دانلود کتاب Organic Trace Analysis

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Cover
Half Title
Also of interest
Organic Trace Analysis
Copyright
Preface
Contents
1. Overview
1.1 General Remarks
1.2 What Does “Organic Traces” Mean?
1.3 Importance of Organic Trace Analysis
1.4 Peculiarities with Organic Trace Analysis
1.5 Essential Matrices in Organic Trace Analysis
1.6 Aims of Organic Trace Analysis
Further Reading
Bibliography
2. Statistical Evaluation
2.1 General Remarks
2.2 Calibration Function
2.3 Sensitivity
2.4 Types of Error
2.5 Limit of Detection/Limit of Quantification
2.6 Precision
2.7 Accuracy
2.8 Correlation and regression
Further Reading
3. Quality Control Strategies
3.1 General Remarks
3.2 Artificially Generated Matrix Surrogates
3.3 Addition of an Internal Standard
3.4 Validation by Applying Independent Analytical Methods
3.5 Validation by Reference Material
3.6 QC by Applying Good Laboratory Practices
Further Reading
Bibliography
4. Sampling of Organic Trace Contaminants
4.1 General Remarks
4.2 Sampling from Organisms
4.2.1 General Remarks
4.2.2 Animal Tissue Samples
4.2.2.1 Aquatic Organisms
4.2.2.2 Terrestrial and Aerial Organisms
4.2.3 Human Samples
4.2.3.1 Hair
4.2.3.2 Blood and Plasma
4.2.3.3 Urine
4.2.4 Plant Sampling
4.3 Trace Gas Sampling
4.3.1 General Remarks
4.3.2 Gas Grab Sampling
4.4 Rain, Surface Water and Particulate Matter Sampling
4.4.1 General Remarks
4.4.2 Rain
4.4.3 Surface Water, Deep Water, Groundwater
4.4.4 Particulate Matter Sampling
4.5 Soil and Sediment Sampling
4.5.1 General Remarks
4.5.2 Soil
4.5.3 Sediment
4.6 Diffusion Sampling (Passive Sampling)
4.7 Sampling of Colloidal Matter (Hydrosol, Aerosol)
4.7.1 General Remarks
4.7.2 Hydrosol Sampling
4.7.3 Aerosol Sampling
4.8 Sources for Artifact Formation
4.8.1 General Remarks
4.8.2 Sources of Artifacts
Further Reading
Bibliography
5. Sample Treatment Before Analysis
5.1 General Remarks
5.2 Sample Pretreatment (Stabilization and Storage)
Bibliography
6. Enrichment and Sample Cleanup
6.1 General Remarks
6.2 Liquid Samples (Water, Body Fluids, Beverages)
6.2.1 Liquid–Liquid Extraction
6.2.2 Pre-concentration after LLE (Evaporation, Freeze-Drying)
6.2.3 Solid-phase Extraction
6.2.4 Solid-phase Microextraction
6.2.5 Dispersive liquid–liquid microextraction
6.2.6 Micellar Extraction
6.2.7 Headspace Extraction
6.2.8 Purge and Trap Extraction
6.3 Solid Samples (Particulate Matter, Soil, Sediment, Plant and Animal Material)
6.3.1 Solid–Liquid Extraction
6.3.1.1 Bioavailable Concentrations
6.3.1.2 Exhaustive Extractions to Release Bioavailable and Inert (“Not Biovailable\") Pollutants
6.3.1.3 QuEChERS Method
6.3.2 Assisted Solid–Liquid Extraction (Soxhlet, ASE, Microwave Extraction, Ultrasonication, Supercritical Fluid Extraction)
6.3.2.1 Soxhlet Extraction
6.3.2.2 Accelerated solvent extraction, Pressurized Solvent Extraction
6.3.2.3 Supercritical Fluid Extraction
6.3.2.4 Ultrasound-Assisted Extraction
6.3.2.5 Microwave-Assisted Extraction
6.3.3 Enzymatic Digestion
6.3.4 Non-extractable Residues
6.3.5 Steam Distillation
6.3.6 Size Fractionation of Dispersed Solid Matter
6.4 Gaseous Samples and Aerosols
