Gas Chromatography with Glass Capillary Columns

Gas Chromatography with Glass Capillary Columns describes glass capillary technology and the selection, installation, evaluation, and use of glass open tubular columns for gas chromatography. Discussions are organized around the glass capillary column; column coating and installation; inlet systems; measurement of column efficiency; temperature programming and carrier flow; and retention behavior. Column selection and stability and sample preparation are also covered. This text is comprised of 13 chapters; the first of which introduces the reader to the practical considerations involved in the selection, installation, evaluation, and use of high-resolution open tubular glass capillary columns, along with the theory of the chromatographic process. The discussion then turns to the influence of operating parameters and storage conditions on the interrelated forces involved in coating glass capillary columns; the dynamic and static techniques of column coating; and design defects in the inlet system caused by excessive volume and dead space. The chapters that follow focus on general considerations in column attachment, measurement of column efficiency, and retention behavior of carrier gas, along with the operating temperature of the column, the choice of carrier gas, and carrier gas velocity. This book also looks at the factors that affect column stability, materials of restricted volatility, and some applications of glass capillary gas chromatography. This reference material is intended primarily for students and researchers interested in gas chromatography with glass capillary columns.

Preface

Chapter 1 Introduction

1.1 General Considerations

1.2 Theory of the Chromatographic Process

1.3 Separation of Components

References

Chapter 2 The Glass Capillary Column

2.1 Introduction

2.2 Surface Pretreatments

References

Chapter 3 Column Coating

3.1 General Considerations

3.2 Dynamic Techniques

3.3 Static Techniques

3.4 PLOT and SCOT Columns

3.5 Bonded Phases

3.6 Packed Capillary and Micropacked Columns

References

Chapter 4 Inlet Systems

4.1 General Considerations

4.2 Precolumn Concentration

4.3 Splitless Injection

4.4 Inlet Splitters

References

Chapter 5 Column Installation

5.1 General Considerations

5.2 Unitized Assemblies

5.3 Make-Up Gas

5.4 Initial Evaluation

References

Chapter 6 Measuring Column Efficiency

6.1 General Considerations

6.2 Separation Number, Trennzahl (TZ)

6.3 Other Concepts of Column Performance

References

Chapter 7 Treatment of Retention Data

7.1 General Considerations

7.2 Calculation of the Hold-up Volume, tM

7.3 The Kovats Retention Index System, I

7.4 Effects of Temperature on I

7.5 Other Retention Systems

7.6 Retention Data as Identification Criteria

References

Chapter 8 Temperature Programming and Carrier Flow Considerations

8.1 General Considerations

8.2 Special Problems with Capillary Systems

8.3 Optimum Practical Gas Velocity

8.4 Retention Temperature and Analysis Time versus Program and Flow Rates

References

Chapter 9 Column Stability

9.1 General Considerations

9.2 Effects of Temperature

9.3 Effect of Injection Size and Sample Composition

9.4 Salvaging Columns

References

Chapter 10 Column Selection

10.1 General Comments

10.2 The Rohrschneider Concept of Polarity

10.3 Other Methods of Selection

10.4 Role of Column Efficiency

References

Chapter 11 Sample Preparation

11.1 General Considerations

11.2 Headspace Concentrates versus Total Volatile Analysis

11.3 Direct Headspace Analysis

11.4 General Considerations on Methods of Isolation and Concentration

11.5 Distillation

11.6 Freeze Concentration

11.7 Extraction

11.8 Zone Refining

11.9 Adsorptive Methods

11.10 Porous Polymer Absorption

References

Chapter 12 Analysis of Materials of Restricted Volatility

12.1 General Comments

12.2 Pyrolysis Gas Chromatography

12.3 Silylation

12.4 Silylation Methods

References

Chapter 13 Applications of Glass Capillary Gas Chromatography

13.1 Introduction

13.2 Air and Smoke Analyses

13.3 Amino Acid Analysis

13.4 Drug and Pharmaceuticals

13.5 Fatty Acid Analysis

13.6 Food and Beverage Analysis

13.7 Pesticides

13.8 Saccharide Analysis

13.9 Steroid Analysis

13.10 Miscellaneous

References

Appendix I Nomenclature

Appendix II Liquid Phases

Appendix III Porous Polymer Data

Appendix IV Silylation and Derivatization Reactions

Index