Gas Chromatography and Mass Spectrometry: A Practical Guide - 2nd Edition - ISBN: 9780123736284, 9780080920153

Gas Chromatography and Mass Spectrometry: A Practical Guide

2nd Edition

Authors: O. David Sparkman Zelda Penton Fulton Kitson
Paperback ISBN: 9780123736284
eBook ISBN: 9780080920153
Imprint: Academic Press
Published Date: 30th March 2011
Page Count: 632
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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), 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.


Key Features

  • 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 as well as the experienced GC/MS user who may not have the breadth of knowledge covered in this book.

Table of Contents



Chapter 1. Introduction and History

1.1. Instrumental Variables

1.2. Operational Variables

Chapter 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

Chapter 3. The GC/MS Interface

3.1. Open-Split Interface

3.2. Jet Separator

Chapter 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

Chapter 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

Chapter 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

Chapter 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

Chapter 8. Alcohols

8.1. GC Conditions for Underivatized Alcohols

8.2. TMS Derivative of >C10 Alcohols

8.3. Mass Spectral Interpretation

8.4. Aminoalcohols

Chapter 9. Aldehydes

9.1. GC Separation of Underivatized Aldehydes

9.2. Derivatization of Formaldehyde

9.3. Mass Spectra of Aldehydes

Chapter 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

Chapter 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

Chapter 12. Amino Acids

12.1. GC Separation

12.2. Derivatization of Amino Acids and PTH–Amino Acids

12.3. Mass Spectral Interpretation

Chapter 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

Chapter 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

Chapter 15. Esters

15.1. GC Separation of Esters of Carboxylic Acids

15.2. Mass Spectra of Esters

Chapter 16. Ethers

16.1. GC Separation of Ethers

16.2. Mass Spectra of Ethers

Chapter 17. Fluorinated Compounds

17.1. GC Separations

17.2. Mass Spectra of Fluorinated Compounds

Chapter 18. Gases

18.1. GC Separations

18.2. General Information

Chapter 19. Glycols

19.1. GC Separations

19.2. Derivatization of Dry Glycols and Glycol Ethers

19.3. Mass Spectral Interpretation

Chapter 20. Halogenated Compounds (Other Than Fluorinated Compounds)

20.1. GC Separations

20.2. Mass Spectra of Halogenated Compounds (Other Than Fluorinated Compounds)

Chapter 21. Hydrocarbons

21.1. GC Separation of Hydrocarbons

21.2. Mass Spectra of Hydrocarbon Compounds

Chapter 22. Isocyanates

22.1. GC Separations

22.2. Mass Spectral Interpretation

Chapter 23. Ketones

23.1. GC Separation of Ketones

23.2. Derivatives of Ketones

23.3. Mass Spectra of Ketones

Chapter 24. Nitriles

24.1. GC Separation of Nitriles

24.2. Mass Spectra

Chapter 25. Nitroaromatics

25.1. GC Separation of Nitroaromatics

25.2. Mass Spectra of Nitroaromatics

Chapter 26. Nitrogen-Containing Heterocyclic Compounds

26.1. GC Separations of Nitrogen-Containing Heterocyclic Compounds

26.2. Mass Spectra of Nitrogen-Containing Heterocyclics

Chapter 27. Nucleosides (TMS Derivatives)

27.1. Derivatization

27.2. GC Separation of Derivatized Nucleosides

27.3. Mass Spectra of TMS–Nucleosides [2]

Chapter 28. Pesticides

28.1. Chlorinated Pesticides

28.2. Organophosphorus Pesticides

28.3. Mass Spectra of Pesticides

Chapter 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

Chapter 30. Phosphorus Compounds

30.1. GC Separations

30.2. Mass Spectra of Phosphorus Compounds

Chapter 31. Plasticizers and Other Polymer Additives (Including Phthalates)

31.1. GC Separations

31.2. Mass Spectra

Chapter 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

Chapter 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

Chapter 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

Chapter 35. Sugars (Monosaccharides)

35.1. GC Separation of Derivatized Sugars

35.2. Mass Spectral Interpretation

Chapter 36. Sulfur Compounds

36.1. GC Separations

36.2. Mass Spectra of Sulfur Compounds

Appendix A. Definitions of Terms Related to Gas Chromatography

Appendix B. Definitions of Terms Related to Mass Spectrometry

Appendix C. Atomic Masses and Isotope Abundances and Other Information for the Determination of an Elemental Composition from Isotope Peak Intensity Ratios

Appendix D. X+1 and X+2 Values for Ions Containing Atoms of C and H Based on Isotope Contributions

Appendix E. Isotope Peak Patterns for Ions Containing Atoms of Cl and/or Br

Appendix F. Steps to Follow in the Determination of an Elemental Composition Based on Isotope Peak Intensity Ratios

Appendix G. Derivatization in GC/MS

Appendix H. Points of Comparison of LC/MS vs GC/MS

Appendix I. List of Available EI Mass Spectral Databases

Appendix J. Information Required for Reporting a GC/MS Analysis

Appendix K. Third-Party Software for Use with GC/MS

Appendix L. GC Installation and Maintenance

Appendix M. Troubleshooting Common GC Problems

Appendix N. Maintenance, Operating Tips, and Troubleshooting for Mass Spectrometers

Appendix O. Mixtures for Determining Mass Spectral Resolution

Appendix P. Cross-Index Chart for GC Stationary Phases

Appendix Q. Ions for Determining Unknown Structures



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About the Author

O. David Sparkman

Affiliations and Expertise

Antioch, CA, USA

Zelda Penton

Fulton Kitson


"The authors have kept this book relevant and timely and have achieved their goal of providing useful information for practitioners. They understand what those who actually use GC/MS need, and continue to add appendixes of numerical information (increased from 12 to 17 in this revision)…The entire book has been updated and improved where needed; for example, chapter 6, covering the challenging topic of quantitation, has been "completely reworked." Sparkman and his collaborators continue to write high-quality books that are extremely useful, precise, and interesting to both novices and experienced scientists. Summing Up: Highly recommended. Upper-division undergraduates through professionals/practicioners."--CHOICE