Gas Chromatography and Mass Spectrometry: A Practical Guide
- 2nd Edition - March 30, 2011
- Authors: O. David Sparkman, Zelda Penton, Fulton G. Kitson
- Language: English
- Paperback ISBN:9 7 8 - 0 - 1 2 - 3 7 3 6 2 8 - 4
- eBook ISBN:9 7 8 - 0 - 0 8 - 0 9 2 0 1 5 - 3
The second edition of Gas Chromatography and Mass Spectrometry: A Practical Guide follows the highly successful first edition by F.G. Kitson, B.S. Larsen, and C.N. McEwen (1996)… Read more
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Request a sales quoteThe second edition of Gas Chromatography and Mass Spectrometry: A Practical Guide follows the highly successful first edition by F.G. Kitson, B.S. Larsen, and C.N. McEwen (1996), which was designed as an indispensible resource for GC/MS practitioners regardless of whether they are a novice or well experienced. The Fundamentals section has been extensively reworked from the original edition to give more depth of an understanding of the techniques and science involved with GC/MS. Even with this expansion, the original brevity and simple didactic style has been retained. Information on chromatographic peak deconvolution has been added along with a more in-depth understanding of the use of mass spectral databases in the identification of unknowns. Since the last edition, a number of advances in GC inlet systems and sample introduction techniques have occurred, and they are included in the new edition. Other updates include a discussion on fast GC and options for combining GC detectors with mass spectrometry.
The section regarding GC Conditions, Derivatization, and Mass Spectral Interpretation of Specific Compound Types has the same number of compound types as the original edition, but the information in each section has been expanded to not only explain some of the spectra but to also explain why certain fragmentations take place. The number of Appendices has been increased from 12 to 17. The Appendix on Atomic Masses and Isotope Abundances has been expanded to provide tools to aid in determination of elemental composition from isotope peak intensity ratios. An appendix with examples on "Steps to follow in the determination of elemental compositions based on isotope peak intensities" has been added. Appendices on whether to use GC/MS or LC/MS, third-party software for use in data analysis, list of information required in reporting GC/MS data, X+1 and X+2 peak relative intensities based on the number of atoms of carbon in an ion, and list of available EI mass spectral databases have been added. Others such as the ones on derivatization, isotope peak patterns for ions with Cl and/or Br, terms used in GC and in mass spectrometry, and tips on setting up, maintaining and troubleshooting a GC/MS system have all been expanded and updated.
The section regarding GC Conditions, Derivatization, and Mass Spectral Interpretation of Specific Compound Types has the same number of compound types as the original edition, but the information in each section has been expanded to not only explain some of the spectra but to also explain why certain fragmentations take place. The number of Appendices has been increased from 12 to 17. The Appendix on Atomic Masses and Isotope Abundances has been expanded to provide tools to aid in determination of elemental composition from isotope peak intensity ratios. An appendix with examples on "Steps to follow in the determination of elemental compositions based on isotope peak intensities" has been added. Appendices on whether to use GC/MS or LC/MS, third-party software for use in data analysis, list of information required in reporting GC/MS data, X+1 and X+2 peak relative intensities based on the number of atoms of carbon in an ion, and list of available EI mass spectral databases have been added. Others such as the ones on derivatization, isotope peak patterns for ions with Cl and/or Br, terms used in GC and in mass spectrometry, and tips on setting up, maintaining and troubleshooting a GC/MS system have all been expanded and updated.