6.4.1 General Remarks
6.4.2 Liquid Absorption of Trace Gases
6.4.3 Solid Adsorption of Trace Gases
6.4.4 Filtration
6.4.5 Diffusion Sampling (Denuder Sampling)
6.4.6 Sampling by Condensation
6.4.7 Size-Resolved Particle (Aerosol) Sampling
Further Reading
Bibliography
7. Chromatography
7.1 General Remarks
7.2 Chromatographic Separation
7.2.1 Adsorption Chromatography
7.2.2 Ion-Exchange Chromatography
7.2.3 Size-Exclusion Chromatography
7.3 Basics and Working Principles
7.3.1 Parameters to Achieve Best Resolving Power
7.3.2 General Recommendations
7.4 High-Performance Liquid Chromatography
7.4.1 General Information
7.4.2 Mobile Phase (HPLC)
7.4.2.1 Polarity of HPLC Solvents
7.4.2.2 HPLC Solvent Selection
7.4.2.3 Isocratic and Gradient Elution
7.4.2.4 HPLC Pumping Systems
7.4.2.5 Sample Injection (HPLC)
7.4.3 Stationary-Phase Materials
7.4.3.1 Normal-Phase Matrices
7.4.3.2 Reversed-Phase Matrices
7.4.3.3 Ion-Exchange Matrices
7.4.3.4 Size-Exclusion (SEC) Matrices
7.4.3.5 Affinity Matrices
7.4.4 Columns
7.4.5 HPLC Detectors
7.4.5.1 UV–Vis Absorption Detectors
7.4.5.2 MS Detector
7.4.5.3 Refractive Index Detector
7.4.5.4 Fluorescence Detector in HPLC
7.4.5.5 Evaporative Light-Scattering Detector
7.4.5.6 Conductivity Detector
7.4.5.7 Electrochemical Detector
7.4.6 Separation Parameters in HPLC
7.4.6.1 Resolution
7.4.6.2 HPLC Column Dimensions
7.4.6.3 Particle Size and Pore Size
7.4.7 Derivatization Methods (Pre-Column, Post-Column) in HPLC
7.4.8 Hyphenated Techniques (HPLC–MS, HPLC-NMR)
7.4.8.1 HPLC–MS
7.4.8.2 HPLC-NMR
7.5 Gas chromatography
7.5.1 General Remarks
7.5.2 Separation Columns and Stationary Phases (GC)
7.5.3 Mobile Phase
7.5.4 Isothermal versus Temperature-Programmed GC
7.5.5 Injection Techniques for GC
7.5.6 GC Separations at Extreme Temperatures
7.5.7 Derivatization Techniques in GC
7.5.8 Change of State During GC Separation (Pyrolysis, Carbon Skeleto
7.5.9 Analyte Detection in GC (Electrical, Electrochemical, Optical)
7.5.9.1 General Requirements
7.5.9.2 Most Common GC Detectors
7.5.9.3 Dedicated GC Detectors
7.5.10 Hyphenated Techniques (GC–MS)
7.5.10.1 General Remarks
7.5.10.2 GC–MS Interfaces
7.5.11 Multidimensional GC Separations (GC
7.5.11.1 General Remarks
7.5.11.2 GC–GC Multidimensional Separation by Heart-Cut
7.5.11.3 GC x GC Comprehensive Multidimensional Separation by Modulation
Further Reading
Bibliography
8. Capillary Electrophoresis (CE)
8.1 General Remarks
8.2 Working Principles
8.2.1 Interaction of Charged Analyte Species with an External Electric Field
8.2.2 Electroendosmotic Flow
8.2.3 Control of EOF
8.2.4 Flow Dynamics, Efficiency and Resolution
8.3 Modes of CE Operation
8.3.1 CZE
8.3.2 Capillary Gel Electrophoresis
8.3.3 Micellar Electrokinetic Capillary Chromatography
8.3.4 Capillary Isoelectric Focusing
8.3.5 Capillary Isotachophoresis
8.4 Sample Injection (CE)
8.4.1 Hydrodynamic Injection
8.4.2 Electrokinetic Injection
8.5 Separation Parameters in CE
8.5.1 Capillary Properties and Conditioning
8.5.2 Temperature Effect in CE
8.5.3 Electric Field in CE
8.6 Detection of Analytes in CE
8.6.1 UV–Vis Detection in CE
8.6.2 Fluorescence and Chemiluminescence Detection in CE
