Open Tubular Column Gas Chromatography in Environmental Sciences

One: Introduction.- 1.1. Organic Contaminants in the Environment.- 1.2. Advances of Trace Organic Analysis.- 1.2.1. Separation Methods.- 1.2.2. Historical Development of WCOT Column Gas Chromatography.- 1.3. Nomenclature and Relationships in Gas Chromatography.- 1.4. Separation Number (Trennzahl).- 1.4.1. Required Column Parameters.- 1.4.2. Minimum Analysis Time.- 1.4.3. Column Length.- 1.5. Thermodynamic Concept of Polarity and Selectivity.- 1.5.1. Polarity.- 1.5.2. Selectivity.- 1.6. Stationary Phases.- References.- Two: Glass WCOT Columns.- 2.1. Glass Surfaces as Support Materials.- 2.1.1. Fused Silica.- 2.1.2. Soft Glasses.- 2.1.3. Borosilicate Glass.- 2.2. Glass Surface Properties.- 2.3. Dehydration and Rehydration of Glass Surfaces.- 2.4. Capillary Tubing Fabrication.- 2.5. WCOT Column Surface Modifications.- 2.5.1. General Considerations.- 2.5.2. Surface-Roughening Techniques.- 2.5.3. HCl-Induced Crystallization in Gaseous Phase.- 2.5.4. Pyrex Glass Surface Modification.- 2.5.5. Deposition of Barium Carbonate.- 2.5.6. Other Roughening Methods.- 2.6. Glass Surface Deactivation and Chemical Modification.- 2.7. Coating the WCOT Column.- 2.7.1. Dynamic Methods.- 2.7.2. Static Techniques.- 2.8. WCOT Column Conditioning.- 2.9. Glass WCOT Column Maintenance.- References.- Three: Inlet Systems.- 3.1. General Considerations.- 3.2. Sample Introduction Techniques.- 3.2.1. Cold Syringe Needle Injection.- 3.2.2. Filled Syringe Needle Injection.- 3.2.3. Air Plug Method.- 3.2.4. Hot Syringe Needle Injection.- 3.2.5. Solvent Flush Technique.- 3.3. Split Sampling Technique.- 3.4. Splitless Sampling Technique.- 3.5. On-Column Injection Techniques.- 3.6. Direct Injection.- 3.7. Column-Switching Techniques.- 3.7.1. Splitless Injection.- 3.7.2. The Back-Flushing Method.- 3.7.3. Preseparation with Packed-Column and Intermediate-Peak Trapping.- 3.7.4. Preseparation with Packed-Column, Dual Injection, and Intermediate-Peak Trapping.- 3.8. Flow Programming in WCOT Column Gas Chromatography.- References.- Four: Detectors.- 4.1. Flame Ionization Detector.- 4.1.1. Optimization of the FID.- 4.1.2. Detector Maintenance.- 4.2. Electron Capture Detector.- 4.2.1. Principles and Operation of the ECD.- 4.2.2. Contamination of the ECD.- 4.2.3. Response Factors.- 4.2.4. Troubleshooting Electron Capture Detectors.- 4.2.5. Cleaning Electron Capture Detectors.- 4.3. Thermionic (Alkali Flame Ionization) Detector.- 4.3.1. Mechanism of Selectivity of a TED Detector.- 4.3.2. Phosphorus Mode.- 4.3.3. Selectivity and Response of TED.- 4.4. Photoionization Detector.- 4.5. The Mass Spectrometer as Detector.- 4.5.1. The Mass Spectrometer.- 4.5.2. Requirements for an Optimal GC/MS Combination.- 4.5.3. Requirements for the Mass Spectrometer.- 4.5.4. Vacuum Technology.- 4.5.5. Ion Source Optics.- 4.5.6. Scanning Time.- 4.5.7. Repetitive Scan.- 4.5.8. Selected Ion Monitoring.- 4.5.9. Computer Compatibility.- 4.6. Operational Modes of an Ion Source.- 4.6.1. Electron Impact Ionization.- 4.6.2. Chemical Ionization.- 4.6.3. Field Ionization.- 4.6.4. Field Desorption.- 4.6.5. Atmospheric Pressure Ionization.- 4.6.6. Tandem Mass Spectrometry (MS/MS) and GC/MS/MS.- 4.7. GC/MS Interface.- 4.7.1. Open Split.- 4.7.2. Direct Coupling.- 4.8. Parameters Affecting Performance of GC/MS System.- References.- Five: Sample Preparation.- 5.1. General Considerations.- 5.2. Planning the Analytical Study.- 5.2.1. Sampling.- 5.2.2. Extraction Procedures.- 5.3. Cleanup Procedures.- 5.3.1. Solvents and Reagent Purity.- 5.3.2. Quality of Adsorbents.