Static Headspace-Gas Chromatography

Name: Static Headspace-Gas Chromatography | Theory and Practice
Brand: Wiley
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Theory and Practice

Bruno Kolb Leslie S. Ettre(Autor*in)

Wiley (Verlag)

2. Auflage

Erschienen am 24. Juli 2006

376 Seiten

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978-0-471-91456-3 (ISBN)

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Inhalt

Cover
Title Page
Copyright Page
Contents
Preface
Preface to the First Edition
List of Acronyms and Symbols
Chapter 1 General Introduction
1.1 Principles of Headspace Analysis
1.2 Types of Headspace Analysis
1.2.1 Principles of Static HS-GC
1.2.2 Principles of Dynamic HS-GC
1.2.2.1 The Trap
1.2.2.2 The Water Problem
1.2.2.3 The Flow Problem
1.2.2.4 The Time Problem
1.2.2.5 Comparison of Static HS-GC with P&T
1.3 The Evolution of the HS-GC Methods
1.4 HS-GS Literature
1.5 Regulatory Methods Utilizing (Static) HS-GC
References
Chapter 2 Theoretical Background of HS-GC and Its Applications
2.1 Basic Theory of Headspace Analysis
2.2 Basic Physicochemical Relationships
2.3 Headspace Sensitivity
2.3.1 Influence of Temperature on Vapor Pressure and Partition Coefficient
2.3.1.1 Enhancement of Lower Boiling Compounds
2.3.2 Influence of Temperature on Headspace Sensitivity for Compounds with Differing Partition Coefficients
2.3.3 Influence of Sample Volume on Headspace Sensitivity for Compounds with Differing Partition Coefficients
2.3.3.1 Sample-to-Sample Reproducibility
2.3.4 Changing the Sample Matrix by Varying the Activity Coefficient
2.4 Headspace Linearity
2.5 Duplicate Analyses
2.6 Multiple Headspace Extraction (MHE)
2.6.1 Principles of MHE
2.6.2 Theoretical Background of MHE
2.6.3 Simplified MHE Calculation
References
Chapter 3 The Technique of HS-GC
3.1 Sample Vials
3.1.1 Vial Types
3.1.2 Selection of the Vial Volume
3.1.3 Vial Cleaning
3.1.4 Wall Adsorption Effects
3.2 Caps
3.2.1 Pressure on Caps
3.2.2 Safety Closures
3.3 Septa
3.3.1 Septa Types
3.3.2 Septum Blank
3.3.3 Should a Septum Be Pierced Twice?
3.3.3.1 Closed-Vial versus Open-Vial Sample Introduction Technique
3.4 Thermostatting
3.4.1 Influence of Temperature
3.4.2 Working Modes
3.5 The Fundamental Principles of Headspace Sampling Systems
3.5.1 Systems Using Gas Syringes
3.5.2 Solid Phase Microextraction (SPME)
3.5.2.1 Comparison of the Sensitivities in HS-SPME and Direct Static HS-GC
3.5.3 Balanced Pressure Sampling Systems
3.5.4 Pressure/Loop Systems
3.5.5 Conditions for Pressurization Systems
3.5.6 Volume of the Headspace Gas Sample
3.5.6.1 Sample Volume with Gas Syringes
3.5.6.2 Sample Volume with Loop Systems
3.5.6.3 Sample Volume with the Balanced Pressure System
3.6 Use of Open-Tubular (Capillary) Columns
3.6.1 Properties of Open-Tubular Columns for Gas Samples
3.6.2 Headspace Sampling with Split or Splitless Introduction
3.6.3 Comparison of Split and Splitless Headspace Sampling
3.6.4 Band Broadening During Sample Introduction
3.6.5 Influence of Temperature on Band Broadening
3.6.5.1 Conclusions
3.6.6 The Combination of Different Columns and Detectors
3.7 Enrichment Techniques in HS-GC
3.7.1 Systems for Cryogenic Trapping
3.7.1.1 Trapping by Cryogenic Condensation
3.7.1.2 Trapping by Cryogenic Focusing
3.7.1.3 Influence of Temperature on Cryogenic Focusing
3.7.1.4 Comparison of the Various Techniques of Cryogenic Trapping
3.7.2 Influence of Water in Cryogenic HS-GC
3.7.2.1 Water Removal in Static HS-GC
3.7.2.2 Applications
3.7.3 Enrichment by Adsorption
3.7.3.1 Water Removal from an Adsorption Trap
3.8 Special Techniques with the Balanced Pressure Systems
3.8.1 Instrumentation for MHE
3.8.2 Backflushing
3.9 Reaction HS-GC
3.9.1 Derivatization in the Headspace Vial
3.9.1.1 Methylation
3.9.1.2 Esterification
3.9.1.3 Transesterification
3.9.1.4 Acetylation
3.9.1.5 Carbonyl Compounds
3.9.2 Subtraction HS-GC
3.9.3 Special Reactions
3.9.4 HS-GC Analysis of Volatile Derivatives from Inorganic Compounds
References
Chapter 4 Sample Handling in HS-GC
4.1 Equilibration
4.1.1 Gas Samples
4.1.2 Liquid Samples
