Handbook of GC MS fundamentals and applications 3rd Edition by Hans Joachim Hubschmann 3527334742 9783527334742

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Product details:

ISBN 10: 3527334742 

ISBN 13: 9783527334742

Author: Hans Joachim Hubschmann

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.

Table of contents:

1 Introduction

1.1 The Historical Development of the GC-MS Technique

2 Fundamentals

2.1 Sample Preparation
 2.1.1 Solid Phase Extraction
 2.1.2 Solid Phase Microextraction
 2.1.3 Pressurized Liquid Extraction
  2.1.3.1 In-Cell Sample Preparation
  2.1.3.2 In-Cell Moisture Removal
  2.1.3.3 In-Cell Hydrocarbon Oxidation
 2.1.4 Online Liquid Chromatography Clean-Up
 2.1.5 Headspace Techniques
  2.1.5.1 Static Headspace Technique
  2.1.5.2 Dynamic Headspace Technique (Purge and Trap)
  2.1.5.3 Coupling of Purge and Trap with GC-MS Systems
  2.1.5.4 Headspace versus Purge and Trap
 2.1.6 Adsorptive Enrichment and Thermal Desorption
  2.1.6.1 Sample Collection
  2.1.6.2 Calibration
  2.1.6.3 Desorption
 2.1.7 Pyrolysis
  2.1.7.1 Foil Pyrolysis
  2.1.7.2 Curie Point Pyrolysis
  2.1.7.3 Micro-furnace Pyrolysis
 2.1.8 Thermal Extraction (Outgassing)
 2.1.9 QuEChERS Sample Preparation

2.2 Gas Chromatography
 2.2.1 Sample Inlet Systems
 2.2.2 Carrier Gas Regulation
  2.2.2.1 Forward Pressure Regulation
  2.2.2.2 Back Pressure Regulation
  2.2.2.3 Carrier Gas Saving
 2.2.3 Injection Port Septa
  2.2.3.1 Septum Purge
  2.2.3.2 The MicroSeal Septum
 2.2.4 Injection Port Liner
  2.2.4.1 Split Injection
  2.2.4.2 Splitless Injection
  2.2.4.3 Liner Activity and Deactivation
  2.2.4.4 Liner Geometry
 2.2.5 Vaporizing Sample Injection Techniques
  2.2.5.1 Hot Needle Thermo Spray Injection Technique
  2.2.5.2 Cold Needle Liquid Band Injection Technique
  2.2.5.3 Filled Needle Injections
  2.2.5.4 Split Injection
  2.2.5.5 Splitless Injection (Total Sample Transfer)
  2.2.5.6 Concurrent Solvent Recondensation
  2.2.5.7 Concurrent Backflush
 2.2.6 Temperature Programmable Injection Systems
  2.2.6.1 The PTV Cold Injection System
  2.2.6.2 The PTV Injection Procedures
  2.2.6.3 On-Column Injection
  2.2.6.4 PTV On-Column Injection
  2.2.6.5 Cryofocussing
  2.2.6.6 PTV Cryo-Enrichment
 2.2.7 Capillary Column Choice and Separation Optimization
  2.2.7.1 Sample Capacity
  2.2.7.2 Internal Diameter
  2.2.7.3 Film Thickness
  2.2.7.4 Column Length
  2.2.7.5 Setting the Carrier Gas Flow
  2.2.7.6 Properties of Column Phases
  2.2.7.7 Properties of Ionic Liquid Phases
 2.2.8 Chromatography Parameters
  2.2.8.1 The Chromatogram and Its Meaning
  2.2.8.2 Capacity Factor k′
  2.2.8.3 Chromatographic Resolution
  2.2.8.4 Factors Affecting the Resolution
  2.2.8.5 Maximum Sample Capacity
  2.2.8.6 Peak Symmetry
  2.2.8.7 Optimization of Carrier Gas Flow
  2.2.8.8 Effect of Oven Temperature Ramp Rate
 2.2.9 Fast Gas Chromatography Solutions
  2.2.9.1 Fast Chromatography
  2.2.9.2 Ultra-Fast Chromatography
 2.2.10 Multi-Dimensional Gas Chromatography
  2.2.10.1 Heart Cutting
  2.2.10.2 Comprehensive GC – GC×GC
  2.2.10.3 Modulation
  2.2.10.4 Detection
  2.2.10.5 Data Handling
  2.2.10.6 Moving Capillary Stream Switching
 2.2.11 Classical Detectors for GC-MS Systems
  2.2.11.1 Flame-Ionization Detector (FID)
  2.2.11.2 Nitrogen-Phosphorous Detector (NPD)
  2.2.11.3 Electron Capture Detector (ECD)
  2.2.11.4 Photo Ionization Detector (PID)
  2.2.11.5 Electrolytical Conductivity Detector (ELCD)
  2.2.11.6 Flamephotometric Detector (FPD)
  2.2.11.7 Pulsed Discharge Detector (PDD)
  2.2.11.8 Olfactometry
  2.2.11.9 Classical Detectors Parallel to the Mass Spectrometer
  2.2.11.10 Microchannel Devices