- 5.3.3. Group Selective Adsorbents.- 5.3.4. Open-Pore Polyurethane.- 5.4. Liquid-Liquid Extraction.- 5.5. Liquid Chromatography.- 5.6. Headspace Analysis.- 5.6.1. Closed-Loop Stripping Techniques.- 5.6.2. Preconcentration of Contaminants Using Automatic Purge and Trap Devices.- 5.7. Thermal Desorption Methods.- 5.8. Steam Distillation.- 5.9. Partitioning Methods.- 5.10. Miscellaneous Methods.- 5.11. Air Sampling.- 5.12. Source Sampling Procedures.- References.- Six: The Retention Index System.- 6.1. Introduction.- 6.2. Kovats Retention Index System.- 6.2.1. Calculation and Precision.- 6.2.2. Effects of Temperature.- 6.3. Compound Identification by Retention Index.- 6.4. Other Retention Systems.- References.- Seven: Quantitative Analysis.- 7.1. General Considerations.- 7.1.1. Peak Height Measurements.- 7.1.2. Peak Area Measurements.- 7.1.3. Digital Integrators.- 7.1.4. Microcomputers.- 7.2. Principles of Quantitative Analysis.- 7.2.1. Normalization.- 7.2.2. External Standardization.- 7.2.3. Internal Standardization.- 7.2.4. Standard Addition.- 7.3. Statistical Considerations.- 7.3.1. Mean Value.- 7.3.2. Standard Deviation.- 7.3.3. Precision and Accuracy.- 7.3.4. Establishing Control Limits.- 7.4. Primary Standards in Air Pollution Analysis.- References.- Eight: Application in Environmental Analysis.- 8.1. Introduction.- 8.2. Analysis of Organic Priority Pollutants in Water.- 8.2.1. Nonvolatile Pollutants.- 8.2.2. Base-Neutral Extraction.- 8.2.3. Acid-Extractable Priority Pollutants.- 8.2.4. Pesticides.- 8.3. Determination of Groups of Compounds.- 8.4. Polycyclic Aromatic Hydrocarbons.- 8.4.1. General Considerations.- 8.4.2. Sampling Requirements.- 8.4.3. High-Resolution WCOT Column Gas Chromatography.- 8.4.4. Detection Systems.- 8.4.5. Quantitative Analysis.- 8.4.6. Qualitative Analysis.- 8.5. Heterocyclic Aromatic Hydrocarbons.- 8.5.1. Nitrogen-Containing PAH (Azaarenes).- 8.5.2. Polycyclic Aromatic Amines (PAA).- 8.5.3. Nitro Polycyclic Aromatic Hydrocarbons.- 8.5.4. Sulfur-containing Polycyclic Aromatic Hydrocarbons.- 8.6. Halogenated Aliphatic Hydrocarbons.- 8.6.1. Halogenated Alkanes and Alkenes.- 8.6.2. Chlorinated Dimethanonaphthalenes and Methanoindene Pesticides.- 8.6.3. Analysis for Mirex and Kepone.- 8.7. Halogenated Aromatic Hydrocarbons.- 8.7.1. Chlorinated Benzenes.- 8.7.2. Polychlorinated and Polybrominated Biphenyls and Terphenyls.- 8.7.3. Polybrominated Biphenyls.- 8.7.4. Polychlorinated Terphenyls.- 8.8. Polychlorinated Dibenzo-1,4-Dioxins.- 8.8.1. Sample Preparation.- 8.8.2. Qualitative PCDD Analysis.- 8.8.3. Quantitative PCDD Analysis.- 8.8.4. Application of WCOT Columns in PCDD Analysis.- 8.9. Chlorinated Dibenzofurans.- 8.10. Chlorinated Phenols and Related Compounds.- 8.10.1. Sample Preparation.- 8.10.2. Extraction and Cleanup Procedures.- 8.10.3. Derivatization of Phenols.- 8.10.4. Qualitative and Quantitative Applications of WCOT Columns.- 8.11. Toxaphene.- 8.11.1. Sample Preparation and Cleanup.- 8.11.2. WCOT Column Gas Chromatography for Toxaphene.- 8.11.3. Quantitative Analysis of Toxaphene.- 8.11.4. Toxaphene Analysis.- 8.12. Phthalate Esters.- 8.12.1. Qualitative Analysis.- 8.12.2. Sample Preparation and Cleanup.- 8.13. Nitrosamines.- 8.13.1. Detection Systems.- 8.13.2. Applications.- 8.14. Nonionic Detergents.- 8.14.1. Extraction Procedures.- 8.14.2. Qualitative and Quantitative Analysis.- 8.15. Miscellaneous Separations.- 8.15.1. Separation of s-Triazines and Substituted Urea Herbicides.- 8.15.2. Volatile Chelates of Metal Ions.- 8.15.3. Odorous Compounds in Water, Fish, and Food.- 8.15.4. Fatty Acids.- References.