Separation Methods In Microanalytical Systems

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ISBN: 9780824725303 | 0824725301
Cover: Hardcover
Copyright: 9/9/2005

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Focusing on what has been one of the driving forces behind the development of lab-on-a-chip devices, Separation Methods in Microanalytical Systems explores the implementation, realization, and operation of separation techniques and related complex workflows on microfabricated devices. The book details the design, manufacture, and integration of diverse components needed to perform an entire analytical procedure on a single miniaturized device. The content applies to a diversity of disciplines including chemical analysis, biomedical diagnostics, environmental monitoring, and drug discovery.Separation Methods in Microanalytical Systems lays its theoretical background in a way that scientists from varied disciplines can approach. The book describes factors that influence the performance of separation, such as microfluidic handling, sample pre-treatment, and detection. It also conveys fabrication and material issues, design challenges, and practical considerations. Several chapters describe specific separation techniques that are central to micro-Total Analysis Systems (µ-TAS) as well as novel methods and emerging trends in microchip-based separations. The book also provides an applications overview that supplies a wealth of examples that help scientists put their ideas in perspective with already existing solutions.This multi-authored volume offers different styles, approaches, and opinions for a given problem, reflecting the various angles researchers take to handle the same issues. A one-stop guide for understanding, designing, and working with separation techniques in microanalytical devices, Separation Methods in Microanalytical Systems is a valuable reference for scientists and engineers already preparing to meet the anticipated demand for function-specific chemical separation systems.

Chapter 1 Analytical Microsystems: A Bird's Eye View

(18)

Carlo S. Effenhauser

1.1 Introduction

(3)

1.2 Microanalytical Separation Systems

(2)

1.3 Strategic Benefits of Analytical Microsystems

(9)

1.3.1 Functional Integration

(1)

1.3.2 Faster Time-to-Result

(3)

1.3.3 Parallelization

(2)

1.3.4 Miniaturization

(1)

1.3.5 Novel Analytical Functions

(2)

1.4 Analytical Microsystems: A Short Conclusion

(1)

Acknowledgments

(1)

References

(4)

Chapter 2 Microfluidics: Some Basics

(36)

Stephen C. Jacobson and Christopher T. Culbertson

2.1 Microfluidic Devices

(2)

2.2 Fluid Transport

(6)

2.2.1 Electroosmotic Flow

(2)

2.2.2 Pressure-Driven Flow

(2)

2.2.3 Combined Flow

(2)

2.3 Separation Mechanisms

(2)

2.3.1 Electrophoresis

(1)

2.3.2 Chromatography

(1)

2.4 Separation Efficiency

(2)

2.4.1 Plate Height

(1)

2.4.2 Plate Number

(1)

2.5 Resolution

(1)

2.6 Peak Capacity

(2)

2.7 Dispersion

(10)

2.7.1 Diffusion

(1)

2.7.2 Injection Plug Length

(1)

2.7.3 Detection Window Length

(1)

2.7.4 Parabolic Flow Profiles

(1)

2.7.5 Thermal or Joule Heating

(1)

2.7.6 Geometric Dispersion

(4)

2.7.7 Mass Transfer Processes

(1)

2.7.8 Electrodispersion

(1)

2.8 Analogous Electrical Circuits

(1)

2.9 Mixing

(1)

2.10 Valving

(3)

2.10.1 Constant Volume (Pinched) Valve

(1)

2.10.2 Variable Volume (Gated) Valve

(2)

2.11 Scaling of Separations

(3)

References

(2)

Chapter 3 Microfabrication and Integration

(52)

Han J.G.E. Gardeniers and Albert van den Berg

3.1 Introduction

(3)

3.2 The Microfabrication Toolbox

(24)

3.2.1 Silicon Micromachining

(8)

3.2.2 Glass Micromachining

(6)

3.2.3 Metal Micromachining

(2)

3.2.4 Plastic Microfabrication

(4)

3.2.5 Sacrificial Layer Etching

(4)

3.3 Surface Properties of Micromachined Structures

(5)

3.4 Wafer Bonding and Lamination

(4)

3.5 Comparison of Materials

(1)

3.6 System Aspects: Integration and Interfacing

(4)

3.7 Summary and Outlook

(4)

References

100

(7)

Chapter 4 New Tools: Scalar Imaging, Velocimetry, and Simulation

107

(34)

Ernest F. Hasselbrink, Jr. and Sneha Madhavan-Reese

4.1 Introduction

108

(1)

4.2 Novel Fluorescence Imaging Techniques

108

(13)

4.2.1 Flow Visualization Using Caged-Dye or Bleached-Dye Methods

108

(3)