2.3 Mass Spectrometry
 2.3.1 Ionization Processes
  2.3.1.1 Reading Mass Spectra
  2.3.1.2 Electron Ionization
  2.3.1.3 Chemical Ionization
 2.3.2 Resolution Power
  2.3.2.1 Resolving Power and Resolution in Mass Spectrometry
  2.3.2.2 Unit Mass Resolution
  2.3.2.3 High Mass Resolution
  2.3.2.4 The Orbitrap Analyser
  2.3.2.5 High and Low Mass Resolution in the Case of Dioxin Analysis
  2.3.2.6 Time-of-Flight Analyser
 2.3.3 Isotope Ratio Monitoring GC-MS
  2.3.3.1 The Principles of Isotope Ratio Monitoring
  2.3.3.2 Notations in irm-GC-MS
  2.3.3.3 Isotopic Fractionation
  2.3.3.4 irm-GC-MS Technology
  2.3.3.5 The Open Split Interface
  2.3.3.6 Compound Specific Isotope Analysis
  2.3.3.7 On-Line Combustion for δ 13C and δ 15N Determination
  2.3.3.8 The Oxidation Reactor
  2.3.3.9 The Reduction Reactor
  2.3.3.10 Water Removal
  2.3.3.11 The Liquid Nitrogen Trap
  2.3.3.12 On-Line High Temperature Conversion for δ 2H and δ 18O Determination
  2.3.3.13 Mass Spectrometer for Isotope Ratio Analysis
  2.3.3.14 Injection of Reference Gases
  2.3.3.15 Isotope Reference Materials
 2.3.4 Acquisition Techniques in GC-MS
  2.3.4.1 Detection of the Complete Mass Spectrum (Full Scan)
  2.3.4.2 Recording Individual Masses (SIM/MID)
  2.3.4.3 High Resolution Accurate Mass MID Data Acquisition
  2.3.4.4 MS/MS – Tandem Mass Spectrometry
 2.3.5 Mass Calibration
 2.3.6 Vacuum Systems

