-phase extraction

393

(66)

Valérie Camel

14.1 Introduction

393

(1)

14.2 Theory

393

(17)

14.2.1 Presentation of the technique

394

(6)

14.2.2 Operation

400

(3)

14.2.3 Advantages of the technique

403

(7)

14.3 Step-by-step method development guide

410

(29)

14.3.1 Selection of solid sorbent

410

(22)

14.3.2 Influential parameters

432

(7)

14.4 Applications of SPE to the determination of some trace elements

439

(11)

14.4.1 Chromium

439

(4)

14.4.2 Iron

443

(2)

14.4.3 Mercury

445

(1)

14.4.4 Selenium

445

(1)

14.4.5 Tin

445

(5)

14.5 Conclusion

450

(1)

References

451

(8)

Chapter 15. Chelation solvent extraction for separation of metal ions

459

(36)

Hideyuki Itabashi and Taketoshi Nakahara

15.1 Introduction

459

(1)

15.2 Theoretical considerations

460

(14)

15.2.1 General principles

460

(5)

15.2.2 Preconcentration of metalions

465

(2)

15.2.3 Mutual separation of metal ions

467

(5)

15.2.4 Speciation of metal ions in natural water

472

(2)

15.3 Adsorption of metal ions using chelating resins

474

(3)

15.3.1 General principles

475

(1)

15.3.2 Features of some chelating resins

475

(2)

15.4 Application of chelation to sample preparation for trace metal analysis

477

(15)

15.4.1 Procedure for the extraction of metal ions from natural waters

477

(11)

15.4.2 Procedure for the extraction of metal ions from high-purity materials and inorganic solid samples

488

(2)

15.4.3 Procedure for the extraction of metal ions from biological samples

490

(1)

15.4.4 Procedure for the speciation of metal ions in natural waters

491

(1)

References

492

(3)

Chapter 16. Cryogenic trapping for speciation analysis

495

(38)

Marie-Pierre Pavageau, Eva Krupp, Alberto de Diego, Christophe Pécheyran and Olivier F.X. Donard

16.1 Introduction

495

(7)

16.2 Definition of volatile species

502

(2)

16.3 Physico-chemical principles and processes associated with cryofocusing

504

(5)

16.4 Analytical constraints

509

(8)

16.4.1 Removal of CO2

510

(2)

16.4.2 Water removal

512

(5)

16.5 Sample preservation and stability

517

(3)

16.6 Instrumentation for cryogenic trapping and selected applications

520

(9)

16.6.1 Cryosampler for determination of industrial and environmental VMCs

520

(3)

16.6.2 Cryogenic trapping for speciation analysis

523

(6)

References

529

(4)

Chapter 17. Biotrapping as an alternative to metal preconcentration and speciation

533

(26)

Yolanda Madrid and Carmen Cámara

17.1 Introduction

533

(2)

17.2 General characteristics of biological substrates

535

(3)

17.2.1 Algae

535

(1)

17.2.2 Bacteria

536

(1)

17.2.3 Fungi

537

(1)

17.3 Uptake mechanisms

538

(3)

17.4 Working procedures

541

(5)

17.4.1 Immobilisation

541

(5)

17.5 Applications

546

(11)

17.5.1 Analytical applications

546

(10)

17.5.2 Technological applications

556

(1)

17.6 Conclusions

557

(1)

References

557

(2)

Chapter 18 Membrane extraction

559

(18)

Jan Ake Jönsson and Lennart Mathiasson

18.1 Introduction

559

(1)

18.2 Membrane extraction techniques

559

(7)

18.2.1 Supported liquid membrane extraction (SLM)

560

(5)

18.2.2 Microporous membrane liquid liquid extraction (MMLLE)

565

(1)

18.3 Chemical principles for metal extraction

566

(1)

18.4 Properties of membrane extraction

566

(4)

18.4.1 Clean-up and selectivity

567

(1)

18.4.2 Enrichment

568

(1)

18.4.3 Automation and unattended operation

569

(1)

18.4.4 Solvent consumption

570

(1)

18.5 Experimental set-up

570

(4)

18.5.1 Flow systems for membrane extraction

570

(1)