4.2.2 Mixing Quantification

111

(6)

4.2.2.1 Mixing Measurement Theory and the Mixture Fraction, ξ(x,y,z)

111

(1)

4.2.2.2 Complications for Experimental Methods

112

(2)

4.2.2.3 The "Unmixedness" Method

114

(3)

4.2.3 Temperature Imaging

117

(1)

4.2.4 Quantitative Imaging Considerations

118

(3)

4.2.4.1 Linearity, Background Signal, and Signal-to-Noise Ratio

118

(2)

4.2.4.2 Intensifiers

120

(1)

4.2.4.3 Photobleaching

121

(1)

4.3 Particle Imaging Velocimetry

121

(9)

4.3.1 Principle

121

(4)

4.3.2 Image Processing and Accuracy

125

(4)

4.3.3 PIV Hardware Selection

129

(1)

4.3.4 PIV Results and Interpretation

129

(1)

4.4 Numerical Simulation

130

(8)

4.4.1 To Simulate, or Not to Simulate?

130

(1)

4.4.2 Fundamentals: Flow Equations, BCs, Domain Selection

131

(5)

4.4.2.1 Equations: Pressure-Driven Flow in Channels with Walls of Zero Surface Charge Density

131

(2)

4.4.2.2 Domain and BC Selection: Pressure-Driven Flow in Channels with Walls of Zero Surface Charge Density

133

(1)

4.4.2.3 Equations: Flow in Channels with Walls of Nonzero Surface Charge Density

134

(2)

4.4.3 Caveats

136

(6)

4.4.3.1 Physics Models

136

(1)

4.4.3.2 Discretization and Convergence

137

(1)

References

138

(3)

Chapter 5 Transport Modes: Realizations and Practical Considerations

141

(24)

Susanne R. Wallenborg, Per Andersson, and Gunnar Thorsén

5.1 General Introduction

141

(1)

5.2 EOF-Based Liquid Transport

142

(10)

5.2.1 Introduction to EOF

142

(1)

5.2.2 EOF in Microchannels

143

(2)

5.2.3 Effects of Going Small

145

(2)

5.2.4 Sample Dispersion

147

(2)

5.2.5 EOF in Open Channels and in Packed Beds

149

(1)

5.2.6 Electrokinetic Pumping

149

(2)

5.2.7 Combining EOF and Hydrodynamic Flow

151

(1)

5.2.8 Summary

152

(1)

5.3 Pressure-Driven Liquid Transport

152

(7)

5.3.1 Introducton

152

(1)

5.3.2 Coupling an External Pump to the Chip

153

(1)

5.3.3 Centrifugal Force-Driven Separations

153

(2)

5.3.4 Flow Generation by Centrifugal Force

155

(4)

5.3.5 Summary

159

(1)

5.4 Other Means of Liquid Transport

159

(2)

References

161

(4)

Chapter 6 Pressure-Driven Separation Methods on a Chip

165

(44)

Gert Desmet, Emil Chmela, and Robert Tijssen

6.1 Introduction

165

(2)

6.2 Fundamental Considerations

167

(19)

6.2.1 General Properties of Pressure-Driven Flows

168

(5)

6.2.2 General Separation Performance Measures

173

(2)

6.2.3 Influence of the Flow Profiles on the Separation Performance

175

(3)

6.2.4 Mass Loadability and Detection Issues: Packed vs. Open-Tubular Channels

178

(1)

6.2.5 Additional Peak Broadening Sources in Pressure-Driven Flows through Flat-Rectangular Channels

179

(5)

6.2.6 Alternatives to PD Flows

184

(2)

6.3 Practical Aspects

186

(7)

6.3.1 Pumps and Valves

186

(1)

6.3.2 Packing Methods, Monolithic Packings, and Micromachined Packings

187

(2)

6.3.3 Injection and Detection Issues

189

(4)

6.4 Overview of Applications

193

(11)

6.4.1 HDC and FFF on a Chip

193

(6)

6.4.2 HPLC on a Chip

199

(4)

6.4.3 Low-Pressure Immunoassays and Enzymatic Assays + Flow-Through Biosensors

203

(1)

6.5 Conclusions and Outlook

204

(1)

References

205

(4)

Chapter 7 Transverse Transport in Microsystems: Theory and Applications

209

(52)

Paul Yager, Catherine Cabrera, and Andrew Kamholz

7.1 Motivations

210

(1)

7.2 Fundamentals of Pressure-Driven Flow in Microchannels

211

(8)

7.2.1 Velocity Profiles in Microsystems

212

(2)

