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Analytical Gas Chromatography WALTER JENNINGS Department of Food Science and Technology University of California Davis, California ACADEMIC PRESS, INC
In gas chromatography this equilibrium is ... electrons cause ionisation of the carrier gas nitrogen. This creates a current between two electrode plates
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Gas Chromatography A Practical Approach Edited by P. J. BAUGH Department of Chemistry and Applied Chemistry University of Salford The Crescent, Salford
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OXFORD UNIVERSITY PRESS Oxford New York Tokyo
Contents List of contributors Abbreviations 1. Introduction to the theory of Chromatographie separations with reference to gas chromatography Keith D. Bartle 1. Introduction and history of GC
1
2. The GC chromatogram
4
3. Resolution in GC
5
4. Band broadening in GC
6
5. GC columns
7
6. Speed of GC analysis
8
7. Retention in GC Effect of temperature Temperature programming Dependence of retention on solute properties in GC Retention indices
10 10 10 12 12
References
13
2. Gas chromatography instrumentation, Operation, and experimental considerations
15
Andrew Tipler 1. Introduction
15
2. Instrumental components and funetion Fundamental components The Chromatographie oven Pneumatics Sample introduction Gas Chromatographie detectors
15 15 16 17 20 31
3. Operation and experimental considerations Where to Start
38 39
Contents Installation and preparation of the Chromatograph Chromatographie method development
39 49
4. Data handling Introduction Potential information from chromatography Detector signal processing Approaches to data handling Microprocessor-based data handling Systems
61 61 61 61 63 63
References
70
3. Development, technology, and utilization of capillary columns for gas chromatography
71
Peter A. Dawes 1. Introduction
71
2. Types of capillary column
72
3. Evolution of the modern capillary column Column support material Stationary phase criteria and development Types of stationary phase for partitioning Manufacturing methods
72 73 73 75 78
4. Column Performance evaluation Resolving power Determination of efficiency and Performance parameters Kövats' retention index Speed of analysis Sample capacity Inertness Bleed
80 81 81 84 84 85 86 90
5. Column selection Stationary phase Internal diameter Film thickness Length
93 94 95 97 98
6. Care of a capillary column Protection of fused silica fabric and installation hints Column contamination Column Operation
98 99 99 101
References
102 x
Contents
4. Applications of packed and capillary GC Peter J.
103
Baugh
1. I n t r o d u c t i o n
103
2. E x p e r i m e n t a l c o n s i d e r a t i o n s Column requirements
104 104
3. M u l t i d i m e n s i o n a l gas c h r o m a t o g r a p h y Capillary-capillary column coupling with differing film thickness of SP Capillary-capillary column coupling with consecutive non-polar and polar SPs Capillary column and FID/ECD as dual detectors Packed-capillary coupling
106 107 107 109 109
4. A p p l i c a t i o n s of p a c k e d a n d c a p i l l a r y c o l u m n s Specific applications for packed columns Comparison of applications of packed and capillary columns Applications of wide-bore capillary columns
109 110 111 115
5. H i g h - t e m p e r a t u r e GC (HTGC) a n d a n a l y s i s of h i g h m o l e c u l a r w e i g h t l o w volatile a n a l y t e s Analysis of polyaromatic hydrocarbons Analysis of triglycerides Analysis of porphyrins Other analytes
121 123 124 125 126
6. Gas—solid c h r o m a t o g r a p h y (GSC) a n d gas—liquid c h r o m a t o g r a p h y (GLC) for t h e a n a l y s i s of h i g h l y volatile organics (HVOs) GSC using packed columns GSC using capillary columns GLC using thick film capillary columns
