Modern Size-Exclusion Liquid Chromatography Practice of Gel Permeation and Gel Filtration Chromatography

by Striegel , Andre; Yau, Wallace W.; Kirkland, Joseph J.; Bly, Donald D.

• ISBN13: 9780470442876
• ISBN10: 0470442875
• Edition: 2nd
• Format: eBook
• Copyright: 2009-11-25
• Publisher: Wiley

Summary

The Second Edition of Modern Size-Exclusion Chromatography offers a complete guide to the theories, methods, and applications of size-exclusion chromatography. It provides an unparalleled, integrated, up-to-date treatment of gel permeation and gel filtration chromatography. With its detailed descriptions of techniques, data handling, compilations of information on columns and column packings, and tables of important solvents and reference materials, the book offers readers everything they need to take full advantage of this popular macromolecular characterization technique.

Since publication of the first edition in 1979, there have been many important advances in the field of size-exclusion chromatography. This Second Edition brings the book thoroughly up to date, with expert coverage of:

• New and emerging industrial and research applications
• Practical aspects of size-exclusion chromatography (SEC) and multidetector and multidimensional SEC technologies for polymer architecture and copolymer analysis
• Updated information on the latest equipment and techniques
• New best practices for the lab
• SEC in relation to polymer characterization techniques such as GPEC, LCCC, and rheology

Throughout the text, detailed examples guide you step by step through all the latest techniques and applications. With its extensive revisions and updates written by leading experts and pioneers in the field, Modern Size-Exclusion Liquid Chromatography remains the definitive resource for the broad range of researchers and scientists who use HPLC and GPC methods.

Author Biography

André M. Striegel, PhD, is Assistant Professor in the Department of Chemistry & Biochemistry at the Florida State University, with previous industrial R&D experience at Solutia. He has published and lectured extensively in the area of polymer chromatography and is the recipient of several national awards in analytical chemistry. WALLACE W. YAU, PhD, received his doctorate in physical chemistry from University of Massachusetts and is currently a scientist specialist at Dow Chemical Co., with past industrial experience at DuPont and Chevron. He has been in GPC research and polymer characterization for the past four decades. JOSEPH J. KIRKLAND, PhD, is author or coauthor of eight widely read books on liquid chromatography, more than 150 peer-reviewed papers, and thirty patents. With over fifty years of industrial experience, he has been the recipient of many major national and international awards in analytical chemistry. DONALD D. BLY, PhD, retired as manager of analytical science, central research, DuPont. He has remained working as a consultant to analytical and analytical-polymer science businesses and has remained active in the American Chemical Society and ASTM.

Table of Contents

Foreword.

Preface.

1 Background.

1.1 Introduction.

1.2 History.

1.3 Utility of SEC.

1.4 Molar Mass Averages and Molar Mass Distribution.

1.5 Structure of The Book.

References.

2 Retention.

2.1 Introduction.

2.2 Solute Retention in LC.

2.3 Solute Retention in SEC.

2.4 SEC Retention Mechanism.

2.5 Theoretical Models of SEC Separation.

2.6 Other Considerations.

References.

3 Band Broadening.

3.1 Introduction.

3.2 LC Plate Theory.

3.3 Mechanism of SEC Band Broadening.

3.4 Influencing Factors.

3.5 Experimental Methods.

References.

4 Resolution.

4.1 Introduction.

4.2 Resolution Concept in SEC of Polymers.

4.3 Molar Mass Accuracy Criterion.

4.4 Applications of Column Performance Criteria .

4.5 Pore Geometry and Operational Effects.

References.

5 Equipment.

5.1 Introduction.

5.2 Extra-Column Effects: General.

5.3 Mobile-Phase Reservoirs, Inlet Filters, and Degassers.

5.4 Solvent-Metering Systems (Pumps).

5.5 Sample Injectors and Autosamplers.

5.6 Miscellaneous Hardware.

5.7 Laboratory Safety.

References.

6 The Column.

6.1 Introduction.

6.2 Column Packings.

6.3 Column-Packing Methods.

6.4 Column Performance.

References.

7 Experimental Variables and Techniques.

7.1 Introduction.

7.2 Solvent Effects.

7.3 Substrate Effects.

7.4 Sample Effects.

7.5 Laboratory Techniques.

7.6 Solvent Selection and Preparation.

7.7 Selection and Use of Standard Reference Materials.

7.8 Detector Selection.

7.9 Column Selection and Handling.

7.10 Chromatographic Design Considerations.

7.11 Making the Separation.

7.12 Troubleshooting.

References.

8 Calibration.

8.1 Introduction.

8.2 Calibration with Narrow-MMD Standards.

8.3 Calibration with Broad-MMD Standards.

8.4 Accuracy of Calibration Methods.

8.5 Actual Molar Mass Across the SEC Elution Curve.

8.6 Linear Calibration Ranges.

8.7 Recent Developments and Recommendations on Band-Broadening Correction.

References.

9 Physical Detectors.

9.1 Introduction.

9.2 Concentration-Sensitive Detectors.

9.3 Static Light-Scattering Detection.

9.4 Quasielastic Light-Scattering Detection.

9.5 Viscometric Detection.

9.6 SEC3.

References.

10 Chemical Detectors.

10.1 Introduction.

10.2 Mass Spectrometry.

10.3 Fourier Transform Infrared Spectroscopy.

10.4 Nuclear Magnetic Resonance Spectroscopy.

10.5 Other Chemical Detectors.

10.6 Coupling of Chemical Detectors.

References.

11 Polymer Architecture and Dilute Solution Thermodynamics.

11.1 Introduction.

11.2 Long-Chain Branching.

11.3 Determining the Short-Chain Branching Distribution.

11.4 Polymer Architecture: Conformation and Topology.

11.5 Star Polymers.

11.6 Determining the Persistence Length.

11.7 Determining the Characteristic Ratio.

11.8 Local Polydispersity.

References.

12 Aqueous SEC.

12.1 Introduction.

12.2 Aqueous SEC Columns.

12.3 Non-Size-Exclusion Effects and Mobile-Phase Additives.

12.4 Select Applications of Aqueous SEC.

References.

13 Oligomeric SEC.

13.1 Introduction.

13.2 What is an Oligomer?

13.3 Preliminary Considerations.

13.4 Oligomeric SEC Columns.

13.5 Select Applications of Oligomeric SEC.

13.6 Optimizing Resolution in Oligomeric SEC.

References.

14 SEC in 2D-LC Separations.

14.1 Introduction.

14.2 Principles of 2D Polymer Separations.

14.3 Designing an Experimental 2D-LC Protocol.

14.4 Eluent Transfer in 2D-LC.

14.5 Stop-Flow SEC × LC.

14.6 Select Applications of 2D-LC.

14.7 SEC in 3D Separations.

References.

15 Special Techniques.

15.1 Introduction.

15.2 Preparative SEC.

15.3 Recycle SEC.

15.4 High-Speed SEC.

15.5 Inverse SEC.

15.6 Vacancy and Differential SEC.

15.7 Size-Exclusion Electrochromatography.

References.

16 High-Temperature SEC and Rheological Connections.

16.1 Introduction.

16.2 High-Temperature SEC.

16.3 Complementarity of SEC and Rheology.

References.

Symbols.

Abbreviations.

Index.