Sample preparation in chromatography / edited by Serban C. Moldoveanu & Victor David.

Format:

Book

Contributor:

Moldoveanu, Șerban.

David, Victor, 1955-

Series:

Journal of chromatography library ; vol. 65.

Journal of chromatography library ; vol. 65

Language:

English

Subjects (All):

Chromatographic analysis.

Sample introduction (Chemistry).

Chromatography.

Sampling Studies.

Medical Subjects:

Chromatography.

Sampling Studies.

Physical Description:

xi, 930 pages : illustrations ; 25 cm.

Place of Publication:

Amsterdam ; Boston : Elsevier Science, 2002.

Summary:

Sample preparation is an essential step in many analyses. This step consists of a variety of preliminary operations performed on the sample to modify it and make it more suitable for analysis.

Contents:

1.1. Overview of a Chemical Analysis 3

1.2. Types of Operations Used in Sample Preparation 10

1.3. Some Theoretical Aspects of Phase Transfers 16

1.4. Introductory Approach to Theory of Distribution Equilibria 24

1.5. Some Aspects of Mass Transfer Processes 33

1.6. Characterization of Chromatographic Separations 43

1.7. General Characteristics of Separations 61

1.8. Elementary Discussion on Thermodynamic and Kinetic Factors in Chemical Reactions 66

1.9. Brief Survey on Molecular Interactions 69

1.10. Empirical and Estimated Parameters for Sample Preparation Problems 77

1.11. Introductory Discussion on Precision, Accuracy, Sensitivity, and Limit of Detection in Chemical Analysis 94

1.12. Validation of an Analytical Method 107

2. Sampling and Its Connection with Sample Preparation

2.1. Relation of Sampling to Sample Preparation 113

2.2. Representative Samples 114

2.3. Techniques for Sample Collection 118

2.4. Handling, Preservation, and Storage of Samples 130

3. Overview on Sample Preparation for Chromatography

3.1. The Role of Sample Preparation 137

3.2. The Use of Preliminary Information for the Choice of a Sample Preparation Procedure 141

3.3. Sample Homogenization and Dissolution 146

3.4. Sample Cleanup, Fractionation, and Concentration 147

3.5. Chemical Modifications of the Sample 152

3.6. Other Types of Sample Modifications 153

3.7. Differences in Sample Preparation for Different Chromatographic Techniques 154

3.8. Quantitation Techniques in Chromatography and Their Relation to Sample Preparation 156

3.9. Method Development in Sample Preparation 159

4. Chromatography as the Core Step in an Analytical Process

4.1. The Choice of the Core Analytical Technique 165

4.2. Gas Chromatography as a Core Step in the Analytical Process 169

4.3. Conventional High Performance Liquid Chromatography as a Core Analytical Technique 182

4.4. Other Chromatography Types Used as a Core Analytical Technique 201

5. Data Processing in Chromatographic Methods

5.1. Information Gain from Chromatographic Data 213

5.2. Qualitative and Quantitative Data from the Chromatographic Process 214

6. Automation in Sample Preparation

6.1. Automation in the Instrumentation Used in Sample Preparation 219

6.2. Computer Assisted Method Development 221

Part 2. Sample Preparation Techniques Using Physical Processes

7. Mechanical Processing in Sample Preparation

7.1. Grinding, Sieving, and Blending 225

7.2. Filtration, Microfiltration, and Ultrafiltration

7.3. Centrifugation 238

8. Phase Transfer Separations Applied in Sample Preparations

8.1. Distillation, Vaporization, and Drying 243

8.2. Dissolution, Crystallization, and Precipitation 255

9. Headspace Sampling Techniques in Gas Chromatography

9.1. Static Headspace Techniques 267

9.2. Dynamic Headspace 272

9.3. Other Headspace Techniques 283

10. Solvent Extraction

10.1. Liquid-Liquid Extraction 287

10.2. Conventional Liquid-Solid Extraction 304