18.5.2 How to set up a membrane extraction experiment for metal ions

571

(3)

Acknowledgements

574

(1)

References

574

(3)

Chapter 19. Derivatization and vapor generation methods for trace element analysis and speciation

577

(16)

Yong Cai

19.1 Introduction

577

(1)

19.2 Theory

578

(5)

19.2.1 Grignard reactions

578

(1)

19.2.2 Hydride generation

579

(1)

19.2.3 Aqueous derivatization with tetraalkyl (aryl)borates

580

(3)

19.3 Method development

583

(2)

19.3.1 Grignard reactions

583

(1)

19.3.2 Aqueous derivatization

584

(1)

19.4 Applications

585

(5)

Acknowledgements

590

(1)

References

590

(3)

Chapter 20. Laser ablation sampling

593

(18)

Richard E. Russo and David P. Baldwin

20.1 Introduction

593

(1)

20.2 Experimental system

594

(5)

20.3 Ablation detection systems

599

(2)

20.4 Calibration

601

(2)

20.5 Fractionation

603

(1)

20.6 Conclusion

604

(2)

Acknowledgements

606

(1)

References

606

(5)

Chapter 21. Flow injection techniques for sample pretreatment

611

(38)

Zhao-Lun Fang

21.1 Introduction

611

(4)

21.1.1 General

611

(1)

21.1.2 General features of flow injection on-line sample pretreatment systems

612

(1)

21.1.3 Classification of FI sample pretreatment systems

612

(1)

21.1.4 Principles and general guidelines for the development of FI systems

613

(1)

21.1.5 Practical hints for manipulation of FI equipment

614

(1)

21.2 FI liquid-liquid extraction systems

615

(11)

21.2.1 Introduction

615

(2)

21.2.2 Apparatus for FI liquid-liquid extraction

617

(6)

21.2.3 Guidelines for the development of FI liquid-liquid extraction systems

623

(1)

21.2.4 Typical manifolds for FI liquid-liquid extraction

624

(2)

21.3 FI solid phase extraction systems

626

(9)

21.3.1 Introduction

626

(1)

21.3.2 Sorption media for FI solid phase extraction

627

(2)

21.3.3 Guidelines for the development of FI solid phase extraction systems

629

(1)

21.3.4 Typical manifolds for FI solid phase extraction

630

(5)

21.4 FI vapor generation systems

635

(6)

21.4.1 Introduction

635

(1)

21.4.2 Gas-liquid separators for FI vapor generation.

635

(1)

21.4.3 Guidelines for development of FI vapor generation systems

636

(2)

21.4.4 Typical FI manifolds for VG-AAS

638

(3)

21.5 FI gas diffusion systems

641

(2)

21.5.1 General

641

(1)

21.5.2 Gas-diffusion separators

641

(1)

21.5.3 Typical FI manifolds for gas-diffusion separation and preconcentration

642

(1)

21.6 FI on-line sample digestion

643

(3)

21.6.1 Introduction

643

(1)

21.6.2 FI on-line sample digestion systems for AAS

644

(1)

21.6.3 FI digestion systems coupled to VG-AAS

644

(1)

21.6.3 FI systems for digestion of solid samples in AAS

645

(1)

21.6.5 FI pretreatment systems with on-line photo-oxidation by UV irradiation

646

(1)

References

646

(3)

Chapter 22. Automation of sample preparation

649

(34)

Maria Dolores Luque de Castro and Jose Luis Luque Garcia

22.1 Introduction

649

(4)

22.1.1 Generalities

649

(1)

22.1.2 Principal shortcomings in automating sample preparation

650

(1)

22.1.3 Batch versus serial approaches to automated sample preparation

651

(1)

22.1.4 Bar codes: a necessary tool in automating routine analyses

652

(1)

22.2 Automation of liquid sample preparation

653

(6)

22.2.1 Continuous systems

653

(3)

22.2.2 Discontinuous approaches

656

(3)

22.3 Automation of solid sample preparation

659

(1)

22.3.1 One-step approaches to automation and acceleration of solid sample preparation

659

(1)

22.3.2 Direct solid sampling

660

(1)

22.4 Robotics

660

(16)

