Modern Practice Of Gas Chromatography

1036 Pages·2004·13.022 MB·English

by  Robert L. Grob, Eugene F. Barry

MODERN PRACTICE OF
GAS CHROMATOGRAPHY
MODERN PRACTICE OF
GAS CHROMATOGRAPHY
FOURTH EDITION
Editedby
Robert L. Grob, Ph.D.
ProfessorEmeritus,AnalyticalChemistry,VillanovaUniversity
Eugene F. Barry, Ph.D.
ProfessorofChemistry,UniversityofMassachusettsLowell
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LibraryofCongressCataloging-in-PublicationData
Modernpracticeofgaschromatography.—4thed./editedbyRobertL.Grob,EugeneF.Barry.
p.cm.
Includesbibliographicalreferencesandindex.
ISBN0-471-22983-0(acid-freepaper)
1.Gaschromatography.I.Grob,RobertLee.II.Barry,EugeneF.
QD79.C45M632004
543(cid:1).85—dc22
2003062033
PrintedintheUnitedStatesofAmerica.
10987654321
To
Our
WivesandFamilies
What is written without effort is in general read without pleasure
—Samuel Johnson (1709–1784)
JohnsonianMiscellanies
Vol. ii, p. 309
CONTRIBUTORS
Juan G. Alvarez, Department of Obstetrics & Gynecology, Beth Israel Hos-
pital, Harvard Medical School, Boston, Massachusetts; Centro de Infertilidad
Masculina Androgen, Hospital San Rafael, La Corun˜a, Spain
Lisa J. Baird, Department of Chemistry, The State University of New York at
Buffalo, Buffalo, New York
Eugene F. Barry, Chemistry Department, University of Massachusetts Lowell,
Lowell, Massachusetts
Reginald J. Bartram, Alltech Associates, Inc., State College, Pennsylvania
Thomas A. Brettell, New Jersey State Police Forensic Science Laboratory,
Hamilton, New Jersey
Gary W. Caldwell, Johnson and Johnson Pharmaceutical Research and Devel-
opment, L.L.C., Spring House, Pennsylvania
Luis A. Colo´n, Department of Chemistry, The State University of New York at
Buffalo, Buffalo, New York
Mark E. Craig, ExxonMobil Chemical Company, Baytown, Texas
Cecil R. Dybowski, Chemistry Department, University of Delaware, Newark,
Delaware
Robert L. Grob, Professor Emeritus of Analytical Chemistry, Villanova Uni-
versity, Villanova, Pennsylvania
John V. Hinshaw, Serveron Corporation, Hillsboro, Oregon
Mary A. Kaiser, E. I. DuPont de Nemours & Company, Central Research &
Development, Wilmington, Delaware
Richard E. Lester, Federal Bureau of Investigation (FBI) Academy, Quan-
tico, Virginia
John A. Masucci, Johnson and Johnson PharmaceuticalResearchand Develop-
ment, L.L.C., Spring House, Pennsylvania
vii
viii CONTRIBUTORS
Richard D. Sacks, Department of Chemistry, University of Michigan, Ann
Arbor, Michigan
Gregory C. Slack, Wyeth Pharmaceuticals, Rouses Point, New York
Edward F. Smith, ExxonMobil Chemical Company, Baytown, Texas
NicholasH.Snow, DepartmentofChemistryandBiochemistry,SetonHallUni-
versity, South Orange, New Jersey
John L. Snyder, Lancaster Laboratories, Inc., Lancaster, Pennsylvania
Clifford C. Walters, ExxonMobil Research & Engineering Company, Clinton,
New Jersey
CONTENTS
Preface xi
1. Introduction 1
RobertL.Grob
PART I THEORY AND BASICS
2. Theory of Gas Chromatography 25
RobertL.Grob
3. Columns: Packed and Capillary; Column Selection 65
in Gas Chromatography
EugeneF.Barry
4. Optimization of Separations and Computer Assistance 193
JohnV.Hinshaw
5. High-Speed Gas Chromatography 229
RichardD.Sacks
PART II TECHNIQUES AND INSTRUMENTATION
6. Detectors in Modern Gas Chromatography 277
LuisA.Colo´nandLisaJ.Baird
7. Techniques for Gas Chromatography/Mass Spectrometry 339
JohnA.MasucciandGaryW.Caldwell