7.2.2 Laminar Flow

214

(2)

7.2.3 Basic Relationships of Laminar Flow

216

(1)

7.2.4 Other Forces that May Move Solutes and Suspended Particles

217

(7)

7.2.4.1 Gravitation

217

(1)

7.2.4.2 Magnetic (Magnetic Field Applied Transverse to Flow Direction)

218

(1)

7.2.4.3 Hydrodynamic Focusing (i.e., Fluid Velocity Momentum Effects on Particles that Are at least 1/100 Size of Channel)

218

(1)

7.2.4.4 Viscosity Preferential Positioning

219

(1)

7.3 Optical Monitoring of Microdevices

219

(5)

7.4 Devices that Rely on Transverse Diffusional Transport in Flow: Field-Flow Fractionation, the H-Filter, and the T-Sensor

224

(8)

7.4.1 Field-Flow Fractionation

224

(1)

7.4.2 The T-Sensor

225

(6)

7.4.2.1 Diffusion Measurements in the T-Sensor

227

(2)

7.4.2.2 Effects of Velocity Profile on Diffusion

229

(1)

7.4.2.3 Chemical Detection: The T-Sensor

230

(1)

7.4.3 Extraction: The H-Filter

231

(1)

7.5 Transverse Electrokinetic Processes and Devices

232

(17)

7.5.1 Fundamentals (Including Resolution Limitations)

232

(7)

7.5.1.1 Basic Physics of the System

232

(1)

7.5.1.2 Surface Charge and Electrophoretic Mobility

233

(1)

7.5.1.3 Electroneutrality and Field Strength

233

(1)

7.5.1.4 Relevant Equations

234

(1)

7.5.1.5 Basics of Electrophoresis

235

(1)

7.5.1.6 Basics of Isoelectric Focusing

236

(2)

7.5.1.7 Basics of Dielectrophoresis

238

(1)

7.5.1.8 Basics of Electric Field-Flow Fractionation

239

(1)

7.5.2 Device and Experimental Design

239

(6)

7.5.2.1 Design Constraints Unique to Electrokinetic Processes

239

(2)

7.5.2.2 Selected Device Designs

241

(3)

7.5.2.3 Experimental Design Constraints: Importance of Buffer Selection, Suppression of EOF

244

(1)

7.5.3 Transverse Electrokinetic Separations of Molecules

245

(25)

7.5.3.1 Small Molecules

245

(1)

7.5.3.2 Proteins

246

(1)

7.5.3.3 Eukaryotic Cells

246

(2)

7.5.3.4 Prokaryotes

248

(1)

7.5.3.5 Other Biological Molecules and Particles

249

(1)

7.6 Future Directions

249

(1)

Acknowledgments

250

(1)

References

250

(11)

Chapter 8 Electro-Driven Separation Methods on Chips

261

(58)

Rikke P.H. Nikolajsen, Gabriela S. Chirica, Yolanda Fintschenko, and Jörg P. Kutter

8.1 Introduction

261

(4)

8.2 Electroosmosis, Electroosmotic Flow, and Electrokinetic Transport

265

(5)

8.3 Electrophoretic Techniques

270

(19)

8.3.1 Free Zone Capillary Electrophoresis

270

(8)

8.3.2 Isotachophoresis

278

(3)

8.3.3 Isoelectric Focusing

281

(3)

8.3.4 Affinity Capillary Electrophoresis

284

(3)

8.3.5 Capillary Gel Electrophoresis

287

(2)

8.4 Micellar Electrokinetic Chromatography

289

(7)

8.5 Capillary Electrochromatography

296

(11)

8.6 More Dimensional Separations

307

(4)

References

311

(8)

Chapter 9 Gas Chromatography on Microchips

319

(40)

Richard J. Kottenstette, Chung-Nin Channy Wong, and Curtis D. Mowry

9.1 Introduction

320

(2)

9.1.1 Gas Sensing

320

(1)

9.1.2 Sensor Arrays and Electronic Noses

321

(1)

9.1.3 Gas Sensing with Microanalytical Systems

322

(1)

9.2 Gas Chromatography — History and Background

322

(5)

9.2.1 History of Microanalytical Gas Chromatographic Systems

324

(2)

9.2.2 Commercial Instrumentation Based on Micromachining

326

(1)

9.3 Prototype Microanalytical GC Systems

327

(1)

9.4 Sample Handling and Injection for Micro-GC

327

(3)

9.4.1 Sample Valves and Loops

327

(1)

9.4.2 Solid-Phase Microextraction

328

(1)

9.4.3 Other Technologies

329

(1)