22.4.1 Workstations, robots, modules and peripherals

662

(8)

22.4.2 The role of robots in the analytical process

670

(4)

22.4.3 Analytical scope of robotics for sample preparation

674

(2)

22.5 Advantages and disadvantages of automation of sample preparation

676

(1)

22.6 Future prospects

677

(1)

References

678

(5)

MATRICES

Chapter 23. Sample preparation for crude oil, petroleum products and polymers

683

(40)

Robert I. Botto

23.1 Introduction

683

(10)

23.1.1 Nature of petroleum crude, products and polymers

683

(3)

23.1.2 Element context and species in petroleum crude, products and polymers

686

(5)

23.1.3 Sample preparation challenges for trace element analysis

691

(2)

23.2 Sample preparation techniques and instrumentation

693

(20)

23.2.1 Ashing techniques

693

(4)

23.2.2 Acid mineralization techniques

697

(7)

23.2.3 Oxygen combustion

704

(2)

23.2.4 Sample component separations/extractive sample preparation

706

(1)

23.2.5 Organic sample dilutions and dissolutions

707

(2)

23.2.6 Stable emulsions

709

(2)

23.2.7 Scrubber sampling for C1-C4 hydrocarbons and gases

711

(2)

23.3 Cleanliness and quality assurance

713

(5)

23.3.1 Equipment cleaning

713

(1)

23.3.2 Clean techniques and disposable equipment

714

(1)

23.3.3 Quality assurance

715

(3)

Acknowledgements

718

(1)

References

719

(4)

Chapter 24. Sample preparation of geological samples, soils and sediments

723

(42)

Philip J. Potts and Philip Robinson

24.1 Introduction

723

(1)

24.2 Sample preparation

723

(5)

24.2.1 Sample collection

724

(2)

24.2.2 Crushing and grinding

726

(1)

24.2.3 Selecting an appropriate test portion

727

(1)

24.3 Choice of approach

728

(2)

24.3.1 Fitness-for-purpose

728

(1)

24.3.2 Choice of sample preparation procedure based on choice of technique

728

(1)

24.3.3 Choice of sample preparation based on the characteristics of elements

729

(1)

24.4 Methods that do not require any sample digestion in situ methods of analysis

730

(3)

24.4.1 Portable X-ray fluorescence

730

(2)

24.4.2 Gamma spectrometry

732

(1)

24.4.3 Laser ablation techniques and other microprobe/microanalytical techniques

732

(1)

24.5 Methods based on solid samples

733

(2)

24.5.1 Direct determinations on powders

733

(1)

24.5.2 Powder pellet for XRF

734

(1)

24.5.3 Glass disks for XRF trace determinations

734

(1)

24.6 Dissolution methods based on acid attack

735

(15)

24.6.1 Properties of acids used in the decomposition of geological materials

736

(2)

24.6.2 Open vessel and low-pressure acid digestion

738

(2)

24.6.3 HF-HNO3 decomposition method in Savillex® screw top vials

740

(1)

24.6.4 Closed vessel high pressure acid digestion

740

(2)

24.6.5 HF/H2SO4 decomposition method in closed, high pressure vessels

742

(1)

24.6.6 HF/HC104-HCl decomposition method in closed, high pressure vessels

742

(1)

24.6.7 Microwave oven digestion

743

(1)

24.6.8 Partial acid attack

744

(1)

24.6.9 Difficult minerals

745

(5)

24.7 Decomposition by molten salt fusion

750

(3)

24.7.1 Total fusion

750

(2)

24.7.2 A LiBO2 fusion procedure

752

(1)

24.7.3 Sintering

752

(1)

24.7.4 Fire assay

752

(1)

24.8 Pre-concentration and separation procedures

753

(2)

24.8.1 Ion exchange

753

(1)

24.8.2 Solvent extraction and co-precipitation

754

(1)

24.8.3 Vapour generation

755

(1)

24.9 Sequential extractions and dissolutions

755

(3)

24.9.1 Procedure of Tessier et al

756

(1)

24.9.2 The "BCR" method

757

(1)

24.9.3 Selective extractions for geochemical exploration

757

(1)