3 Evaluation of GC-MS Analyses

3.1 Display of Chromatograms
 3.1.1 Total Ion Current Chromatograms
 3.1.2 Mass Chromatograms
3.2 Substance Identification
 3.2.1 Extraction of Mass Spectra
  3.2.1.1 Manual Spectrum Subtraction
  3.2.1.2 Deconvolution of Mass Spectra
 3.2.2 The Retention Index
 3.2.3 Libraries of Mass Spectra
  3.2.3.1 Universal Mass Spectral Libraries
  3.2.3.2 Application Libraries of Mass Spectra
 3.2.4 Library Search Programs
  3.2.4.1 The NIST Search Procedure
  3.2.4.2 The PBM Search Procedure
  3.2.4.3 The SISCOM Procedure
 3.2.5 Interpretation of Mass Spectra
  3.2.5.1 Isotope Patterns
  3.2.5.2 Fragmentation and Rearrangement Reactions
  3.2.5.3 DMOX Derivatives for Location of Double Bond Positions
 3.2.6 Mass Spectroscopic Features of Selected Substance Classes
  3.2.6.1 Volatile Halogenated Hydrocarbons
  3.2.6.2 Benzene/Toluene/Ethylbenzene/Xylenes (BTEX, Alkylaromatics)
  3.2.6.3 Polyaromatic Hydrocarbons (PAHs)
  3.2.6.4 Phenols
  3.2.6.5 Pesticides
  3.2.6.6 Polychlorinated Biphenyls (PCBs)
  3.2.6.7 Polychlorinated Dioxins/Furans (PCDDs/PCDFs)
  3.2.6.8 Drugs
  3.2.6.9 Explosives
  3.2.6.10 ChemicalWarfare Agents
  3.2.6.11 Brominated Flame Retardants (BFR)
3.3 Quantitation
 3.3.1 Acquisition Rate
 3.3.2 Decision Limit
 3.3.3 Limit of Detection
 3.3.4 Limit of Quantitation
 3.3.5 Sensitivity
 3.3.6 The Calibration Function
 3.3.7 Quantitation and Standardization
  3.3.7.1 External Standardization
  3.3.7.2 Internal Standardization
  3.3.7.3 The Standard Addition Procedure
 3.3.8 The Accuracy of Analytical Data
3.4 Frequently Occurring Impurities

4 Applications
4.1 Air Analysis According to EPA Method TO-14
4.2 BTEX in Surface Water as of EPA Method 8260
4.3 Analysis of Additives in Edible Oils
4.4 Analysis of Alcohols in Biological Matrices
4.5 Aroma Analysis in Flavoured Mineral Water
4.6 Analysis of Aromatic Amines in Azo Dyes
4.7 Analysis of Pesticide Residues in Fruits and Vegetables
4.8 Analysis of Pesticides in Drinking Water
4.9 Analysis of Brominated Flame Retardants in Dust
4.10 Analysis of Brominated Flame Retardants in Plastic Materials
4.11 Analysis of Residual Solvents in Pharmaceutical Products
4.12 Analysis of Chlorinated Paraffins
4.13 Determination of Chloropropanols in Hydrolyzed Vegetable Protein
4.14 Identification of Chemical Warfare Agents
4.15 Analysis of Decomposition Products in Waste Oil
4.16 Determination of Odour Compounds in Olive Oil
4.17 Determination of Organotin Compounds
4.18 Analysis of Phthalates in Toys
4.19 Analysis of Phenols in Water
4.20 Analysis of Plasticizers in Paperboard Packaging
4.21 Identification of Products of Pyrolysis
4.22 Analysis of Pyrazines in Coffee
4.23 Determination of Residual Solvents According to Ph. Eur. 10.0
4.24 Analysis of Residual Solvents in Packaging Materials
4.25 Determination of Steroid Hormones in Water
4.26 Determination of Sulphur Compounds in Natural Gas
4.27 Determination of Terpenes in Herbal Preparations
4.28 Determination of VOCs in Paints and Coatings
4.29 Determination of VOCs in Soil
4.30 Determination of VOCs in Water
4.31 Characterization of Volatile Compounds in Cheese
4.32 Analysis of Volatile Organic Compounds in Mineral Oil Products
4.33 Determination of VOCs in Pharmaceuticals
4.34 Fragrance Profiling of Perfumes
4.35 Determination of Off-Flavours in Beverages
4.36 Investigation of Odour Complaints in the Environment
4.37 Investigation of Flavour Compounds in Wine
4.38 Identification of Unknown Substances in Complex Mixtures

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