9.5 Microfabricated GC Columns

330

(1)

9.6 Theory of Microfabricated GC Columns

330

(8)

9.6.1 Transport Model

330

(4)

9.6.2 Separation Model

334

(3)

9.6.3 Is Smaller Better?

337

(1)

9.6.4 Theory Discussion

338

(1)

9.7 GC Column Fabrication and Coating

338

(3)

9.8 Micro-GC Detectors

341

(9)

9.8.1 Thermal Conductivity

342

(2)

9.8.2 Surface Acoustic Wave

344

(1)

9.8.3 Chemiresistors

344

(1)

9.8.4 Flame Ionization and Flame Atomic Emission Detector

345

(1)

9.8.5 Photoionization

346

(1)

9.8.6 Glow Discharge and Molecular Emission

346

(1)

9.8.7 Photoacoustic Detector

347

(1)

9.8.8 Miniature Mass Analysis

347

(3)

9.9 Improvements and Future Directions

350

(4)

9.9.1 Column Coating

350

(1)

9.9.2 Microfluidics, Pumps and Valves, Transfer Tubes

350

(1)

9.9.3 Detectors

351

(1)

9.9.4 Power

351

(1)

9.9.5 Materials Deposition and Fabrication

351

(1)

9.9.6 Integration

352

(2)

9.9.7 New Technologies

354

(1)

References

354

(5)

Chapter 10 Sample Preparation on Microchips

359

(74)

Jan Lichtenberg, Sander Koster, Laura Ceriotti, Nico F. de Rooij, and Elisabeth Verpoorte

10.1 Introduction

360

(4)

10.2 Basic Sample Clean-Up

364

(19)

10.2.1 Physical Particle Filtering

364

(6)

10.2.1.1 Filters Based on Lithographically Defined Constrictions

365

(3)

10.2.1.2 Filters Based on Sacrificial Layer Technology

368

(2)

10.2.2 Filtering by Diffusion

370

(1)

10.2.3 Cell Lysis

370

(3)

10.2.4 Dialysis

373

(10)

10.2.4.1 The Dialysis Process

374

(2)

10.2.4.2 Microdialysis Probe Designs

376

(1)

10.2.4.3 Factors Influencing the Performance of Microdialysis

376

(3)

10.2.4.4 Examples of Microdialysis on a Chip

379

(4)

10.3 Analyte Extraction/Preconcentration

383

(25)

10.3.1 Liquid–Liquid Extraction

383

(2)

10.3.1.1 Factors Influencing Extraction Efficiency and Selectivity

384

(1)

10.3.1.2 Examples on Chip

384

(1)

10.3.2 Solid-Phase Extraction

385

(10)

10.3.2.1 Adsorption Mechanisms

386

(3)

10.3.2.2 Practical Considerations for SPE on Chip

389

(2)

10.3.2.3 Examples of SPE on a Chip

391

(4)

10.3.3 Electrokinetic-Mobility-Based Sample Preconcentration

395

(1)

10.3.4 Creating Electrokinetic Velocity Gradients

395

(6)

10.3.4.1 Molecular Transport at an Electrokinetic Velocity Gradient

398

(3)

10.3.4.2 Effects of Induced, Pressure-Driven Flow

401

(1)

10.3.5 Techniques for Electrokinetic Sample Preconcentration for Microchip Devices

401

(5)

10.3.5.1 Field-Amplified Sample Stacking

401

(3)

10.3.5.2 Field-Amplified Injection

404

(1)

10.3.5.3 Thermal Gradient Focusing

405

(1)

10.3.5.4 Stacking of Neutral Analytes

405

(1)

10.3.6 Isotachophoresis for Sample Preconcentration and Clean-Up

406

(2)

10.4 Biochemical Sample Pretreatment

408

(15)

10.4.1 DNA Purification

408

(5)

10.4.2 Nucleic Acid Amplification

413

(6)

10.4.3 Biomolecule Fragmentation

419

(15)

10.4.3.1 Enzymatic Digestion of DNA

419

(1)

10.4.3.2 Enzymatic Digestion of Proteins

420

(1)

10.4.3.3 Physical Biomolecule Fragmentation

421

(2)

10.5 Conclusion

423

(1)

Acknowledgments

424

(1)

References

424

(9)

Chapter 11 Detection on Microchips: Principles, Challenges, Hyphenation, and Integration

433

(66)

Stephanie Pasas, Barbara Fogarty, Bryan Huynh, Nathan Lacher, Brian Carlson, Scott Martin, Walter Vandaveer IV, and Susan Lunte