4.1.2.1 General Properties
4.1.2.2 Reduction of the Equilibration Time for Liquid Samples
4.1.3 Solid Samples
4.2 Solution Approach
4.3 Sample Handling and Sample Introduction
4.3.1 Gas Samples
4.3.2 Liquid Samples
4.3.3 Solid Samples
4.4 Preparation of Standard Solutions
4.4.1 Preparation of a Standard Solution from a Liquid or Solid Substance
4.4.2 Preparation of a Standard Solution from a Gaseous Compound
4.5 Influence of the Matrix
4.5.1 Clean Matrix Is Available
4.5.2 Matrix Effect Can Be Eliminated
4.5.3 Artificial Matrix Can Be Prepared
4.6 Methods Aiming at Complete Evaporation of the Analyte
4.6.1 The Total Vaporization Technique (TVT)
4.6.2 The Full Evaporation Technique (FET)
4.6.3 Calculation of the Extraction Yield in FET
4.6.4 Comparison of Headspace Sensitivities
References
Chapter 5 Headspace Methods for Quantitative Analysis
5.1 Internal Normalization
5.2 Internal Standard Method
5.2.1 Blood Alcohol Determination
5.3 External Standard Method
5.4 Standard Addition Method
5.4.1 Single Addition
5.4.2 Handling of the Added Standard
5.4.3 Determination by Multiple Additions
5.5 Multiple Headspace Extraction (MHE)
5.5.1 Principles of MHE
5.5.2 Calibration in MHE
5.5.2.1 External Standard
5.5.2.2 Internal Standard
5.5.2.3 Standard Addition
5.5.3 The Use of Gaseous External Standards in MHE
5.5.3.1 Correction for Sample Volume
5.5.4 The Role of Quotient Q
5.5.4.1 Relationship between Q and Pressures
5.5.4.2 Value of Q in the Case of Total Vaporization
5.5.4.3 The Relative Position of the MHE Plots as a Function of Q
5.5.5 The Correlation Coefficient r
5.5.6 Evaluation of the Shape of the Regression Plot
5.5.7 Influence of K/ß
5.6 Analysis of Solid Samples (Adsorption Systems)
5.6.1 Suspension Approach
5.6.2 Surface-Modification Techniques
5.6.3 Highly Adsorptive Solid Samples
5.7 Calibration Techniques with Headspace Samples of Varying Volumes
5.8 Analysis of Gas Samples
References
Chapter 6 Method Development in HS-GC
6.1 General Guidelines
6.2 Determination of the Residual Monomer Content of Polystyrene Pellets
6.2.1 First Approach: Use of Internal Standard with MHE
6.2.2 Second Approach: Single Determination with Internal Standard
6.2.3 Third Approach: Use of External Standard with MHE
6.2.4 Fourth Approach: Use of the Solution Approach
6.3 Determination of Residual Solvents in a Printed Plastic Film
6.3.1 First Approach: Use of External Standard with MHE
6.3.2 Second Approach: Use of Standard Addition with MHE
6.3.3 Third Approach: Use of Internal Standard
6.3.4 Fourth Approach: Use of Standard Addition
6.4 Determination of the Volatile Constituents of a Cathodic Electrolytic Plating Bath
6.4.1 First Approach: Use of External Standard with MHE
6.4.2 Second Approach: Dilution and Use of External Standard
Chapter 7 Nonequilibrium Static Headspace Analysis
7.1 Accelerated Analysis
7.2 Heat-Sensitive Samples
References
Chapter 8 Qualitative Analysis by HS-GC
8.1 The Use of HS-GC in "Fingerprinting
8.2 The Use of Headspace Sampling in Hyphenated Systems
8.3 The Use of HS-GC in Microbiology
References
Chapter 9 Special Measurements
9.1 Determination of Vapor Pressures
9.2 Determination of Activity Coefficients
9.3 Determination of Related Physicochemical Functions
9.4 Determination of Phase Distribution (Partition Coefficient)
9.4.1 The Vapor-Phase Calibration (VPC) Method
9.4.2 The Phase Ratio Variation (PRV) Method
9.4.2.1 Principles
9.4.2.2 Limitation of the PRV Method
9.4.3 MHE Methods for the Determination of the Partition Coefficient
9.4.3.1 VPC/MHE Method
9.4.3.2 PRV/MHE Method
9.5 Reaction Constant Measurements
9.6 Determination of Solute Solubility by MHE
9.7 Gas-Solid Systems
9.7.1 Determination of Adsorption Isotherms
9.7.2 Determination of the Rate of Release of a Volatile Analyte
9.8 Validation of Headspace Instrumentation: Investigation of Detector Linearity and Detection Limit
9.8.1 Definitions
9.8.2 Linear Range of the Detector
9.8.3 Precision of the Range
9.8.4 Minimum Detectability
References
Index
EULA

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