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Investigating gas chromatography.
Experiment #8 from Organic Chemistry with Vernier
Introduction
Gas Chromatography is a technique widely used to separate complex mixtures of substances. Compounds present in a volatile liquid or gaseous solute are isolated after traveling through a coated column based on the substance’s size and intermolecular interactions. If a compound tends to bind to the column through intermolecular interactions, it takes a longer time to emerge compared with a compound that does not tend to stick onto the column. The level of binding experienced between the substances and the column is determined based on the number and strength of intermolecular interactions between the two species. Substances that pass quickly through the column exhibit fewer intermolecular interactions with the column.
The Vernier Mini GC uses a metal column with a nonpolar coating, called the stationary phase. A sample, consisting of one or more compounds, is injected into the column and is carried through the stationary phase by atmospheric air, which acts as the mobile phase. The nonpolar coating of the stationary phase most strongly retains solutes of the same polarity. Organic compounds flowing out of the chromatography column are then detected by a chemical sensor that produces electrical responses proportional to the concentration of the compounds. The presence of such a chemical at the detector is seen as a peak on a chromatogram. The unique time it takes for a compound to exit the column after it is injected is called the retention time. With a gas chromatograph, a compound can be identified from a mixture by its retention time.
Several factors can affect a compound’s retention time. More volatile compounds (i.e., compounds with a lower boiling point) will move through the column faster because they are flowing in the mobile phase and not strongly bonded with the stationary phase. The surface functional groups present on the compound are also a factor. For example, alcohols may weakly bond with a polar stationary phase more than esters because alcohols are capable of forming hydrogen bonds. The molecular weight of a compound may also play a role to a slight extent, although it is not a direct relationship that the heavier the molecule, the slower it will travel through a GC column.
As you will discover in this experiment, the instrument settings also affect a compound’s retention time. When separating compounds with a wide range of boiling points and polarities, it helps to raise the column temperature during the separation. Temperature programming reduces elution times of highly retained compounds. Adjusting the pressure will have a similar affect; higher pressures cause greater strain on the intermolecular interactions between the compound and stationary phase, ultimately reducing the retention time.
In this experiment, you will gain experience with the Vernier Mini GC by injecting a known sample into the device. The sample contains five compounds that will separate under the proper conditions. You will test this one mixture of compounds repeatedly and vary the profile of the Mini GC operation to obtain the best possible separation of this mixture.
In this experiment, you will
- Measure and analyze the chromatogram of a mixture of five compounds as they pass through a Vernier Mini GC.
- Vary the temperature-pressure profile of the Mini GC and observe how the chromatogram is affected by such changes.
- Determine the best temperature-pressure profile to obtain clear separation of all five compounds.
Sensors and Equipment
This experiment features the following sensors and equipment. Additional equipment may be required.
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This experiment is #8 of Organic Chemistry with Vernier . The experiment in the book includes student instructions as well as instructor information for set up, helpful hints, and sample graphs and data.
Practical Gas Chromatography
A Comprehensive Reference
- © 2014
- Katja Dettmer-Wilde 0 ,
- Werner Engewald 1
Institute of Functional Genomics, University of Regensburg, Regensburg, Germany
You can also search for this editor in PubMed Google Scholar
Institute for Analytical Chemistry, University of Leipzig, Leipzig, Germany
- A practical reference for making the most out of gas chromatography
- Comprehensive coverage of fundamentals, instrumentation and cutting-edge applications
- Edited and written by renowned experts
- Includes supplementary material: sn.pub/extras
176k Accesses
68 Citations
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About this book
Gas chromatography continues to be one of the most widely used analytical techniques, since its applications today expand into fields such as biomarker research or metabolomics. This new practical textbook enables the reader to make full use of gas chromatography. Essential fundamentals and their implications for the practical work at the instrument are provided, as well as details on the instrumentation such as inlet systems, columns and detectors. Specialized techniques from all aspects of GC are introduced ranging from sample preparation, solvent-free injection techniques, and pyrolysis GC, to separation including fast GC and comprehensive GCxGC and finally detection, such as GC-MS and element-specific detection. Various fields of application such as enantiomer, food, flavor and fragrance analysis, physicochemical measurements, forensic toxicology, and clinical analysis are discussed as well as cutting-edge application in metabolomics is covered.