8.6.3 Amperometric and Conductometric Detection in CE
8.6.4 Hyphenated Techniques (CE-MS)
8.6.5 Indirect Detection Methods in CE
8.6.6 Increasing the Sensitivity of Detection in CE
Further Reading
Bibliography
9. Mass Spectrometry
9.1 Introduction
9.2 Basic Equipment
9.3 Ionization in MS
9.3.1 Hard Ionization by Electron Impact
9.3.2 Soft Ionization
9.4 Separation of m/z Species
9.4.1 One-Dimensional Mass Separation
9.4.2 Two-Dimensional Mass Separation
9.4.3 Three-Dimensional Mass Separation by Ion Trap MS
9.5 Molecular Imaging by MS
Further Reading
Bibliography
10. Receptor-based Bioanalysis for Mass Screening
10.1 General Remarks
10.2 Natural Receptors (Enzymes and Antibodies)
10.3 Working Principle of Enzymes (Enzymatic Catalysis, Enzymatic Inhibition)
10.4 Working Principle of Antibodies (IA, Test Format, Microarray, Dip Stick)
10.5 Principles of Effect-Directed Analysis
Further Reading
Bibliography
11. Selected Applications
11.1 Trace Analysis of Polycyclic Aromatic Hydrocarbons (PAHs)
11.1.1 General Remarks (Occurrence, Physical and Chemical Properties)
11.1.2 Sampling Strategies for PAHs (Water, Air, Soil, Body Fluids)
11.1.2.1 Water
11.1.2.2 Air (Ambient Air; Combustion Aerosol)
11.1.2.3 PAHs in Soil
11.1.2.4 PAHs in Body Fluids
11.1.3 Wet-chemical Analysis (HPLC, Thin-layer Chromatography)
11.1.3.1 HPLC Analysis of PAHs
11.1.3.2 Thin-layer Chromatography of PAHs
11.1.4 GC Analysis of PAH
11.1.5 Immunological Bioanalysis of PAHs
11.1.5.1 Soil
11.1.5.2 Water
11.1.6 In situ PAH Analysis by Spectroscopic Techniques (Laser Fluorescence, Photoelectron Emission)
11.1.6.1 Time-resolved Laser Fluorescence PAH Sensor
11.1.6.2 PAH Monitoring in Ambient Aerosol by Photoelectric Aerosol Charging
11.2 Polychlorinated Biphenyls, Dibenzodioxins and -Furans
11.2.1 General Remarks on Occurrence and Importance
11.2.1.1 PCBs
11.2.1.2 Polychlorinated dibenzodioxins and –furans
11.2.2 Sampling Strategies for Polyhalogenated Aromatic Hydrocarbons
11.2.3 GC Analysis of PCDDs/PCDFs and PCBs
11.2.3.1 GC-ECD
11.2.3.2 GC x GC-ECD
11.2.3.3 GC/MS
11.2.4 Bioanalytical Methods for PCDD/PCDF and PCB Screening
11.2.4.1 CALUX
11.2.4.2 Immunoassay (IA) for PCDD/PCDF Analysis
11.2.4.3 Immunoassay (IA) for PCB Sum Analysis
11.3 Organophosphorus Compounds
11.3.1 General Remarks on Occurrence and Importance
11.3.2 Sampling Strategies for OPs (Water, Soil, Air, Body Fluid, Food and Nutraceuticals, Living Tissue)
11.3.2.1 Water
11.3.2.2 Plants and Food
11.3.2.3 OPs in Soil
11.3.2.4 OPs in Animal and Human Tissues
11.3.2.5 Air
11.3.3 GC Analysis of OPs
11.3.4 Wet-chemical Analysis of OPs (HPLC–MS, TLC, Capillary Electrophoresis)
11.3.4.1 HPLC for OP Analysis
11.3.4.2 TLC for OP Analysis
11.3.4.3 Capillary Electrophoresis for OP Analysis
11.3.5 Bioanalysis of OPs
11.3.5.1 Detection in Biosensing of OPs
11.3.5.2 Enzymatic Assays for Analysis of OPs
11.3.5.3 Immunoassays for Analysis of OPs
11.3.5.4 Whole Cell Bioassays
Further Reading: Polycyclic Aromatic Hydrocarbons
Further Reading: Polychlorinated Biphenyls (PCBs), Dibenzodioxins (PCDDs) and –Furans (PCDFs)
Further Reading: Organophosphates
Bibliography
List of Abbreviations
Index