GCMS书籍：《Handbook of GCMS：Fundmentals and Applications》

仪器资料 · 发表于 2017-9-30 08:43:55

1 Introduction 1
2 Fundamentals 7
2.1 Sample Preparation 7
2.1.1 Solid Phase Extraction 10
2.1.1.1 Solid Phase Microextraction 12
2.1.2 Supercritical Fluid Extraction 15
2.1.3 Pressurized Fluid Extraction 26
2.1.4 Online Liquid Chromatography Clean-up 29
2.1.5 Headspace Techniques 30
2.1.5.1 Static Headspace Technique 31
2.1.5.2 Dynamic Headspace Technique (Purge and Trap) 39
2.1.5.3 Headspace versus Purge and Trap 49
2.1.6 Adsorptive Enrichment and Thermodesorption 54
2.1.6.1 Sample Collection 57
2.1.6.2 Calibration 59
2.1.6.3 Desorption 60
2.1.7 Pyrolysis and Thermal Extraction 63
2.1.7.1 Foil Pyrolysis 64
2.1.7.2 Curie Point Pyrolysis 66
2.1.7.3 Thermal Extraction 68
2.2 Gas Chromatography 70
2.2.1 Fast Gas Chromatography 70
2.2.1.1 Fast Chromatography 70
2.2.1.2 Ultra Fast Chromatography 74
2.2.2 Two Dimensional Gas Chromatography 75
2.2.2.1 Heart Cutting 79
2.2.2.2 Comprehensive GCGC 79
2.2.2.3 Modulation 83
2.2.2.4 Detection 84
2.2.2.5 Data Handling 85
2.2.2.6 Moving Capillary Stream Switching 87
2.2.3 GC/MS Sample Inlet Systems 90
2.2.3.1 Carrier Gas Regulation 91
2.2.3.2 The Microseal Septum 94
2.2.3.3 Hot Sample Injection 95
2.2.3.4 Cold Injection Systems 100
2.2.3.5 Injection Volumes 108
2.2.3.6 On-column Injection 112
2.2.3.7 Cryofocusing 116
2.2.4 Capillary Columns 118
2.2.4.1 Sample Capacity 128
2.2.4.2 Internal Diameter 129
2.2.4.3 Film Thickness 130
2.2.4.4 Column Length 131
2.2.4.5 Adjusting the Carrier Gas Flow 132
2.2.4.6 Properties of Stationary Phases 134
2.2.5 Chromatography Parameters 137
2.2.5.1 The Chromatogram and its Meaning 138
2.2.5.2 Capacity Factor k 139
2.2.5.3 Chromatographic Resolution 140
2.2.5.4 Factors Affecting the Resolution 144
2.2.5.5 Maximum Sample Capacity 146
2.2.5.6 Peak Symmetry 146
2.2.5.7 Optimisation of Flow 147
2.2.6 Classical Detectors for GC/MS Systems 151
2.2.6.1 FID 151
2.2.6.2 NPD 153
2.2.6.3 ECD 155
2.2.6.4 PID 157
2.2.6.5 ELCD 159
2.2.6.6 FPD 161
2.2.6.7 PDD 162
2.2.6.8 Connection of Classical Detectors Parallel to the Mass Spectrometer 164
2.3 Mass Spectrometry 166
2.3.1 Resolving Power and Resolution in Mass Spectrometry 167
2.3.1.1 High Resolution 174
2.3.1.2 Unit Mass Resolution 178
2.3.1.3 High and Low Resolution in the Case of Dioxin Analysis 181
2.3.2 Time-of-Flight Analyser 183
2.3.3 Isotope Ratio Monitoring GC/MS 188
2.3.4 Ionisation Procedures 206
2.3.4.1 Electron Impact Ionisation 206
2.3.4.2 Chemical Ionisation 212
2.3.5 Measuring Techniques in GC/MS 231
2.3.5.1 Detection of the Complete Spectrum (Full Scan) 231
2.3.5.2 Recording Individual Masses (SIM/MID) 233
2.3.5.3 High Resolution Accurate Mass MID Data Acquisition 246
2.3.6 MS/MS –Tandem Mass Spectrometry 250
2.3.7 Mass Calibration 261
2.4 Special Aspects of GC/MS Coupling 269
2.4.1 Vacuum Systems 269
2.4.2 GC/MS Interface Solutions 274
2.4.2.1 Open Split Coupling 274
2.4.2.2 Direct Coupling 276
2.4.2.3 Separator Techniques 277
References for Chapter 2 278
3 Evaluation of GC/MS Analyses 293
3.1 Display of Chromatograms 293
3.1.1 Total Ion Current Chromatograms 294
3.1.2 Mass Chromatograms 295
3.2 Substance Identification 297
3.2.1 Extraction of Mass Spectra 297
3.2.2 The Retention Index 309
3.2.3 Libraries of Mass Spectra 313
3.2.3.1 Universal Mass Spectral Libraries 314
3.2.3.2 Application Libraries of Mass Spectra 317
3.2.4 Library Search Procedures 320
3.2.4.1 The INCOS/NIST Search Procedure 321
3.2.4.2 The PBM Search Procedure 328
