GC/MS: A Practical User's Guide, Second Edition

GC/MS......Page 4
CONTENTS......Page 10
PREFACE......Page 14
PART I A GC/MS PRIMER......Page 16
1 Introduction......Page 18
1.1 Why Use GC/MS?......Page 19
1.2 Interpretation of Fragmentation Data Versus Spectral Library Searching......Page 20
1.3 The Gas Chromatograph/Mass Spectrometer......Page 21
1.4 Systems and Costs......Page 30
1.5 Competitive Analytical Systems......Page 32
2 Sample Preparation and Introduction......Page 36
2.1 Direct Sample Injection into the Mass Spectrometer......Page 37
2.2 Sample Purification......Page 38
2.3 Manual GC Injection......Page 40
2.4 Automated GC/MS Injection......Page 42
3.1 The GC Oven and Temperature Control......Page 44
3.2 Selecting GC Columns......Page 45
3.3 Separation Parameters and Resolution......Page 47
3.4 GC Control Variables......Page 49
3.5 Derivatives......Page 51
4.1 Vacuum Pumps......Page 52
4.2 Interfaces and Sources......Page 55
4.3 Quadrupole Operation......Page 58
4.4 The Ion Detector......Page 60
5.1 Mode Selection......Page 62
5.2 Setting Up......Page 63
5.3 Mass Spectrometer Tuning and Calibration......Page 65
5.5 Data Collection Processing......Page 67
PART II A GC/MS OPTIMIZATION......Page 72
6 Chromatographic Methods Development......Page 74
6.1 Isothermal Operation......Page 75
6.3 Assisted Re-Equilibration......Page 76
6.4 Hinge Point Gradient Modification......Page 77
6.5 Pressure Gradient Development......Page 78
6.6 Column Replacement......Page 79
7.1 Mass Spectrometer Calibration with Calibration Gases......Page 82
7.2 Mass Axis Tuning......Page 84
7.3 System Tuning for Environmental Analysis......Page 86
7.4 Acquiring Information......Page 88
7.5 Data Displays and Library Searches......Page 90
8.1 Peak Identification and Integration......Page 92
8.2 Multi-Instrument Control......Page 94
8.4 Replacement Control and Processing Systems......Page 95
8.5 File Conversion and Data File Exchange......Page 96
8.6 Data Re-Entry and Transcription Errors......Page 98
9.1 Gas Chromatograph Maintenance......Page 100
9.2 Mass Spectrometer Maintenance......Page 102
9.3 System Electrical Grounding......Page 107
PART III SPECIFIC APPLICATIONS OF GC/MS......Page 108
10 GC/MS in The Environmental Laboratory......Page 110
10.1 Volatile Organic Analysis: EPA Method 624......Page 111
10.2 SemiVolatile Organic Analysis: EPA Method 625......Page 115
10.3 EPA and State Reporting Requirements......Page 120
11 GC/MS in Forensics, Toxicology, and Space Science......Page 124
11.2 Clinical Drug Analysis......Page 125
11.4 Astrochemistry......Page 126
12 An Introduction to Structural Interpretation......Page 128
12.1 History of the Sample......Page 130
12.2 Elemental Composition......Page 131
12.3 Search for Logical Fragmentation Intervals......Page 133
13 Ion Trap GC/MS Systems......Page 134
13.2 Ion Trap Operation......Page 135
13.3 The Linear Ion Trap Analyzer......Page 139
13.6 Ion Trap GC/MS/MS......Page 140
14 Other GC/MS Systems......Page 142
14.1 Sequential Mass Spectrometry (Triple-Quadrupole or Tandem GC/MS)......Page 143
14.2 Magnetic Sector Systems......Page 145
14.3 Laser Time-of-Flight (GC/TOF-MS) GC/MS Systems......Page 147
14.4 Fourier Transform (GC/FT-MS) GC/MS Systems......Page 148
15 An Introduction to LC/MS......Page 152
15.1 Liquid Interfacing into the Mass Spectrometer......Page 153
15.2 Electrospray and Nano-Spray LC/MS......Page 154
15.3 Ion Spray LC/MS......Page 155
15.5 LC/MS Versus GC/MS......Page 157
16 Innovation in GC/MS......Page 160
16.1 Microfludics in GC/MS......Page 161
16.4 Portable GC/MS Systems......Page 162
16.5 New Column Technology......Page 163
A.1 GC FAQs......Page 166
A.3 MS FAQs......Page 168
A.4 GC/MS FAQs......Page 170
B.1 GC Injector Problems......Page 174
B.2 GC Column Problems......Page 175
B.3 MS Vacuum and Power Problems......Page 177
B.4 MS Source and Calibration Problems......Page 178
B.5 MS Sensitivity and Detector Problems......Page 179
Appendix C Sources of GC/MS Background Contamination......Page 180
Appendix D A Glossary of GC/MS Terms......Page 182
E.2 Books......Page 188
INDEX......Page 190