24.10 Summary and conclusions

758

(1)

References

758

(7)

Chapter 25. Sample preparation for food analysis

765

(92)

Milan Ihnat

25.1 Introduction

765

(1)

25.2 Literature

766

(2)

25.2.1 Books on sample treatment, decomposition

767

(1)

25.2.2 Books including chapters, sections on or discussing sample treatment, decomposition

767

(1)

25.2.3 Reviews on sample treatment, decomposition

767

(1)

25.2.4 Other reviews including coverage of sample treatment, decomposition

768

(1)

25.2.5 Papers, publications, containing (major) writing on sample treatment

768

(1)

25.3 Pretreatment

768

(2)

25.4 Classification of sample treatment methods

770

(1)

25.5 Compilation of sample treatment methods for foods

770

(69)

25.5.1 No treatment

833

(1)

25.5.2 Dry ashing

834

(2)

25.5.3 Wet digestion-conventional

836

(2)

25.5.4 Wet digestion-microwave-assisted

838

(1)

25.5.5 Slurry sample preparation

838

(1)

25.6 Specific cases: methods, elements, matrices

839

(4)

25.6.1 Analytical method

839

(2)

25.6.2 Elements

841

(1)

25.6.3 Matrix and constituents

842

(1)

25.7 Examples of specific, recommended sample treatment procedures

843

(3)

25.7.1 Conventional wet digestion with nitric and perchloric acids

843

(2)

25.7.2 Dry ashing with or without ashing aid

845

(1)

25.7.3 Microwave-assisted wet digestion

845

(1)

25.8 Closing remarks

846

(1)

References

847

(10)

Chapter 26. The determination of trace elements in water

857

(46)

Scott N. Willie

26.1 Direct methods of determination

857

(3)

26.2 Preconcentration techniques-multielement

860

(5)

26.3 Preconcentration-individual elements

865

(1)

26.4 Determination of trace elements as volatile species

865

(14)

26.5 Mercury

879

(1)

26.6 Luminescence

880

(5)

26.7 Voltammetry

885

(6)

26.8 Total-reflection X-Ray fluorescence spectrometry

891

(3)

26.9 Conclusions

894

(1)

References

894

(9)

Chapter 27. Aerosol sampling and sample preparation for elemental analysis

903

(32)

József Hlavay

27.1 Introduction

903

(3)

27.1.1 Objectives of monitoring

904

(2)

27.2 Sampling of aerosols

906

(18)

27.2.1 General considerations

906

(3)

27.2.2 Sampling of aerosol by impactors

909

(7)

27.2.3 Ambient sampling for the respirable fraction

916

(2)

27.2.4 High-volume aerosol samplers

918

(4)

27.2.5 Speciation aerosol sampling system

922

(2)

27.2.6 Passive samplers

924

(1)

27.3 Sequential extraction schemes for aerosol samples

924

(6)

27.4 Discussion

930

(1)

Acknowledgements

931

(1)

General terms used in sampling

931

(1)

References

932

(3)

Chapter 28. sample preparation for industrial waste analysis

935

(30)

Peter Drouin and Ray E. Clement

28.1 Types of industrial waste

935

(1)

28.2 Safety considerations for industrial waste analysis

936

(1)

28.3 Sample characteristics and industrial waste sampling

936

(2)

28.4 Digestions

938

(12)

28.4.1 Aqueous sample types-US EPA methods

939

(3)

28.4.2 Solid sample types-US EPA methods

942

(1)

28.4.3 Reported studies-hot plate digestion

943

(2)

28.4.4 Reported studies-microwave digestion methods

945

(4)

28.4.5 Ultrasound-assisted extractions

949

(1)

28.4.6 Alkaline digestions

949

(1)

28.4.7 Laboratory safety

950

(1)

28.5 Leach procedures

950

(7)

28.5.1 Toxicity characteristic leaching procedure

951

(1)

28.5.2 TCLP regulatory limits

951

(1)

28.5.3 TCLP method summary

952

(1)

28.5.4 TCLP applications

953

(1)

28.5.5 TCLP and sequential extractions

954

(2)

28.5.6 TCLP limitations

956

(1)

28.6 Certified reference materials

957

(1)

