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Tables of Contents for Static Headspace-Gas Chromatography
Chapter/Section Title
Page #
Page Count
Preface
xi
4
List of Acronyms and Symbols
xv
Chapter 1 General Introduction
1
12
1.1 Principles of Headspace Analysis
1
2
1.2 Types of Headspace Analysis
3
1
1.3 The Evolution of the HS-GC Methods
4
2
1.4 Headspace-Gas Chromatography Literature
6
1
1.5 Regulatory Methods Utilizing (Static) HS-GC
7
1
References
8
5
Chapter 2 Theoretical Background of Headspace-Gas Chromatography and Its Applications
13
32
2.1 Basic Theory of Headspace Analysis
13
3
2.2 Basic Physicochemical Relationships
16
2
2.3 Headspace Sensitivity
18
18
2.3.1 Influence of Temperature on Vapor Pressure and Partition Coefficient
20
2
2.3.2 Influence of Temperature on Headspace Sensitivity for Compounds with Differing Partition Coefficients
22
5
2.3.3 Influence of Sample Volume on Headspace Sensitivity for Compounds with Differing Partition Coefficients
27
9
2.4 Headspace Linearity
36
2
2.5 Duplicate Analyses
38
2
2.6 Multiple Headspace Extraction (MHE)
40
3
2.6.1 Principles of MHE
40
1
2.6.2 Theoretical Background of MHE
41
2
2.6.3 Simplified MHE Calculation
43
1
References
43
2
Chapter 3 The Technique of Headspace-Gas Chromatography
45
72
3.1 Sample Vials
45
4
3.1.1 Types
45
1
3.1.2 Selection of the Vial Volume
46
2
3.1.3 Vial Cleaning
48
1
3.1.4 Wall Adsorption Effects
48
1
3.2 Caps
49
3
3.2.1 Pressure on Caps
51
1
3.2.2 Safety Closures
51
1
3.3 Septa
52
7
3.3.1 Types
52
1
3.3.2 Septum Blank
53
2
3.3.3 Should a Septum Be Pierced Twice?
55
4
3.4 Thermostatting
59
5
3.4.1 Influence of Temperature
60
2
3.4.2 Working Modes
62
2
3.5 The Fundamentals of Headspace Sampling
64
15
3.5.1 Systems Using Gas Syringes
64
1
3.5.2 Balanced Pressure Sampling Systems
65
4
3.5.3 Pressure/Loop Systems
69
2
3.5.4 Conditions for Pressurization Systems
71
1
3.5.5 Use of Open-Tubular Columns
72
2
3.5.6 Volume of the Headspace Sample
74
5
3.6 Instrumentation of MHE
79
2
3.7 Backflushing
80
5
3.8 Cryogenic Sample Concentration
85
15
3.8.1 The Need for Cryogenic Sample Concentration
85
2
3.8.2 Systems for Cryogenic Trapping
87
5
3.8.3 Influence of Water in Cryogenic HS-GC
92
8
3.9 Reaction Headspace-Gas Chromatography
100
15
3.9.1 Derivatization in the Headspace Vial
100
6
3.9.2 Subtraction HS-GC
106
1
3.9.3 Special Reactions
106
6
3.9.4 HS-GC Analysis of Volatile Derivatives from Inorganic Compounds
112
3
References
115
2
Chapter 4 Sample Handling in HS-GC
117
32
4.1 Equilibration
118
8
4.1.1 Gas Samples
119
1
4.1.2 Liquid Samples
120
3
4.1.3 Solid Samples
123
3
4.2 Solution Approach
126
3
4.3 Sample Handling and Sample Introduction
129
5
4.3.1 Gas Samples
129
2
4.3.2 Liquid Samples
131
1
4.3.3 Solid Samples
132
2
4.4 Preparation of Standard Solutions
134
5
4.4.1 Preparation of a Standard Solution from a Liquid or Solid Substance
134
3
4.4.2 Preparation of a Standard Solution from a Gaseous Compound
137
2
4.5 Influence of the Matrix
139
3
4.5.1 Clean Matrix Is Available
139
1
4.5.2 Matrix Effect Can Be Eliminated
140
2
4.5.3 Artificial Matrix Can Be Prepared
142
1
4.6 Methods Aiming at the Complete Evaporation of the Analyte
142
6
4.6.1 The Total Vaporization Technique (TVT)
142
2
4.6.2 The Full Evaporation Technique (FET)
144
1
4.6.3 Calculation of the Extraction Yield in FET
