Hans-Joachim Hubschmann. Handbook ofgc-ms. Fundamentals and Applications. Third Edition. Wl LEY-VCH. VerlagGmbH & Co. KG aa
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1 Hans-Joachim Hubschmann Handbook ofgc-ms Fundamentals and Applications Third Edition Wl LEY-VCH VerlagGmbH & Co. KG aa
2 VII Foreword XIII Preface to the Third Edition XV 1 Introduction The Historical Development of the GC-MS Technique 4 2 Fundamentals Sample Preparation Solid Phase Extraction Solid Phase Microextraction Pressurized Liquid Extraction In-Cell Sample Preparation In-Cell Moisture Removal In-Cell Hydrocarbon Oxidation Online Liquid Chromatography Clean-Up Headspace Techniques Static Headspace Technique Dynamic Headspace Technique (Purge and Trap) Coupling of Purge and Trap with GC-MS Systems Headspace versus Purge and Trap Adsorptive Enrichment and Thermal Desorption Sample Collection Calibration Desorption Pyrolysis Foil Pyrolysis Curie Point Pyrolysis Micro-furnace Pyrolysis Thermal Extraction (Outgassing) QuEChERS Sample Preparation Gas Chromatography Sample Inlet Systems 85
3 VIII Carrier Gas Regulation Forward Pressure Regulation Back Pressure Regulation Carrier Gas Saving Injection Port Septa Septum Purge The MicroSeal Septum Injection Port Liner Split Injection Splitless Injection Liner Activity and Deactivation Liner Geometry Vaporizing Sample Injection Techniques Hot Needle Thermo Spray Injection Technique Cold Needle Liquid Band Injection Technique Filled Needle Injections Split Injection Splitless Injection (Total Sample Transfer) Concurrent Solvent Recondensation Concurrent Backflush Temperature Programmable Injection Systems The PTV Cold Injection System The PTV Injection Procedures On-Column Injection PTV On-Column Injection Cryofocussing PTV Cryo-Enrichment Capillary Column Choice and Separation Optimization Sample Capacity Internal Diameter Film Thickness Column Length Setting the Carrier Gas Flow Properties of Column Phases Properties of Ionic Liquid Phases Chromatography Parameters The Chromatogram and Its Meaning Capacity Factor k' Chromatographic Resolution Factors Affecting the Resolution Maximum Sample Capacity Peak Symmetry Optimization of Carrier Gas Flow Effect of Oven Temperature Ramp Rate Fast Gas Chromatography Solutions 169
4 GC IX Fast Chromatography Ultra-Fast Chromatography Multi-Dimensional Gas Chromatography Heart Cutting Comprehensive GC Modulation Detection Data Handling 188 X GC Moving Capillary Stream Switching Classical Detectors for GC-MS Systems Flame-Ionization Detector (FID) Nitrogen-Phosphorous Detector (NPD) Electron Capture Detector (ECD) Photo Ionization Detector (PID) Electrolytical Conductivity Detector (ELCD) Flamephotometric Detector (FPD) Pulsed Discharge Detector (PDD) Olfactometry Classical Detectors Parallel to the Mass Spectrometer MicroChannel Devices Mass Spectrometry Ionization Processes Reading Mass Spectra Electron Ionization Chemical Ionization Resolution Power Resolving Power and Resolution in Mass Spectrometry Unit Mass Resolution High Mass Resolution The Orbitrap Analyser High and Low Mass Resolution in the Case of Dioxin Analysis Time-of-Flight Analyser Isotope Ratio Monitoring GC-MS The Principles of Isotope Ratio Monitoring Notations in irm-gc-ms Isotopic Fractionation irm-gc-ms Technology The Open Split Interface Compound Specific Isotope Analysis On-Line Combustion for 5 13C and 5 15N Determination The Oxidation Reactor The Reduction Reactor Water Removal The Liquid Nitrogen Trap 277
5 Tandem X j On-Line High Temperature Conversion for 8 2H and 5 lso Determination Mass Spectrometer for Isotope Ratio Analysis Injection of Reference Gases Isotope Reference Materials Acquisition Techniques in GC-MS Detection of the Complete Mass Spectrum (Full Scan) Recording Individual Masses (SIM/MID) High Resolution Accurate Mass MID Data Acquisition MS/MS Mass Calibration Vacuum Systems 332 References 336 Mass Spectrometry Evaluation of GC-MS Analyses Display of Chromatograms Total Ion Current Chromatograms Mass Chromatograms Substance Identification Extraction of Mass Spectra Manual Spectrum Subtraction Deconvolution of Mass Spectra The Retention Index Libraries of Mass Spectra Universal Mass Spectral Libraries Application Libraries ofmass Spectra Library Search Programs The NIST Search Procedure The PBM Search Procedure The SISCOM Procedure Interpretation of Mass Spectra Isotope Patterns Fragmentation and Rearrangement Reactions DMOX Derivatives for Location of Double Bond Positions Mass Spectroscopic Features of Selected Substance Classes Volatile Halogenated Hydrocarbons Benzene/Toluene/Ethylbenzene/Xylenes (BTEX, Alkylaromatics) Polyaromatic Hydrocarbons (PAHs) Phenols Pesticides Polychlorinated Biphenyls (PCBs) Polychlorinated Dioxins/Furans (PCDDs/PCDFs) 4S Drugs Explosives 455
6 Analysis XI Chemical Warfare Agents Brominated Flame Retardants (BFR) Quantitation Acquisition Rate Decision Limit Limit of Detection Limit of Quantitation Sensitivity The Calibration Function Quantitation and Standardization External Standardization Internal Standardization The Standard Addition Procedure The Accuracy of Analytical Data Frequently Occurring Impurities 479 References Applications Air Analysis According to EPA Method TO BTEX in Surface Water as of EPA Method Simultaneous Determination of Volatile Halogenated Hydrocarbons and BTEX Static Headspace Analysis of Volatile Priority Pollutants MAGIC 60 - of Volatile Organic Compounds irm-gc-ms of Volatile Organic Compounds Using Purge and Trap Extraction Geosmin and Methylisoborneol in Drinking Water Polycyclic Musks in Waste Water Organotin Compounds in Water Multi-Method for Pesticides by Single Quadrupole MS Analysis of Dithiocarbamate Pesticides GC-MS/MS Target Compound Analysis of Pesticide Residues in Difficult Matrices Multi-Component Pesticide Analysis by MS/MS Multiresidue Pesticides Analysis in Ayurvedic Churna Determination of Polar Aromatic Amines by SPME Analysis of Nitrosamines in Beer Phthalates in Liquors Analysis of the Natural Spice Ingredients Capsaicin, Piperine, Thymol and Cinnamaldehyde Aroma Profiling of Cheese by Thermal Extraction Allergens Analysis of Azo Dyes in Leather and Textiles Identification of Extractables and Leachables Metabolite Profiling of Natural Volatiles and Extracts 652
7 XII j 4.24 Fast GC Quantification of 16 EC Priority PAH Components Multiclass Environmental Contaminants in Fish FastGCofPCBs Congener Specific Isotope Analysis of Technical PCB Mixtures Dioxin Screening in Food and Feed Confirmation Analysis of Dioxins and Dioxin-like PCBs Analysis of Brominated Flame Retardants PBDE SPME Analysis of PBBs Analysis of Military Waste Comprehensive Drug Screening and Quantitation Determination of THC-Carbonic Acid in Urine by NCI Detection of Drugs in Hair Screening for Drugs of Abuse Structural Elucidation by Chemical Ionization and MS/MS Volatile Compounds in Car Interior Materials 752 References 758 Glossary 769 Further Reading 843 Index 845
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