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STATIC HEADSPACE-GAS CHROMATOGRAPHY
THE ONLY REFERENCE TO PROVIDE BOTH CURRENT AND THOROUGH COVERAGE OF THIS IMPORTANT ANALYTICAL TECHNIQUE
Static headspace-gas chromatography (HS-GC) is an indispensable technique for analyzing volatile organic compounds, enabling the analyst to assay a variety of sample matrices while avoiding the costly and time-consuming preparation involved with traditional GC.
Static Headspace-Gas Chromatography: Theory and Practice has long been the only reference to provide in-depth coverage of this method of analysis. The Second Edition has been thoroughly updated to reflect the most recent developments and practices, and also includes coverage of solid-phase microextraction (SPME) and the purge-and-trap technique. Chapters cover:
Principles of static and dynamic headspace analysis, including the evolution of HS-GC methods and regulatory methods using static HS-GC
Basic theory of headspace analysis--physicochemical relationships, sensitivity, and the principles of multiple headspace extraction
HS-GC techniques--vials, cleaning, caps, sample volume, enrichment, and cryogenic techniques
Sample handling
Cryogenic HS-GC
Method development in HS-GC
Nonequilibrium static headspace analysis
Determination of physicochemical functions such as vapor pressures, activity coefficients, and more
Comprehensive and focused, Static Headspace-Gas Chromatography, Second Edition provides an excellent resource to help the reader achieve optimal chromatographic results. Practical examples with original data help readers to master determinations in a wide variety of areas, such as forensic, environmental, pharmaceutical, and industrial applications.
Auteur
Dr. BRUNO KOLB is an internationally recognized expert on gas chromatography. Until his retirement in 1996, he managed the GC Applications Laboratory at Perkin-Elmer Corporation, Germany; he has also been involved in instrument development with special emphasis on specific detectors. He has been a guest lecturer at the University of Konstanz, as well as at international meetings. He has published many journal articles and book chapters, and is the author of a textbook on gas chromatography.
Dr. LESLIE S. ETTRE was a senior scientist at Perkin-Elmer Corporation until his retirement in 1990. Between 1988 and 1995 he served as an adjunct professor in the Department of Chemical Engineering at Yale University, and from 1995 until 2004 he continued his association with the school as a research affiliate. In addition to lecturing widely in the field of gas chromatography, Dr. Ettre has published over 200 scientific and technical papers, and is the author and editor of numerous books, including Encyclopedia of Industrial Chemical Analysis. He has received numerous awards, including the National Award in Chromatography of the American Chemical Society and the AJP Martin Award of the Chromatographic Societythe highest honors in the United States and Europe, respectively.
Résumé
STATIC HEADSPACE-GAS CHROMATOGRAPHY THE ONLY REFERENCE TO PROVIDE BOTH CURRENT AND THOROUGH COVERAGE OF THIS IMPORTANT ANALYTICAL TECHNIQUE Static headspace-gas chromatography (HS-GC) is an indispensable technique for analyzing volatile organic compounds, enabling the analyst to assay a variety of sample matrices while avoiding the costly and time-consuming preparation involved with traditional GC. Static Headspace-Gas Chromatography: Theory and Practice has long been the only reference to provide in-depth coverage of this method of analysis. The Second Edition has been thoroughly updated to reflect the most recent developments and practices, and also includes coverage of solid-phase microextraction (SPME) and the purge-and-trap technique. Chapters cover:
Contenu
Preface xi
Preface to the First Edition xv
List of Acronyms and Symbols xix
1 General Introduction 1
1.1 Principles of Headspace Analysis 1
1.2 Types of Headspace Analysis 3
1.2.1 Principles of Static HS-GC 4
1.2.2 Principles of Dynamic HS-GC 5
1.2.2.1 The Trap 5
1.2.2.2 The Water Problem 7
1.2.2.3 The Flow Problem 7
1.2.2.4 The Time Problem 8
1.2.2.5 Comparison of Static HS-GC with P&T 9
1.3 The Evolution of the HS-GC Methods 10
1.4 HS-GS Literature 12
1.5 Regulatory Methods Utilizing (Static) HS-GC 13
References 15
2 Theoretical Background of HS-GC and Its Applications 19
2.1 Basic Theory of Headspace Analysis 19
2.2 Basic Physicochemical Relationships 23
2.3 Headspace Sensitivity 25
2.3.1 Influence of Temperature on Vapor Pressure and Partition Coefficient 26
2.3.1.1 Enhancement of Lower Boiling Compounds 28
2.3.2 Influence of Temperature on Headspace Sensitivity for Compounds with Differing Partition Coefficients 29
2.3.3 Influence of Sample Volume on Headspace Sensitivity for Compounds with Differing Partition Coefficients 34
2.3.3.1 Sample-to-Sample Reproducibility 36
2.3.4 Changing the Sample Matrix by Varying the Activity Coefficient 37
2.4 Headspace Linearity 42
2.5 Duplicate Analyses 43
2.6 Multiple Headspace Extraction (MHE) 45
2.6.1 Principles of MHE 45
2.6.2 Theoretical Background of MHE 46
2.6.3 Simplified MHE Calculation 49
References 49
3 The Technique of HS-GC 51
3.1 Sample Vials 53
3.1.1 Vial Types 53
3.1.2 Selection of the Vial Volume 54
3.1.3 Vial Cleaning 55
3.1.4 Wall Adsorption Effects 55
3.2 Caps 56
3.2.1 Pressure on Caps 58
3.2.2 Safety Closures 58
3.3 Septa 58
3.3.1 Septa Types 58
3.3.2 Septum Blank 60
3.3.3 Should a Septum Be Pierced Twice? 62
3.3.3.1 Closed-Vial versus Open-Vial Sample Introduction Technique 65
3.4 Thermostatting 66
3.4.1 Influence of Temperature 66
3.4.2 Working Modes 69
3.5 The Fundamental Principles of Headspace Sampling Systems 70
3.5.1 Systems Using Gas Syringes 70
3.5.2 Solid Phase Microextraction (SPME) 73
3.5.2.1 Comparison of the Sensitivities in HS-SPME and Direct Static HS-GC 80
3.5.3 Balanced Pressure Sampling Systems 81
3.5.4 Pressure/Loop Systems 83
3.5.5 Conditions for Pressurization Systems 84
3.5.6 Volume of the Headspace Gas Sample 86
3.5.6.1 Sample Volume with Gas Syringes 87
3.5.6.2 Sample Volume with Loop Systems 87
3.5.6.3 Sample Volume with the Balanced Pressure System 88
3.6 Use of Open-Tubular (Capillary) Columns 89
3.6.1 Properties of Open-Tubular Columns for Gas Samples 89
3.6.2 Headspace Sampling with Split or Splitless Introduction 90
3.6.3 Comparison of Split and Splitless Headspace Sampling 93
3.6.4 Band Broadening During Sample Introduction 96
3.6.5 Influence of Temperature on Band Broadening 99
3.6.5.1 Conclusions 101
3.6.6 The Combination of Different Columns and Detectors 101
3.7 Enrichment Techniques in HS-GC 105
3.7.1 Systems for Cryogenic Trapping 108
3.7.1.1 Trapping by Cryogenic Condens…