28.7 Summary and future developments

957

(3)

28.8 Useful World Wide Websites

960

(1)

Acknowledgements

961

(1)

References

961

(4)

Chapter 29. Sample preparation for semiconductor materials

965

(26)

Katsu Kawabata, Yoko Kishi, Fuhe Li and Scott Anderson

29.1 Introduction

965

(4)

29.2 Contamination control

969

(7)

29.2.1 Clean room

969

(2)

29.2.2 Equipments, reagents and standards

971

(5)

29.3 Sample preparation

976

(10)

29.3.1 Preparation and analysis of samples

978

(8)

29.4 Conclusion

986

(1)

References

986

(5)

TRACE ELEMENT SPECIATION

Chapter 30. Sampling and sample treatment in the analysis of organotin compounds in environmental samples

991

(36)

Roberto Morabito

30.1 Introduction

991

(3)

30.2 Critical steps in organotin analysis

994

(11)

30.2.1 Sampling

994

(4)

30.2.2 Storage

998

(2)

30.2.3 Sample treatment

1000

(5)

30.3 Improving the quality of organotin measurements in Europe

1005

(15)

30.4 Detailed procedure for the GC-MS determination of organotin compounds in environmental samples 1017

Acknowledgements

1020

(1)

References

1021

(6)

Chapter 31. Sample preparation for arsenic speciation

1027

(18)

Walter Goessler and Doris Kuehnelt

31.1 Introduction

1027

(1)

31.2 Occurrence and distribution of arsenic in the environment

1028

(5)

31.2.1 Marine environment

1028

(3)

31.2.2 Terrestrial environment

1031

(1)

31.2.3 Humans

1031

(2)

31.3 Stability of arsenic compounds

1033

(5)

31.3.1 Arsenite and arsenate

1034

(1)

31.3.2 Methylarsonous acid and dimethylarsinous acid

1035

(1)

31.3.3 Methylarsonic acid and dimethylarsinic acid

1036

(1)

31.3.4 Arsenobetaine, arsenocholine, trimethylarsine oxide, and the tetramethylarsonium ion

1037

(1)

31.3.5 Arsenosugars

1037

(1)

31.4 Extraction of arsenic compounds from environmental samples

1038

(3)

31.5 Conclusions

1041

(1)

References

1041

(4)

Chapter 32. Sample preparation for speciation of selenium

1045

(18)

Claudia Ponce de Leon, Anne P. Vonderheide and Joseph A. Caruso

32.1 Why selenium speciation?

1045

(1)

32.2 General sample preparation

1045

(1)

32.3 Mammals

1046

(4)

32.3.1 Body fluid analysis

1046

(3)

32.3.2 Tissue sample analysis

1049

(1)

32.4 Fish/birds

1050

(1)

32.5 Plants

1051

(4)

32.5.1 Leafy plants

1052

(1)

32.5.2 Broccoli

1053

(1)

32.5.3 Spices (garlic, onion, white clover)

1053

(1)

32.5.4 Grains

1054

(1)

32.5.5 Nuts

1054

(1)

32.5.6 Mushrooms

1054

(1)

32.6 Microorganisms

1055

(1)

32.7 Environmental

1055

(4)

32.7.1 Air

1055

(1)

32.7.2 Water

1056

(2)

32.7.3 Soil and sediments (solid matrices)

1058

(1)

References

1059

(4)

Chapter 33. Sample preparation for mercury speciation

1063

(18)

Holger Hintelmann

33.1 Introduction

1063

(1)

33.2 Aqueous solution chemistry of methylmercury

1063

(2)

33.3 Sample collection, preservation and storage

1065

(4)

33.3.1 Cleaning of sampling and laboratory equipment

1066

(1)

33.3.2 Water sampling

1066

(1)

33.3.3 Preservation and storage of water samples

1067

(1)

33.3.4 Preservation and storage of tissue and vegetation samples

1068

(1)

33.3.5 Preservation and storage of soil and sediment samples

1068

(1)

33.4 Sample preparation

1069

(6)

33.4.1 Extraction of methylmercury from water

1071

(1)

33.4.2 Extraction of methylmercury from soils, sediments and particles

1072

(1)