11.1 Introduction to Detectors for Microchip-Based Separation Techniques

434

(4)

11.1.1 Sample Volume Considerations

435

(1)

11.1.2 Detector and Time Constant

436

(1)

11.1.3 Substrate Material

437

(1)

11.1.4 Detection Modes

437

(1)

11.2 Fluorescence Detection

438

(25)

11.2.1 Introduction

438

(1)

11.2.2 Instrumental Design

439

(9)

11.2.2.1 Excitation Sources

439

(1)

11.2.2.2 Detection

440

(3)

11.2.2.3 Optical Configurations

443

(2)

11.2.2.4 On-Chip Integration of Fluorescence Detection

445

(3)

11.2.2.5 Other Considerations

448

(1)

11.2.3 Derivatization Chemistries

448

(4)

11.2.3.1 Derivatization Reagents

448

(1)

11.2.3.2 Pre- and Postcolumn Derivatization Strategies

449

(3)

11.2.4 Direct vs. Indirect Fluorescence Detection

452

(1)

11.2.5 Applications

452

(3)

11.2.5.1 DNA

453

(1)

11.2.5.2 Protein, Peptides, and Amino Acids

453

(2)

11.2.6 Other Optical Detection Methods

455

(8)

11.2.6.1 Absorbance Detection

455

(4)

11.2.6.2 Chemiluminescence

459

(2)

11.2.6.3 Shah Convolution Fourier Transform

461

(1)

11.2.6.4 Refractive Index

462

(1)

11.2.6.5 Raman Spectra

462

(1)

11.2.6.6 Near-IR Spectra

463

(1)

11.2.7 Future Directions

463

(1)

11.3 Mass Spectrometric Detection

463

(11)

11.3.1 Introduction

463

(1)

11.3.2 Ionization Methods

464

(1)

11.3.2.1 Electrospray Ionization

464

(1)

11.3.2.2 Matrix-Assisted Laser Desorption Ionization

465

(1)

11.3.3 Mass Analyzers

465

(3)

11.3.3.1 Quadrupole Mass Spectrometer

466

(1)

11.3.3.2 Time-of-Flight Mass Analyzer

467

(1)

11.3.3.3 Tandem Mass Spectrometry

467

(1)

11.3.4 Microchip Substrates for CE–MS

468

(1)

11.3.5 Interfacing Microchip CE to MS

469

(3)

11.3.5.1 Microchip CE-Electrospray Ionization

469

(1)

11.3.5.2 Microchip CE-MALDI

470

(2)

11.3.6 Applications

472

(1)

11.3.7 Future Directions

473

(1)

11.4 Electrochemical Detection

474

(15)

11.4.1 Introduction to Electrochemical Detection

474

(1)

11.4.2 Amperometric Detection

474

(8)

11.4.2.1 Introduction to Amperometric Detection

474

(1)

11.4.2.2 Instrumental Design

475

(6)

11.4.2.3 Applications

481

(1)

11.4.3 Conductivity Detection

482

(6)

11.4.3.1 Introduction

482

(1)

11.4.3.2 Instrumental Design and Considerations

483

(4)

11.4.3.3 Applications

487

(1)

11.4.4 Potentiometric Detection

488

(1)

11.4.5 Future Direction of Electrochemical Detection

489

(1)

11.5 Conclusions

489

(1)

Acknowledgments

489

(1)

References

490

(9)

Chapter 12 Analytical Applications on Microchips

499

(44)

Shaorong Liu and Vladislav Dolnik

12.1 Introduction

499

(1)

12.2 Analysis of DNA

500

(19)

12.2.1 DNA Fragment Sizing

500

(6)

12.2.2 DNA Genotyping

506

(4)

12.2.3 Detection of DNA Mutation

510

(3)

12.2.4 DNA Sequencing

513

(6)

12.3 Analysis of Proteins and Peptides

519

(11)

12.3.1 Capillary SDS Electrophoresis in Sieving Matrix

519

(2)

12.3.2 Capillary Isoelectric Focusing

521

(3)

12.3.3 Multidimensional Electrophoresis of Proteins

524

(3)

12.3.4 Zone Electrophoresis

527

(1)

12.3.5 Enzymatic Assays

527

(3)

12.4 Analysis of Low Molecular Weight Compounds

530

(6)

12.4.1 Explosive Residues and Warfare Agents

530

(1)

12.4.2 Pharmaceuticals and Drugs of Abuse

531

(1)

12.4.3 Small Molecules in Body Fluids

532

(2)

12.4.4 Miscellaneous

534

(2)

12.5 Conclusions

536

(1)

References

537

(6)

Index

543

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