- Covers the practical instruction necessary for successful operation of GC/MS equipment
- Reviews the latest advances in instrumentation, ionization methods, and quantitation
- Includes troubleshooting techniques and a variety of additional information useful for the GC/MS practitioner
- A true benchtop reference
- A guide to a basic understanding of the components of a Gas Chromatograph-Mass Spectrometer (GC-MS)
- Quick References to data interpretation
- Ready source for information on new analyses
Immediate value to the novice, experienced GC/MS user who may not have the breadth of knowledge covered in this book
Preface
Acknowledgments
1. Introduction and History
1.1. Instrumental Variables
1.2. Operational Variables
2. Gas Chromatography
2.1. Overview of a Gas Chromatograph
2.2. Sample Introduction
2.3. Separation of Components in the GC System
2.4. Overview of GC Detectors
2.5. Adding Versatility to the GC/MS System with Valves, Splitters, and Thermal Modulators
3. The GC/MS Interface
3.1. Open-Split Interface
3.2. Jet Separator
4. Mass Spectrometry Instrumentation
4.1. Overview of Mass Spectrometers
4.2. Resolution, Resolving Power, and Mass Accuracy
4.3. Vacuum System
4.4. Ionization Types
4.5. m/z Analyzer Types
4.6. Ion Detection
4.7. m/z Scale Calibration
4.8. Tuning the Mass Spectrometer
4.9. Data Acquisition
4.10. Tandem Mass Spectrometry (MS/MS)
4.11. Conclusion
5. Mass Spectral Data Interpretation
5.1. Using the Database Search
5.2. Identification of a Molecular Ion Peak in an EI Mass Spectrum
5.3. What to Do If There Is No Molecular Ion Peak
5.4. Selecting the Spectrum to Be Interpreted
5.5. Reading an EI Mass Spectrum
5.6. Final Remarks
6. Quantitation with GC/MS
6.1. Introduction
6.2. Selection of the Quantitation Ion
6.3. Quantitation Methods
6.4. Making Standard Solutions
6.5. External Standard Method
6.6. Internal Standard Method
6.7. Standard Additions
6.8. Concluding Remarks
7. Acids
7.1. GC Separations of Underivatized Carboxylic Acids
7.2. General Derivatization Procedure for C8–C24 Carboxylic Acids
7.3. GC Separation of Derivatized Carboxylic Acids
7.4. Mass Spectral Interpretation
8. Alcohols
8.1. GC Conditions for Underivatized Alcohols
8.2. TMS Derivative of >C10 Alcohols
8.3. Mass Spectral Interpretation
8.4. Aminoalcohols
9. Aldehydes
9.1. GC Separation of Underivatized Aldehydes
9.2. Derivatization of Formaldehyde
9.3. Mass Spectra of Aldehydes
10. Amides
10.1. GC Separation of Underivatized Amides
10.2. Derivatization of Amides
10.3. GC Separation of Derivatized Amides (TMS or Methyl-8®)
10.4. Mass Spectra of Amides
10.5. Mass Spectra of Derivatized Amide
11. Amines
11.1. GC Separations of Underivatized Amines
11.2. Derivatization of Amines and Diamines
11.3. GC Separation of Derivatized Amines
11.4. Mass Spectral Interpretation of Amines
11.5. Amino Alcohols (Aliphatic)
11.6. Aminophenols
11.7. Solvent Consideration
12. Amino Acids
12.1. GC Separation
12.2. Derivatization of Amino Acids and PTH–Amino Acids
12.3. Mass Spectral Interpretation
13. Common Contaminants
13.1. Contaminants Occasionally Observed after Derivatization with TMS Reagents
13.2. Contaminants Occasionally Observed in Underivatized Samples
13.3. Column Bleed
14. Drugs and Their Metabolites
14.1. GC Separations
14.2. Sample Preparation
14.3. Derivatization of Drugs and Metabolites
14.4. Mass Spectral Interpretation
15. Esters
15.1. GC Separation of Esters of Carboxylic Acids
15.2. Mass Spectra of Esters
16. Ethers
16.1. GC Separation of Ethers
