Gas Chromatography and Mass Spectrometry: A Practical Guide

Gas Chromatography and Mass Spectrometry: A Practical Guide

2nd Edition - March 30, 2011

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  • Authors: O David Sparkman, Zelda Penton, Fulton Kitson
  • eBook ISBN: 9780080920153
  • Paperback ISBN: 9780123736284

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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

  • Preface


    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


Product details

  • No. of pages: 632
  • Language: English
  • Copyright: © Academic Press 2011
  • Published: March 30, 2011
  • Imprint: Academic Press
  • eBook ISBN: 9780080920153
  • Paperback ISBN: 9780123736284

About the Authors

O David Sparkman

Affiliations and Expertise

Antioch, CA, USA

Zelda Penton

Fulton Kitson

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