145
2
4.6.4 Comparison of Headspace Sensitivities
147
1
References
148
1
Chapter 5 Headspace Methods for Quantitative Analysis
149
62
5.1 Internal Normalization
150
5
5.2 Internal Standard Method
155
4
5.3 External Standard Method
159
4
5.4 Standard Addition Method
163
11
5.4.1 Single Addition
163
4
5.4.2 Handling of the Added Standard (GPA and SPA)
167
4
5.4.3 Determination with Multiple Additions
171
3
5.5 Multiple Headspace Extraction (MHE)
174
17
5.5.1 Principles of MHE
174
1
5.5.2 Calibration in MHE
175
6
5.5.3 The Use of Gaseous Externals Standards in MHE
181
1
5.5.4 The Role of Quotient Q
182
4
5.5.5 The Correlation Coefficient r
186
1
5.5.6 Evaluation of the Shape of the Regression Plots
186
3
5.5.7 Influence of K/XXX
189
2
5.6 Analysis of Solid Samples (Adsorption Systems)
191
14
5.6.1 Suspension Approach
191
6
5.6.2 Surface Modification Techniques
197
7
5.6.3 Highly Adsorptive Samples
204
1
5.7 Calibration Techniques with Headspace Samples of Varying Volumes
205
2
5.8 Analysis of Gas Samples
207
3
References
210
1
Chapter 6 Method Development in HS-GC
211
16
6.1 General Guidelines
211
2
6.2 Determination of the Residual Monomer Content of Polystyrene Pellets
213
5
6.2.1 First Approach: Use of Internal Standard with MHE
213
3
6.2.2 Second Approach: Single Determination with Internal Standard
216
1
6.2.3 Third Approach: Use of External Standard with MHE
217
1
6.2.4 Fourth Approach: Use of the Solution Approach
218
1
6.3 Determination of Residual Solvents in a Printed Plastic Film
218
5
6.3.1 First Approach: Use of External Standard with MHE
218
2
6.3.2 Second Approach: Use of Standard Addition with MHE
220
2
6.3.3 Third Approach: Use of Internal Standard
222
1
6.3.4 Fourth Approach: Use of Standard Addition
222
1
6.4 Determination of the Volatile Constituents of a Cathodic Electrolytic Plating Bath
223
4
6.4.1 First Approach: Use of External Standard with MHE
223
1
6.4.2 Second Approach: Dilution and Use of External Standard
224
3
Chapter 7 Nonequilibrium Static Headspace Analysis
227
8
7.1 Accelerated Analysis
227
3
7.2 Heat-Sensitive Samples
230
3
References
233
2
Chapter 8 Qualitative Analysis by HS-GC
235
16
8.1 The Use of HS-GC in "Fingerprinting"
238
3
8.2 The Use of Headspace Sampling in Hyphenated Systems
241
2
8.3 The Use of HS-GC in Microbiology
243
7
References
250
1
Chapter 9 Special Measurements
251
36
9.1 Determination of Vapor Pressures
251
3
9.2 Determination of Activity Coefficients
254
2
9.3 Determination of Related Physicochemical Functions
256
4
9.4 Determination of Phase Distribution (Partition Coefficient)
260
12
9.4.1 The Vapor Phase Calibration (VPC) Method
260
4
9.4.2 The Phase Ratio Variation (PRV) Method
264
3
9.4.3 MHE Methods for the Determination of the Partition Coefficient
267
5
9.5 Reaction Constant Measurements
272
1
9.6 Gas-Solid Systems
273
5
9.6.1 Determination of Adsorption Isotherms
273
1
9.6.2 Determination of the Rate of Release of a Volatile Analyte
274
4
9.7 Validation of the Headspace Instrumentation: Investigation of Detector Linearity and Detection Limit
278
7
9.7.1 Definitions
278
2
9.7.2 Linear Range of the Detector
280
2
9.7.3 Precision of the Range
282
2
9.7.4 Minimum Detectability
284
1
References
285
2
Compound Index: Analytes, Samples, Solvents, and Reagents
287
6
Subject Index
293