8. Qualitative and Quantitative Analysis by Gas Chromatography 403
RobertL.GrobandMaryA.Kaiser
9. Inlet Systems for Gas Chromatography 461
NicholasH.Snow
10. Gas Management Systems for Gas Chromatography 491
ReginaldJ.Bartram
ix
x CONTENTS
PART III APPLICATIONS
11. Sample Preparation Techniques for Gas Chromatography 547
NicholasH.SnowandGregoryC.Slack
12. Physicochemical Measurements by Gas Chromatography 605
MaryA.KaiserandCecilR.Dybowski
13. Petroleum and Petrochemical Analysis by Gas
Chromatography 643
EdwardF.Smith,MarkE.Craig,andCliffordC.Walters
14. Clinical and Pharmaceutical Applications of Gas 739
Chromatography
JuanG.Alvarez
15. Environmental Applications of Gas Chromatography 769
JohnL.Snyder
16. Forensic Science Applications of Gas Chromatography 883
ThomasA.Brettell
17. Validation and QA/QC of Gas Chromatographic Methods 969
ThomasA.BrettellandRichardE.Lester
APPENDIXES
Appendix A. Effect of Detector Attenuation Change and Chart
Speed on Peak Height, Peak Width, and Peak Area 991
RobertL.GrobandEugeneF.Barry
Appendix B. Gas Chromatographic Acronyms and Symbols
and Their Definitions 995
RobertL.GrobandEugeneF.Barry
Appendix C. Useful Hints for Gas Chromatography 1007
RobertL.GrobandEugeneF.Barry
INDEX 1011
PREFACE
ThefourtheditionofModernPracticeofGasChromatography representsanum-
ber of changes from the first three editions. First, a number of new contributing
authors have been involved. These authors were chosen because of their exper-
tise and active participation in the various areas related to gas chromatography
(GC). Second, the contents of the various chapters have been changed so as
to be all-inclusive. For example, a discussion of the necessary instrumentation
has been included in chapters covering such topics as columns, detectors, fast
gas chromatography, and sample preparation. Third, separate chapters are ded-
icated to gas chromatography/mass spectrometry, sample preparation, fast gas
chromatography, optimization and computer assistance, and QA/QC validation
of gas chromatographic methods. Another change has been the elimination of
several chapters because of their adequate coverage in other texts. The editors
aresatisfiedthatthisneweditionrepresentsanall-inclusivetextthatmaybeused
for university courses as well as short courses.
No bookwill pleaseeveryone.Eachpersonhascertainideasconcerningwhat
should be coveredand how much detail should be given to eachtopic. Coverage
of the theory and basics of GC is what we consider necessary to the beginner
for this technique and the nomenclature is that most recently recommended by
the IUPAC Commission. The techniques and instrumentation section is greatly
detailed, and the application chapters cover topics that would be of interest to
most people utilizing the gas chromatographic technique.
The editors thank the contributing authors for their cooperation and profes-
sionalism, thus making this fourth edition a reality. A special thanks to Dr.
NicholasH.Snow,ofSetonHallUniversityforhiscontributions overandabove
the professional level. Most importantly, the editors thank their wives Marjorie
and Dee for their interest, encouragement, and cooperation during these many
months of preparation. Dr. Grob especially wishes to thank his son, G. Duane
Grobforallhisassistanceandencouragementin thecomputer aspectsof putting
this book together.
ROBERT L. GROB
Malvern,Pennsylvania
2004
EUGENE F. BARRY
Nashua,NewHampshire
2004
xi