33.4.3 Extraction of methylmercury from biological tissue

1073

(1)

33.4.4 Direct techniques involving no sample preparation

1074

(1)

33.4.5 Extraction of mercury species other than methylmercury

1074

(1)

33.5 Quality control

1075

(4)

33.5.1 Artifactual formation of methylmercury

1075

(1)

33.5.2 Spike recoveries

1076

(1)

33.5.3 Reference materials

1077

(2)

Acknowledgements

1079

(1)

References

1079

(2)

Chapter 34. Sample preparation for speciation of lead

1081

(34)

Freddy C. Adams and Monika Heisterkamp

34.1 Introduction

1081

(2)

34.2 Toxicity of organolead compounds

1083

(2)

34.3 The history of leaded gasoline

1085

(3)

34.4 Properties of organolead compounds

1088

(2)

34.5 Synthesis of organolead compounds

1090

(2)

34.6 The biogeochemical cycle of lead

1092

(1)

34.7 Analytical techniques for speciation analysis of organolead compounds

1092

(19)

34.7.1 Hyphenated techniques for organometal determinations

1093

(3)

34.7.2 Sample preparation

1096

(1)

34.7.3 Sample pretreatment using gas chromatographic separation

1097

(3)

34.7.4 Extraction recovery

1100

(1)

34.7.5 Separation

1101

(3)

34.7.6 Detection of organolead compounds after chromatography

1104

(3)

34.7.7 Procedures for the determination of organolead compounds in dust material

1107

(2)

34.7.8 Comparison of the different hyphenated systems

1109

(2)

References

1111

(4)

Chapter 35. Sample preparation for chromium speciation

1115

(58)

Miguel de la Guardia and Angel Morales-Rubio

35.1 The element and its reactivity

1115

(2)

35.2 The presence of Cr in nature and industrial processes

1117

(1)

35.3 Chemical species of Cr present in real samples

1118

(2)

35.4 Analytical methodologies available for determination of Cr

1120

(1)

35.5 Analytical methodologies for Cr speciation in water

1120

(16)

35.5.1 Speciation of chromium in aqueous matrices

1121

(1)

35.5.2 Types of samples analyzed

1121

(2)

35.5.3 Pretreatments and techniques applied

1123

(1)

35.5.4 Speciation chromium using atomic spectrometry and MS-based techniques

1124

(6)

35.5.5 Determination of chromium speciation using molecular spectrophotometry

1130

(6)

35.6 Analytical methodologies for Cr speciation in biological fluids

1136

(9)

35.6.1 Speciation of chromium in biological fluids

1136

(1)

35.6.2 Types of samples analyzed

1137

(1)

35.6.3 Pretreatments and techniques applied

1137

(1)

35.6.4 Chromium speciation using atomic spectrometry detection

1138

(5)

35.6.5 Chromium speciation using molecular spectrophotometry detection

1143

(2)

35.7 Analytical methodologies for speciation of Cr in solid samples

1145

(12)

35.7.1 Speciation of chromium in solid samples

1145

(1)

35.7.2 Types of samples analyzed

1145

(10)

35.7.3 Solid sample treatments for speciation of chromium

1155

(2)

35.8 Final considerations

1157

(1)

References

1158

(15)

Chapter 36. Sample preparation for metal-based drugs

1173

(12)

Ronald R. Barefoot

36.1 Introduction

1173

(1)

36.2 Platinum-based drugs

1173

(7)

36.2.1 Preparation of biological samples

1175

(1)

36.2.2 Cisplatin

1176

(1)

36.2.3 Carboplatin

1177

(1)

36.2.4 Oxaliplatin

1177

(1)

36.2.5 Ormaplatin

1178

(1)

36.2.6 Lobaplatin

1178

(1)

36.2.7 JM216

1178

(1)

36.2.8 Validated methods of analysis

1179

(1)

36.3 Gold-based drugs

1180

(1)

36.3.1 Sample preparation

1175

(6)

36.4 Mercury

1181

(1)

36.5 Vanadium

1181

(1)

36.6 Lead

1182

(1)

36.7 Conclusions

1182

(1)