16.2. Mass Spectra of Ethers
17. Fluorinated Compounds
17.1. GC Separations
17.2. Mass Spectra of Fluorinated Compounds
18. Gases
18.1. GC Separations
18.2. General Information
19. Glycols
19.1. GC Separations
19.2. Derivatization of Dry Glycols and Glycol Ethers
19.3. Mass Spectral Interpretation
20. Halogenated Compounds (Other Than Fluorinated Compounds)
20.1. GC Separations
20.2. Mass Spectra of Halogenated Compounds (Other Than Fluorinated Compounds)
21. Hydrocarbons
21.1. GC Separation of Hydrocarbons
21.2. Mass Spectra of Hydrocarbon Compounds
22. Isocyanates
22.1. GC Separations
22.2. Mass Spectral Interpretation
23. Ketones
23.1. GC Separation of Ketones
23.2. Derivatives of Ketones
23.3. Mass Spectra of Ketones
24. Nitriles
24.1. GC Separation of Nitriles
24.2. Mass Spectra
25. Nitroaromatics
25.1. GC Separation of Nitroaromatics
25.2. Mass Spectra of Nitroaromatics
26. Nitrogen-Containing Heterocyclic Compounds
26.1. GC Separations of Nitrogen-Containing Heterocyclic Compounds
26.2. Mass Spectra of Nitrogen-Containing Heterocyclics
27. Nucleosides (TMS Derivatives)
27.1. Derivatization
27.2. GC Separation of Derivatized Nucleosides
27.3. Mass Spectra of TMS–Nucleosides [2]
28. Pesticides
28.1. Chlorinated Pesticides
28.2. Organophosphorus Pesticides
28.3. Mass Spectra of Pesticides
29. Phenols
29.1. GC Separations of Underivatized Phenols and Dihydroxybenzenes
29.2. Derivatization of Phenols and Dihydroxybenzenes
29.3. GC Separations of Derivatized Phenols and Dihydroxybenzenes
29.4. Mass Spectra of Phenols
29.5. Aminophenols
29.6. Antioxidants
30. Phosphorus Compounds
30.1. GC Separations
30.2. Mass Spectra of Phosphorus Compounds
31. Plasticizers and Other Polymer Additives (Including Phthalates)
31.1. GC Separations
31.2. Mass Spectra
32. Prostaglandins (MO–TMS Derivatives)
32.1. Derivatization (MO–TMS)
32.2. GC Separation of Derivatized Prostaglandins
32.3. Mass Spectra of MO–TMS Derivatives of Prostaglandins
33. Solvents and Their Impurities
33.1. GC Separations of Industrial Solvent Mixtures
33.2. GC Separations of Impurities in Industrial Solvents
33.3. Mass Spectra of Solvents and Their Impurities
34. Steroids
34.1. GC Separation of Underivatized Steroids
34.2. Derivatization of Steroids
34.3. GC Separation of Derivatized Steroids
34.4. Mass Spectra of Underivatized Steroids
34.5. Mass Spectra of TMS Derivatives of Steroids
34.6. Mass Spectra of MO–TMS Derivatives
35. Sugars (Monosaccharides)
35.1. GC Separation of Derivatized Sugars
35.2. Mass Spectral Interpretation
36. Sulfur Compounds
36.1. GC Separations
36.2. Mass Spectra of Sulfur Compounds
Appendix
A. Definitions of Terms Related to Gas Chromatography
B. Definitions of Terms Related to Mass Spectrometry
C. Atomic Masses and Isotope Abundances and Other Information for the Determination of an Elemental Composition from Isotope Peak Intensity Ratios
D. X+1 and X+2 Values for Ions Containing Atoms of C and H Based on Isotope Contributions
E. Isotope Peak Patterns for Ions Containing Atoms of Cl and/or Br
F. Steps to Follow in the Determination of an Elemental Composition Based on Isotope Peak Intensity Ratios
G. Derivatization in GC/MS
H. Points of Comparison of LC/MS vs GC/MS
I. List of Available EI Mass Spectral Databases
J. Information Required for Reporting a GC/MS Analysis
K. Third-Party Software for Use with GC/MS
L. GC Installation and Maintenance
M. Troubleshooting Common GC Problems
N. Maintenance, Operating Tips, and Troubleshooting for Mass Spectrometers