10.3. Accelerated Solvent Extraction 310

10.4. Microwave-Assisted Solvent Extraction 314

10.5. Simultaneous Distillation and Extraction 317

10.6. Supercritical Solvent Extraction 322

11. Sorbent Extraction

11.1. Solid Phase Extraction Procedures 341

11.2. Solid Phase Microextraction 373

11.3. Matrix Solid Phase Dispersion 394

11.4. Other Solid Phase Sample Preparation Techniques 396

12. Chromatographic Procedures as Preliminary Separation

12.1. Gas Chromatography as a Sample Preparation Technique and Bidimensional GC 403

12.2. Liquid Chromatography as a Sample Preparation Technique 408

12.3. Size Exclusion Used in Sample Preparation 415

13. Membrane Separations

13.1. Gas Diffusion through Membranes and Stripping 423

13.2. Reverse Osmosis and Dialysis 425

14. Electroseparation Techniques in Sample Preparation

14.1. Electrophoretic Techniques 433

14.2. Other Electroseparation Techniques 440

15. Other Separation Techniques in Sample Preparation

15.1. Ion Exchange in Sample Preparation 443

15.2. Other Techniques in Sample Preparation 459

Part 3. Sample Preparation Techniques Involving Chemical Modifications

16. Chemical Modifications for Dissolution and Fractionation

16.1. Chemical Modifications for Sample Dissolution 463

16.2. Changes in pH and Chemical Modifications for Fractionation Purposes 466

17. Purpose of Derivatization in Chromatographic Analysis

17.1. General Aspects Regarding Derivatization 473

17.2. Preparation of the Sample for Derivatization and Common Derivatization Labware 476

17.3. Derivatization for Improving Gas Chromatographic Process 478

17.4. Derivatization for Improving Detection in GC 486

17.5. Derivatization for Improving Mass Spectral Identification 493

17.6. Derivatization for Improving Detection in HPLC and TLC 502

17.7. Derivatization for Chiral Separations 514

18. Chemical Reactions Used in Derivatization

18.1. Reactions with Formation of Alkyl or Aryl Derivatives 525

18.2. Silylation Reactions 545

18.3. Acylation Reactions 569

18.4. Reactions of Addition to Carbon-Heteroatom Multiple Bonds Used for Derivatization 581

18.5. Derivatization Reactions with Formation of Cyclic Compounds 591

18.6. Other Derivatization Reactions 613

18.7. Derivatization Reactions Involving Solid Phase Reagents 623

18.8. Derivatization on a Solid Support 629

19. Derivatization Reactions for Analytes with Various Functional Groups

19.1. Derivatization of Compounds with Alcohols, Epoxide, or Ether Groups 639

19.2. Derivatization Reactions for Phenols 669

19.3. Derivatization Reactions for Thiols and Sulfides 675

19.4. Derivatization of Compounds with Amino and Other Nitrogen-Containing Groups 683

19.5. Derivatization of Aldehydes and Ketones 724

19.6. Derivatization of Carboxylic Acids 739

19.7. Derivatization of Amides, Esters, and Other Derivatives of Carboxylic Acids, and of Carbonic Acid 761

19.8. Derivatization of Other Types of Organic Groups and of Organometallic and Inorganic Compounds 776

19.9. Derivatization of Carbohydrates 788

19.10. Derivatization of Amino Acids and Related Compounds 798

19.11. Derivatization of Other Multifunctional Compounds 814

20. Chemical Degradation of Polymers and Pyrolysis

20.1. Chemical Degradation of Polymeric Carbohydrates 847

20.2. Chemical Degradation of Proteins for Analytical Purposes 859

20.3. Chemical Degradation of other Macromolecular Compounds 864

20.4. Overview of Analytical Pyrolysis 869

20.5. Pyrolysis as a Chemical Modification Technique 877

20.6. Instrumentation Used in Analytical Pyrolysis 895

20.7. Application of Analytical Pyrolysis 901.

Notes:

Includes bibliogrphical references and index.

ISBN:

0444503943

OCLC:

49044741