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Table of contents (25 chapters)
Front matter, introduction.
- Werner Engewald, Katja Dettmer-Wilde
Theory of Gas Chromatography
Columns and stationary phases.
- Werner Engewald, Katja Dettmer-Wilde, Harald Rotzsche
Selection of Capillary Columns and Operating Conditions
Inlet systems and sample introduction.
- Maurus Biedermann
- Jan T. Andersson
Qualitative Analysis
- Katja Dettmer-Wilde, Werner Engewald
Quantitative Analysis
Gas chromatography-mass spectrometry.
- Monika Moeder
Element-Specific Detection
- Sibylle Mothes, Jürgen Mattusch
Solvent-Free Extraction and Injection Techniques
- Maik A. Jochmann, Jens Laaks, Torsten C. Schmidt
Shortening Analysis Time (Fast GC)
- Hans-Ulrich Baier
Multidimensional and Comprehensive Two-Dimensional Gas Chromatography
- Mohamed Adahchour, Udo A. Th. Brinkman
QA/QC in Gas Chromatography
- Peter Schultze
Applications
The analytical separation of enantiomers by gas chromatography on chiral stationary phases.
- Markus Juza, Volker Schurig
Sample Preparation Techniques for GC
- Lourdes Ramos
Derivatization
Katja Dettmer-Wilde
“This textbook is worth reading by beginners in the fields of GC as well as those advanced users looking for inspiration in GC applications. In any library used by analytical scientists, this textbook is a must. It is an ideal combination of theory and practice written and edited by passionate chromatographers. … the book is worth buying and it may serve as your reference in practical GC analysis.” (Martin Vogel, Analytical and Bioanalytical Chemistry, Vol. 408 (29), November, 2016)
“This is a mammoth work and one must congratulate the editors on the result of their task. … all users of GC will learn a lot fromthis book and, no matter how expert, they will find new and relevant information on their own specific problems.” (Edward R. Adlard, Chromatographia, Vol. 78, 2015)
Editors and Affiliations
Werner Engewald
About the editors
Katja Dettmer-Wilde is Principal Investigator heading the mass spectrometry - metabolomics group at the Institute of Functional Genomics, University of Regensburg, Germany. She studied chemistry at the University of Leipzig and got her PhD with Werner Engewald working on the analysis of volatile organic compounds by GC-MS. Since her postdoctoral studies at the University of California Davis she has been focusing on hyphenated separation techniques in metabolomics.
Werner Engewald is professor emeritus of the University of Leipzig, Germany. He is one of the leading gas chromatographers worldwide and has made substantial contributions towards the development of this technique. He regularly gives courses for GC users. He was awarded the Martin gold medal of the Chromatographic Society in 2002 and the Clemens-Winkler-Medal of the Division of Analytical Chemistry of the German Chemical Society in 2009.
Bibliographic Information
Book Title : Practical Gas Chromatography
Book Subtitle : A Comprehensive Reference
Editors : Katja Dettmer-Wilde, Werner Engewald
DOI : https://doi.org/10.1007/978-3-642-54640-2
Publisher : Springer Berlin, Heidelberg
eBook Packages : Chemistry and Materials Science , Chemistry and Material Science (R0)
Copyright Information : Springer-Verlag Berlin Heidelberg 2014
Hardcover ISBN : 978-3-642-54639-6 Published: 14 November 2014
Softcover ISBN : 978-3-662-51861-8 Published: 23 August 2016
eBook ISBN : 978-3-642-54640-2 Published: 05 November 2014
Edition Number : 1
Number of Pages : XV, 902
Number of Illustrations : 207 b/w illustrations, 249 illustrations in colour
Topics : Chromatography , Pharmacology/Toxicology , Monitoring/Environmental Analysis
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