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Tables of Contents for Gc/MS
Chapter/Section Title
Page #
Page Count
Preface
xi
 
PART I. A GC/MS PRIMER
1
58
1. INTRODUCTION
3
20
1.1. Why Use GC/MS?
4
1
1.2. Interpretation of Fragmentation Data Versus Spectral Library Searching
5
1
1.3. The Gas Chromatograph/Mass Spectrometer
6
10
1.3.1. A Model of the GC/MS System
7
3
1.3.2. A Column Separation Model
10
1
1.3.3. GC/MS Data Models
11
5
1.4. Systems and Costs
16
3
1.5. Competitive Analytical Systems
19
4
1.5.1. Liquid Chromatography/Mass Spectrometry (LC/MS)
19
1
1.5.2. Capillary Zone Electrophoresis/Mass Spectrometry (CZE/MS)
20
1
1.5.3. Supercritical Fluid Chromatography/Mass Spectrometry (SFC/MS)
21
2
2. SAMPLE PREPARATION AND INTRODUCTION
23
8
2.1. Direct Sample Injection into the Mass Spectrometer
23
2
2.1.1. Direct Insertion Probes and Fast Atom Bombardment
24
1
2.1.2. Head Space Analyzers
25
1
2.2. Sample Purification
25
2
2.3. Manual GC Injection
27
2
2.4. Automated GC/MS Injection
29
2
3. THE GAS CHROMATOGRAPH
31
9
3.1. The GC Oven and Temperature Control
31
1
3.2. Selecting GC Columns
32
2
3.3. Separation Parameters and Resolution
34
2
3.4. GC Control Variables
36
2
3.5. Derivatives
38
2
4. THE MASS SPECTROMETER
40
10
4.1. Vacuum Pumps
40
3
4.2. Interfaces and Sources
43
4
4.3. Quadrupole Operation
47
2
4.4. The Ion Detector
49
1
5. GETTING STARTED IN GC/MS
50
9
5.1. Mode Selection
50
1
5.2. Setting Up
51
2
5.3. Mass Spectrometer Tuning and Calibration
53
2
5.4. Sample Injection and Chromatographic Separation
55
3
5.5. Data Collection Processing
58
1
PART II. GC/MS OPTIMIZATION
59
38
6. CHROMATOGRAPHIC METHODS DEVELOPMENT
61
7
6.1. Isothermal Operation
62
1
6.2. Linear Temperature Gradients
63
1
6.3. Assisted Reequilibration
63
1
6.4. Hinge Point Gradient Modification
64
2
6.5. Pressure Gradient Development
66
1
6.6. Column Replacement
67
1
7. MASS SPECTROMETER SETUP AND OPERATION
68
11
7.1. Mass Spectrometer Calibration with Calibration Gases
68
2
7.2. Mass Axis Tuning
70
2
7.3. Using System Tuning Compounds in Environmental Analysis
72
3
7.4. Acquiring Information
75
2
7.5. Data Displays and Library Searches
77
2
8. DATA PROCESSING AND NETWORK INTERFACING
79
8
8.1. Peak Identification and Integration
79
2
8.2. Multi-instrument Control
81
1
8.3. Networking Connection
82
1
8.4. Replacement Control and Processing Systems
82
1
8.5. File Conversion and Data File Exchange
83
2
8.6. Data Reentry and Transcription Errors
85
2
9. SYSTEM MAINTENANCE AND TROUBLESHOOTING
87
10
9.1. Gas Chromatograph Maintenance
87
2
9.1.1. Injector Port and Liner
87
1
9.1.2. Septum Replacement
88
1
9.1.3. Syringe Cleaning
88
1
9.1.4. Carrier Gas Selection and Purification
88
1
9.2. Mass Spectrometer Maintenance
89
5
9.2.1. Problem Diagnostics
89
1
9.2.2. Source Cleaning
90
3
9.2.3. Cleaning Quadrupole Rods
93
1
9.2.4. Detector Replacement
93
1
9.2.5. Pump Maintenance and Oil Change
94
1
9.3. System Electrical Grounding
94
3
PART III. SPECIFIC APPLICATIONS OF MASS SPECTROMETRY
97
47
10. GC/MS IN THE ENVIRONMENTAL LABORATORY
99
15
10.1. Volatile Organic Analysis: EPA Method 624
100
4
10.2. Semi-volatile Organic Analysis: EPA Method 625
104
9
10.3. EPA and State Reporting Requirements
113
1
11. AN INTRODUCTION TO STRUCTURAL INTERPRETATION
114
7
11.1. History of the Sample
116
1
11.2. Elemental Composition
117
2
11.3. Search for Logical Fragmentation Intervals
119
2
12. ION TRAP GC/MS SYSTEMS
121
7
12.1. Ion Trap Components
122
1
12.2. Ion Trap Operation
122
4
12.3. Ion Traps in the Environmental Laboratory
126
1
12.4. Chemical Ionization in the Ion Trap
126
1
12.5. Ion Trap GC/MS/MS
127
1
13. OTHER GC/MS SYSTEMS
128
9
13.1. Sequential Mass Spectrometry (Triple-Quadruple or Tandem GC/MS)
128
3
13.2. Magnetic Sector Systems
131
2
13.3. Laser Time-of-Flight (GC/TOF-MS) GC/MS Systems
133
1
13.4. Fourier Transform (GC/FT-MS) GC/MS Systems
134
3
14. AN INTRODUCTION TO LC/MS
137
7
14.1. Liquid Interfacing into the Mass Spectrometer
138
1
14.2. Thermospray LC/MS
139
1
14.3. Electrospray LC/MS
140
1
14.4. Atmospheric Pressure Interface LC/MS
141
1
14.5. Ion Spray LC/MS
142
1
14.6. Automated Mass Chromatogram Quantitation
143
1
14.7. Future of LC/MS
143
1
APPENDIX A. GC/MS TROUBLESHOOTING QUICK REFERENCE
144
6
APPENDIX B. SOURCES OF GC/MS BACKGROUND AND CONTAMINATION
150
3
APPENDIX C. GLOSSARY OF GC/MS TERMS
153
6
APPENDIX D. GC/MS SELECTED READING LIST
159
2
INDEX
161