3.2.4.3 The SISCOM Procedure 331
3.2.5 Interpretation of Mass Spectra 335
3.2.5.1 Isotope Patterns 337
3.2.5.2 Fragmentation and Rearrangement Reactions 343
3.2.5.3 DMOX Derivatives for Location of Double Bond Positions 350
3.2.6 Mass Spectroscopic Features of Selected Substance Classes 351
3.2.6.1 Volatile Halogenated Hydrocarbons 351
3.2.6.2 Benzene/Toluene/Ethylbenzene/Xylenes (BTEX, Alkylaromatics) 358
3.2.6.3 Polyaromatic Hydrocarbons (PAH) 358
3.2.6.4 Phenols 358
3.2.6.5 Pesticides 364
3.2.6.6 Polychlorinated Biphenyls (PCBs) 378
3.2.6.7 Polychlorinated Dioxins/Furans (PCDDs/PCDFs) 382
3.2.6.8 Drugs 383
3.2.6.9 Explosives 386
3.2.6.10 Chemical Warfare Agents 391
3.2.6.11 Brominated Flame Retardants (BFR) 394
3.3 Quantitation 395
3.3.1 Decision Limit 396
3.3.2 Limit of Detection 397
3.3.3 Limit of Quantitation 397
3.3.4 Sensitivity 399
3.3.5 The Calibration Function 399
3.3.6 Quantitation and Standardisation 401
3.3.6.1 External Standardization 401
3.3.6.2 Internal Standardisation 402
3.3.6.3 The Standard Addition Procedure 406
3.4 Frequently Occurring Impurities 407
References for Chapter 3 415
4 Applications 421
4.1 Air Analysis According to EPA Method TO-14 421
4.2 BTEX Using Headspace GC/MS 429
4.3 Simultaneous Determination of Volatile Halogenated Hydrocarbons
and BTEX 433
4.4 Static Headspace Analysis of Volatile Priority Pollutants 437
4.5 MAGIC 60 – Analysis of Volatile Organic Compounds 443
4.6 irm-GC/MS of Volatile Organic Compounds Using Purge and
Trap Extraction 451
4.7 Vinyl Chloride in Drinking Water 454
4.8 Chloral Hydrate in Surface Water 458
4.9 Field Analysis of Soil Air 461
4.10 Residual Monomers and Polymerisation Additives 465
4.11 Geosmin and Methylisoborneol in Drinking Water 468
4.12 Substituted Phenols in Drinking Water 472
4.13 GC/MS/MS Target Compound Analysis of Pesticide Residues
in Difficult Matrices 477
4.14 Multi-component Pesticide Analysis by MS/MS 489
4.15 Multi-method for the Determination of 239 Pesticides 498
4.16 Nitrophenol Herbicides in Water 505
4.17 Dinitrophenol Herbicides in Water 508
4.18 Hydroxybenzonitrile Herbicides in Drinking Water 514
4.19 Routine Analysis of 24 PAHs in Water and Soil 521
4.20 Fast GC Quantification of 16 EC Priority PAH Components 525
4.21 Analysis of Water Contaminants by On-line SPE-GC/MS 532
4.22 Determination of Polar Aromatic Amines by SPME 534
4.23 Congener Specific Isotope Analysis of Technical PCB Mixtures 540
4.24 Polychlorinated Biphenyls in Indoor Air 545
4.25 Confirmation Analysis of Dioxins and Dioxin-like PCBs 548
4.26 Fast GC Analysis for PCBs 554
4.27 Analysis of Brominated Flame Retardants PBDE 560
4.28 Trace Analysis of BFRs in Waste Water Using SPME-GC/MS/MS 568
4.29 Analysis of Military Waste 572
4.30 Detection of Drugs in Hair 582
4.31 Detection of Morphine Derivatives 584
4.32 Detection of Cannabis Consumption 589
4.33 Analysis of Steroid Hormones Using MS/MS 592
4.34 Determination of Prostaglandins Using MS/MS 596
4.35 Detection of Clenbuterol by CI 603
4.36 General Unknown Toxicological-chemical Analysis 607
4.37 Clofibric Acid in Aquatic Systems 611
4.38 Polycyclic Musks in Waste Water 616
4.39 Identification and Quantification of Trichothecene Mycotoxins 621
4.40 Highly Sensitive Screening and Quantification of Environmental
Components Using Chemical Ionisation with Water 625
4.41 Characterization of Natural Waxes by Pyrolysis-GC/MS 629
4.42 Quantitative Determination of Acrylate Copolymer Layers 633
References for Chapter 4 638
5 Glossary 639
Subject Index 693