O. Mixtures for Determining Mass Spectral Resolution
P. Cross-Index Chart for GC Stationary Phases
Q. Ions for Determining Unknown Structures
Index
Acknowledgments
1. Introduction and History
1.1. Instrumental Variables
1.2. Operational Variables
2. Gas Chromatography
2.1. Overview of a Gas Chromatograph
2.2. Sample Introduction
2.3. Separation of Components in the GC System
2.4. Overview of GC Detectors
2.5. Adding Versatility to the GC/MS System with Valves, Splitters, and Thermal Modulators
3. The GC/MS Interface
3.1. Open-Split Interface
3.2. Jet Separator
4. Mass Spectrometry Instrumentation
4.1. Overview of Mass Spectrometers
4.2. Resolution, Resolving Power, and Mass Accuracy
4.3. Vacuum System
4.4. Ionization Types
4.5. m/z Analyzer Types
4.6. Ion Detection
4.7. m/z Scale Calibration
4.8. Tuning the Mass Spectrometer
4.9. Data Acquisition
4.10. Tandem Mass Spectrometry (MS/MS)
4.11. Conclusion
5. Mass Spectral Data Interpretation
5.1. Using the Database Search
5.2. Identification of a Molecular Ion Peak in an EI Mass Spectrum
5.3. What to Do If There Is No Molecular Ion Peak
5.4. Selecting the Spectrum to Be Interpreted
5.5. Reading an EI Mass Spectrum
5.6. Final Remarks
6. Quantitation with GC/MS
6.1. Introduction
6.2. Selection of the Quantitation Ion
6.3. Quantitation Methods
6.4. Making Standard Solutions
6.5. External Standard Method
6.6. Internal Standard Method
6.7. Standard Additions
6.8. Concluding Remarks
7. Acids
7.1. GC Separations of Underivatized Carboxylic Acids
7.2. General Derivatization Procedure for C8–C24 Carboxylic Acids
7.3. GC Separation of Derivatized Carboxylic Acids
7.4. Mass Spectral Interpretation
8. Alcohols
8.1. GC Conditions for Underivatized Alcohols
8.2. TMS Derivative of >C10 Alcohols
8.3. Mass Spectral Interpretation
8.4. Aminoalcohols
9. Aldehydes
9.1. GC Separation of Underivatized Aldehydes
9.2. Derivatization of Formaldehyde
9.3. Mass Spectra of Aldehydes
10. Amides
10.1. GC Separation of Underivatized Amides
10.2. Derivatization of Amides
10.3. GC Separation of Derivatized Amides (TMS or Methyl-8®)
10.4. Mass Spectra of Amides
10.5. Mass Spectra of Derivatized Amide
11. Amines
11.1. GC Separations of Underivatized Amines
11.2. Derivatization of Amines and Diamines
11.3. GC Separation of Derivatized Amines
11.4. Mass Spectral Interpretation of Amines
11.5. Amino Alcohols (Aliphatic)
11.6. Aminophenols
11.7. Solvent Consideration
12. Amino Acids
12.1. GC Separation
12.2. Derivatization of Amino Acids and PTH–Amino Acids
12.3. Mass Spectral Interpretation
13. Common Contaminants
13.1. Contaminants Occasionally Observed after Derivatization with TMS Reagents
13.2. Contaminants Occasionally Observed in Underivatized Samples
13.3. Column Bleed
14. Drugs and Their Metabolites
14.1. GC Separations
14.2. Sample Preparation
14.3. Derivatization of Drugs and Metabolites
14.4. Mass Spectral Interpretation
15. Esters
15.1. GC Separation of Esters of Carboxylic Acids
15.2. Mass Spectra of Esters
16. Ethers
16.1. GC Separation of Ethers
16.2. Mass Spectra of Ethers
17. Fluorinated Compounds
17.1. GC Separations
17.2. Mass Spectra of Fluorinated Compounds
18. Gases
18.1. GC Separations
18.2. General Information
19. Glycols
19.1. GC Separations
19.2. Derivatization of Dry Glycols and Glycol Ethers
19.3. Mass Spectral Interpretation
20. Halogenated Compounds (Other Than Fluorinated Compounds)
20.1. GC Separations
20.2. Mass Spectra of Halogenated Compounds (Other Than Fluorinated Compounds)