References

1182

(3)

Chapter 37. Sample preparation for speciation analysis for metallobiomolecules

1185

(26)

Joanna Szpunar, Brice Bouyssiere and Ryszard Lobinski

37.1 Introduction

1185

(1)

37.2 Elemental species in biological systems: metallobiomolecules

1186

(2)

37.3 Tailoring sample preparation: definition of the analyte moiety

1188

(1)

37.4 Homogenization and analyte recovery using unreactive buffers

1188

(2)

37.5 Analyte recovery through partial degradation of sample matrix

1190

(3)

37.5.1 Extraction with protein denaturating reagents

1190

(1)

37.5.2 Enzymatic extraction of organometallic compounds

1190

(1)

37.5.3 Controlled enzymatic degradation prior to speciation of metal complexes

1191

(1)

37.5.4 Sequential enzymatic extractions for the evaluation of the bioaccessibility of metals in foodstuffs

1192

(1)

37.6 Fractionation of metal species according to the molecular weight prior to analytical chromatography or capillary electrophoresis

1193

(2)

37.6.1 Ultrafiltration

1194

(1)

37.6.2 Gel filtration

1194

(1)

37.7 Multidimensional LC clean-up procedures prior to characterization of metal species by electrospray MS

1195

(1)

37.8 Sample preparation prior to speciation analysis of biological fluids

1196

(4)

37.8.1 Arsenic in urine

1196

(1)

37.8.2 Selenium in urine

1197

(1)

37.8.3 Metal complexes in biological fluids

1198

(1)

37.8.4 Metallodrug metabolites in biological fluids

1199

(1)

37.9 Sample preparation prior to speciation analysis in solid matrices

1200

(5)

37.9.1 Organoarsenic species in marine biota and foodstuffs

1200

(1)

37.9.2 Low-molecular organoselenium species in yeast and plants

1201

(2)

37.9.3 High-molecular selenium species in animal tissues and yeast

1203

(1)

37.9.4 Metal complexes with metallothioneins

1203

(2)

37.10 Sources of error

1205

(1)

References

1206

(5)

Chapter 38. Sample preparation for the analysis of volatile metals species

1211

(22)

Jörg Feldmann

38.1 Introduction

1211

(1)

38.2 Species of interest

1212

(4)

38.3 Characterization of gas samples

1216

(1)

38.4 Sample preparation strategies

1216

(6)

38.4.1 Sampling

1217

(1)

38.4.2 Preconcentration

1217

(5)

38.5 Specific procedures

1222

(7)

38.5.1 Cryotrapping methods

1223

(4)

38.5.2 Solid phase micro extraction

1227

(1)

38.5.3 Adsorption method

1227

(2)

38.6 Problems and future studies

1229

(1)

References

1230

(3)

Chapter 39. Sequential extraction

1233

(24)

Angels Sahuquillo and Gemma Rauret

39.1 Sequential extraction procedures: a special case of sample dissolution

1233

(2)

39.1.1 A brief historical introduction

1233

(1)

39.1.2 Definition of sequential extraction procedures

1234

(1)

39.2 Types, uses and limitations of SEPS

1235

(11)

39.2.1 Characteristics of the extraction agents

1235

(1)

39.2.2 SEPS more widely used

1235

(4)

39.2.3 Types of matrices and elements analysed

1239

(2)

39.2.4 Use of the information obtained

1241

(1)

39.2.5 Limitations of SEPS

1242

(4)

39.3 Sample pre-treatment for SEPS

1246

(4)

39.3.1 Drying

1246

(2)

39.3.2 Grinding and sieving steps

1248

(1)

39.3.3 Use of inert atmosphere

1249

(1)

39.3.4 Recommendations

1250

(1)

39.4 Application of other extraction techniques to SEPS

1250

(2)

39.4.1 Microwave

1250

(1)

39.4.2 Ultrasound

1251

(1)

39.4.3 Other alternatives

1251

(1)

39.4.4 Conclusions

1251

(1)

39.5 Quality control for SEPS

1252

(1)

References

1253

(4)

Index

1257

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Sample Preparation for Trace Element Analysis

Summary

Table of Contents

Supplemental Materials