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: 9780471201724
• ISBN10: 0471201723
• Edition: 2nd
• Format: Hardcover
• Copyright: 2009-06-29
• 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 rheologyThroughout 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

Background.

Introduction

History

Utility of SEC

Molar Mass Averages and Molar Mass Distribution

Structure of This Book

Retention.

Introduction

Solute Retention in LC

Solute Retention in SEC

SEC Retention Mechanism

Theoretical Models of SEC Separation

Other Considerations

Band Broadening.

Introduction

LC Plate Theory

Mechanism of SEC Band Broadening

Influencing Factors

Experimental Methods

Resolution.

Introduction

Resolution Concept in SEC of Polymers

Molar Mass Accuracy Criterion

Applications of Column Performance Criteria

Pore Geometry and Operational Effects

EQuipment.

Introduction

Extracolumn Effects - General

Mobile-Phase Reservoirs, Inlet Filters, and Degassers

Solvent-Metering Systems (Pumps

Sample Injectors and Autosamplers

Miscellaneous Hardware

Laboratory Safety

The Column.

Introduction

Column Packings

Column Packing Methods

Column Performance

Experimental Variables And Techniques.

Introduction

Solvent Effects

Substrate Effects

Sample Effects

Laboratory Techniques

Solvent Selection and Preparation

Selection and Use of Standard Reference Materials

Detector Selection

Column Selection and Handling

Chromatographic Design Considerations

Making the Separation

Troubleshooting

Calibration.

Introduction

Calibration with Narrow-MMD Standards

Calibration with Broad-MMD Standards

Accuracy of Calibration Methods

Actual Molar Mass Across the SEC Elution Curve

Linear Calibration Ranges

Recent Developments and Recommendations on Band-Broadening Correction (BBC

Physical Detectors.

Introduction

Concentration-Sensitive Detectors

Static Light Scattering Detection, SLS

Quasi-Elastic Light Scattering Detection, QELS

Viscometric Detection, VISC

SEC3

Chemical Detectors.

Introduction

Mass Spectrometry, MS

Fourier Transform Infrared Spectroscopy, FT-IR

Nuclear Magnetic Resonance Spectroscopy, NMR

Other Chemical Detectors

Coupling of Chemical Detectors

Polymer Architecture And Dilute Solution Thermodynamics.

Introduction

Long-Chain Branching, LCB

Determining the Short-Chain Branching Distribution, SCBD

Polymer Architecture: Conformation and Topology

Star Polymers

Determining the Persistence Length, Lp

Determining the Characteristic Ratio, Cn

Local Polydispersity

Aqueous Sec.

Introduction

Aqueous SEC Columns

Non-Size-Exclusion Effects and Mobile Phase Additives

Select Applications of Aqueous SEC

OLigomeric Sec.

Introduction

What is an Oligomer?

Preliminary Considerations

Oligomeric SEC Columns

Select Applications of Oligomeric SEC

Optimizing Resolution in Oligomeric SEC

Sec In 2D-Lc Separations.

Introduction

Principles of 2D Polymer Separations

Designing an Experimental 2D-LC Protocol

Eluent Transfer in 2D-LC

Stop-Flow SEC - LC

Select Applications of 2D-LC

SEC in 3D Separations

Special Techniques.

Introduction

Preparative SEC

Recycle SEC

High-Speed SEC

Inverse SEC, ISEC

Vacancy and Differential SEC

Size-Exclusion Electrochromatography, SEEC

High-Temperature Sec And Rheological Connections.

Introduction

High-Temperature SEC, HT-SEC

Complementarity of SEC and Rheology

Symbols

Abbreviations

Index

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