21. Hydrocarbons
21.1. GC Separation of Hydrocarbons
21.2. Mass Spectra of Hydrocarbon Compounds
22. Isocyanates
22.1. GC Separations
22.2. Mass Spectral Interpretation
23. Ketones
23.1. GC Separation of Ketones
23.2. Derivatives of Ketones
23.3. Mass Spectra of Ketones
24. Nitriles
24.1. GC Separation of Nitriles
24.2. Mass Spectra
25. Nitroaromatics
25.1. GC Separation of Nitroaromatics
25.2. Mass Spectra of Nitroaromatics
26. Nitrogen-Containing Heterocyclic Compounds
26.1. GC Separations of Nitrogen-Containing Heterocyclic Compounds
26.2. Mass Spectra of Nitrogen-Containing Heterocyclics
27. Nucleosides (TMS Derivatives)
27.1. Derivatization
27.2. GC Separation of Derivatized Nucleosides
27.3. Mass Spectra of TMS–Nucleosides [2]
28. Pesticides
28.1. Chlorinated Pesticides
28.2. Organophosphorus Pesticides
28.3. Mass Spectra of Pesticides
29. Phenols
29.1. GC Separations of Underivatized Phenols and Dihydroxybenzenes
29.2. Derivatization of Phenols and Dihydroxybenzenes
29.3. GC Separations of Derivatized Phenols and Dihydroxybenzenes
29.4. Mass Spectra of Phenols
29.5. Aminophenols
29.6. Antioxidants
30. Phosphorus Compounds
30.1. GC Separations
30.2. Mass Spectra of Phosphorus Compounds
31. Plasticizers and Other Polymer Additives (Including Phthalates)
31.1. GC Separations
31.2. Mass Spectra
32. Prostaglandins (MO–TMS Derivatives)
32.1. Derivatization (MO–TMS)
32.2. GC Separation of Derivatized Prostaglandins
32.3. Mass Spectra of MO–TMS Derivatives of Prostaglandins
33. Solvents and Their Impurities
33.1. GC Separations of Industrial Solvent Mixtures
33.2. GC Separations of Impurities in Industrial Solvents
33.3. Mass Spectra of Solvents and Their Impurities
34. Steroids
34.1. GC Separation of Underivatized Steroids
34.2. Derivatization of Steroids
34.3. GC Separation of Derivatized Steroids
34.4. Mass Spectra of Underivatized Steroids
34.5. Mass Spectra of TMS Derivatives of Steroids
34.6. Mass Spectra of MO–TMS Derivatives
35. Sugars (Monosaccharides)
35.1. GC Separation of Derivatized Sugars
35.2. Mass Spectral Interpretation
36. Sulfur Compounds
36.1. GC Separations
36.2. Mass Spectra of Sulfur Compounds
Appendix
A. Definitions of Terms Related to Gas Chromatography
B. Definitions of Terms Related to Mass Spectrometry
C. Atomic Masses and Isotope Abundances and Other Information for the Determination of an Elemental Composition from Isotope Peak Intensity Ratios
D. X+1 and X+2 Values for Ions Containing Atoms of C and H Based on Isotope Contributions
E. Isotope Peak Patterns for Ions Containing Atoms of Cl and/or Br
F. Steps to Follow in the Determination of an Elemental Composition Based on Isotope Peak Intensity Ratios
G. Derivatization in GC/MS
H. Points of Comparison of LC/MS vs GC/MS
I. List of Available EI Mass Spectral Databases
J. Information Required for Reporting a GC/MS Analysis
K. Third-Party Software for Use with GC/MS
L. GC Installation and Maintenance
M. Troubleshooting Common GC Problems
N. Maintenance, Operating Tips, and Troubleshooting for Mass Spectrometers
O. Mixtures for Determining Mass Spectral Resolution
P. Cross-Index Chart for GC Stationary Phases
Q. Ions for Determining Unknown Structures
Index
- No. of pages: 632
- Language: English
- Edition: 2
- Published: March 30, 2011
- Imprint: Academic Press
- Paperback ISBN: 9780123736284
- eBook ISBN: 9780080920153
OS
O. David Sparkman
Affiliations and expertise
Antioch, CA, USARead Gas Chromatography and Mass Spectrometry: A Practical Guide on ScienceDirect