The only comprehensive reference on this popular and rapidly developing technique provides a detailed overview, ranging from fundamentals to applications, including a section on the evaluation of GC-MS analyses.
As such, it covers all aspects, including the theory and principles, as well as a broad range of real-life examples taken from laboratories in environmental, food, pharmaceutical and clinical analysis. It also features a glossary of approximately 300 terms and a substance index that facilitates finding a specific application.
The first two editions were very well received, making this handbook a must-have in all analytical laboratories using GC-MS.
Autorentext
Hans-Joachim Huebschmann graduated as Certified Food Chemist from the Technical University in Berlin, Germany, working in the field of LC-MS residue analysis of anabolic agents and pesticides in food. He started his career in diagnostics and medical analytical instruments before working for a number of German companies in gas chromatography and mass spectrometry. In 2002 he joined Thermo Fisher Scientific in Bremen, Germany, and held different international positions including Channel Manager for inorganic and isotope ratio mass spectrometry, Product Manager for high resolution GC-MS and GC-MS/MS, setting up the well-known POPs Center of Excellence in Bremen, Germany. From his role as the Technology Manager for GC-MS in Austin, Texas, USA, he moved to Thermo Asia operations in Singapore as the Technology Director for GC & GC-MS. Hans very recently joined CTC Analytics AG, a privately owned Swiss company, supporting and developing front-end automation in gas and liquid chromatography for innovative sample preparation solutions.
Klappentext
Nowadays, gas chromatography/mass spectrometry is a frequently-used technique, with applications in food, pharmaceutical, clinical and environmental analysis. It allows both the separation of mixtures and the identification of the individual compounds of a mixture in one instrument.
This is the only comprehensive reference on the technique, providing a detailed overview ranging from fundamentals to applications. As such, it covers all aspects, including the theory and principles, as well as a broad range of real-life examples taken from laboratories. It also features a glossary of approximately 300 terms and a substance index that facilitates finding a specific application.
A must-have in all analytical laboratories using GC-MS.
Inhalt
Foreword XIII
Preface to the Third Edition XV
1 Introduction 1
1.1 The Historical Development of the GC-MS Technique 4
2 Fundamentals 7
2.1 Sample Preparation 7
2.1.1 Solid Phase Extraction 8
2.1.2 Solid Phase Microextraction 14
2.1.3 Pressurized Liquid Extraction 19
2.1.3.1 In-Cell Sample Preparation 23
2.1.3.2 In-Cell Moisture Removal 23
2.1.3.3 In-Cell Hydrocarbon Oxidation 24
2.1.4 Online Liquid Chromatography Clean-Up 25
2.1.5 Headspace Techniques 26
2.1.5.1 Static Headspace Technique 27
2.1.5.2 Dynamic Headspace Technique (Purge and Trap) 37
2.1.5.3 Coupling of Purge and Trap with GC-MS Systems 50
2.1.5.4 Headspace versus Purge and Trap 51
2.1.6 Adsorptive Enrichment and Thermal Desorption 57
2.1.6.1 Sample Collection 61
2.1.6.2 Calibration 62
2.1.6.3 Desorption 65
2.1.7 Pyrolysis 68
2.1.7.1 Foil Pyrolysis 70
2.1.7.2 Curie Point Pyrolysis 72
2.1.7.3 Micro-furnace Pyrolysis 75
2.1.8 Thermal Extraction (Outgassing) 76
2.1.9 QuEChERS Sample Preparation 79
2.2 Gas Chromatography 85
2.2.1 Sample Inlet Systems 85
2.2.2 Carrier Gas Regulation 87
2.2.2.1 Forward Pressure Regulation 87
2.2.2.2 Back Pressure Regulation 88
2.2.2.3 Carrier Gas Saving 89
2.2.3 Injection Port Septa 91
2.2.3.1 Septum Purge 93
2.2.3.2 The MicroSeal Septum 93
2.2.4 Injection Port Liner 95
2.2.4.1 Split Injection 95
2.2.4.2 Splitless Injection 96
2.2.4.3 Liner Activity and Deactivation 96
2.2.4.4 Liner Geometry 98
2.2.5 Vaporizing Sample Injection Techniques 99
2.2.5.1 Hot Needle Thermo Spray Injection Technique 100
2.2.5.2 Cold Needle Liquid Band Injection Technique 102
2.2.5.3 Filled Needle Injections 103
2.2.5.4 Split Injection 104
2.2.5.5 Splitless Injection (Total Sample Transfer) 104
2.2.5.6 Concurrent Solvent Recondensation 107
2.2.5.7 Concurrent Backflush 108
2.2.6 Temperature Programmable Injection Systems 114
2.2.6.1 The PTV Cold Injection System 115
2.2.6.2 The PTV Injection Procedures 117
2.2.6.3 On-Column Injection 124
2.2.6.4 PTV On-Column Injection 127
2.2.6.5 Cryofocussing 128
2.2.6.6 PTV Cryo-Enrichment 129
2.2.7 Capillary Column Choice and Separation Optimization 130
2.2.7.1 Sample Capacity 139
2.2.7.2 Internal Diameter 140
2.2.7.3 Film Thickness 141
2.2.7.4 Column Length 143
2.2.7.5 Setting the Carrier Gas Flow 144
2.2.7.6 Properties of Column Phases 145
2.2.7.7 Properties of Ionic Liquid Phases 150
2.2.8 Chromatography Parameters 153
2.2.8.1 The Chromatogram and Its Meaning 155
2.2.8.2 Capacity Factor k 156
2.2.8.3 Chromatographic Resolution 157
2.2.8.4 Factors Affecting the Resolution 159
2.2.8.5 Maximum Sample Capacity 163
2.2.8.6 Peak Symmetry 164
2.2.8.7 Optimization of Carrier Gas Flow 164
2.2.8.8 Effect of Oven Temperature Ramp Rate 168
2.2.9 Fast Gas Chromatography Solutions 169
2.2.9.1 Fast Chromatography 171
2.2.9.2 Ultra-Fast Chromatography 175
2.2.10 Multi-Dimensional Gas Chromatography 178
2.2.10.1 Heart Cutting 180
2.2.10.2 Comprehensive GC - GC×GC 180
2.2.10.3 Modulation 185
2.2.10.4 Detection 186
2.2.10.5 Data Handling 188
2.2.10.6 Moving Capillary Stream Switching 189
2.2.11 Classical Detectors for GC-MS Systems 192
2.2.11.1 Flame-Ionization Detector (FID) 192
2.2.11.2 Nitrogen-Phosphorous Detector (NPD) 194
2.2.11.3 Electron Capture Detector (ECD) 196
2.2.11.4 Photo Ionization Detector (PID) 199