127 127 128 129
7. C o n c l u s i o n s
131
References
131
5. Chemical derivatization in gas chromatography David G.
133
Watson
1. I n t r o d u c t i o n
133
2. A p p a r a t u s Sample Containers and reaction vessels Hearing and evaporation Sample and reagent handling Removal of derivatizing reagents
134 134 135 135 136
3. S t a n d a r d p r o c e d u r e s i n d e r i v a t i z a t i o n
136
xi
Contents 4. Derivatization reactions involving one reagent Silylation reactions Acylation reactions Alkylation reactions Condensation reactions Derivatives of miscellaneous types
137 137 141 145 150 152
5. Mixed derivatives Silyl-acyl and silyl-carbamate derivatives Acyl/acyl derivatives Acyl/alkyl derivatives Acyl/amide derivatives Silyl/alkyl oxime and acyl/oxime derivatives Derivatization procedures for Prostaglandins
154 154 156 157 158 159 161
6. Bifunctional and mixed bifunctional monofunctional derivatives Bifunctional silylating agents Aldehydes and ketones as bifunctional derivatizing agents Alkyl boronates as bifunctional derivatizing agents
162 163 163 164
7. Derivatives used for Separation of enantiomers Acylation with chiral reagents Chiral alkylating reagents Formation of diastereomeric amides
166 166 168 168
References
169
6. Gas chromatography in analytical toxicology: principles and practice
m
Robert J. Flanagan 1. Introduction
171
2. Use of GC in analytical toxicology Sample collection and storage Sample preparation Columns and column packings Detectors General considerations
172 172 173 181 186 188
3. Applications of GC in analytical toxicology Screening for unknowns Drugs Pesticides Gases, solvents, and other poisons
192 193 194 200 202
4. Conclusions
206
Acknowledgements
208
References
208 xii
Contents
Gas chromatography in clinical chemistry
213
Jagadish Chakraborty 1. Introduction
213
2. Applications of GC Organic volatiles Organic acids Cholesterol and related Compounds Amines and related Compounds Polyols and sugars
214 214 219 226 229 232
3. Conclusions
235
References
235
Chiral separations by gas chromatography
237
David R. Taylor 1. Introduction Terminology and definitions
237 238
2. Role of derivatization in chiral separations by GC Typical protocols for diastereoisomeric derivatization
240 243
3. GC on chiral stationary phases (CSP) Phases based on monomeric peptides Phases based on polymeric amides Chiral GC using metal complexation Inclusion phases for chiral GC
245 247 252 260 269
4. Applications of chiral stationary phases in GC
277
5. Conclusions and future prospects
278
References
278
Environmental analysis using gas chromatography
283
Gerry A. Best and J. Paul Dawson 1. Introduction Pathways to the environment Instrumentation
283 283 285
2. The need for GC analysis of environmental samples Pollution problems Statutory regulations
285 285 285
3. Analytical quality control of GC data
286
4. Isolation of target Compounds from the sample matrix
289
xiii
Contents Contamination Procedure for the extraction of organochlorine Compounds and PCBs from water Procedure for the extraction of organochlorine Compounds from samples of effluent Extraction of organochlorine Compounds from Sediment samples Extraction of organochlorine Compounds from tissue samples
290
5. Clean-up procedures Clean-up and Separation of extracts using alumina and silica columns Modified method for clean-up and Separation using alumina/ silica nitrate and silica gel Clean-up and Separation of extracts using solid-phase extraction (SPE) cartridges Extraction of semi-volatile Compounds from water samples using extraction discs
297
6. Analysis of pentachlorophenol
306
7. Determination of non-persistent pesticides present in water samples Extraction and determination of organophosporus and organonitrogen Compounds in water Extraction and clean-up of permethrin from water samples Extraction and determination of phenoxyacetic acid type of herbicides
291 293 295 297
298 300 303 304
307 308 310 311
8. GC Separation and quantification of target Compounds Choice of column Calculation of concentration in samples using the internal Standard method Typical GC chromatograms for target Compound analysis
313 313 315 315
9. Sampling and analysis of gases and vapours Sampling Desorption of components
316 316 322
10. Determination of types of oil in pollution samples Oil fingerprinting Oil fingerprinting—GC operating conditions
323 323 326
References
327
10. The role of gas chromatography in petroleum exploration
331
Gareth E. Harriman 1. Introduction
331
2. Composition of crude oils and source rock extracts
332
XIV
Contents 3. Whole oil GC
333
4. GC analysis of fractions isolated from crude oils and source rock extracts
337
5. GC-MS analysis of fractions isolated from crude oils and source rock extracts
343
6. Conclusions
354
References
356
11. Combined gas chromatography-mass spectrometry
359
Richard P. Evershed 1. General considerations
359
2. GC-MS Instrumentation Use of packed columns Use of capillary columns Ion sources Use of different mass analysers Ion detection Data collection and interpretation
360 360 360 362 364 367 368
3. Applications Mixture analysis Trace analysis
368 368 381
References
390
Appendices AI Combined gas chromatography—Fourier transform infrared spectroscopy 393 Peter Jackson 1. Introduction
