Gas Chromatography – Mass Spectrometry

(principle and applications)

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 CONTENTS

Introduction
 GC
 MS

GC-MS
 Principle
 Instrumentation
 Application

References

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 INTRODUCTION
History: In 1958, Holmes and Morell successfully combined Gas
Chromatography (GC) with Mass spectrometer (MS) to produce the first
hyphenated system.

Basic concepts:
GC- Technique for separation of
Gaseous and volatile substances.

Interface – To transport sample into

ion source of mass analyzer.

MS- Technique for determination of

molecular weight.

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 GAS CHROMATOGRAPHY

What is Gas chromatography?

Gas chromatography, GC is used in analytical chemistry for
separating and analyzing compounds that can be vaporized
without decomposition.

Basic Principle of GC
Sample vaporized by injection into a heated system, eluted
through a column by inert gaseous mobile phase and detected.

Types
-Gas liquid chromatography, GLC.
-Gas solid chromatography, GSC.

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 BASIC COMPONENTS
1. Carrier gas

2. A sample injection system

3. Column

3. Column oven

5. Detectors

6. An amplification
and recorder system
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 MASS SPECTROMETRY
What is Mass spectrometry?
Mass spectrometry, MS is an analytical technique that measures the mass-
to-charge ratio of charged particles.
Principle
Gas-phase ions are separated according to mass/charge ratio and
sequentially detected.
Power
supplies

iIon Mass
Ion source Ion Sensor
acceleration Analyzer

Vacuum
Pump
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 WHY GC- MS
Drawbacks of GC-
Lack of definitive proof of nature of detected compound.
Useful only for thermostable and volatile samples.
 Drawbacks of MS-
Handling of mixture of compounds .

GC-MS –
 It show high resolution separation.
 Highly sensitive.
 Specific structure determination.
 Identifies the actual presence of a particular substance in a
given sample.

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 GASS CHROMATOGRAPHY-MASS
SPECTROMETRY (GC-MS)
Gas chromatography/mass spectrometry (GC/MS) is the synergistic
combination of two powerful analytical techniques.

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 HOW DOES GC/MS WORK
GC equipment (using capillary column) can be directly
interfaced with rapid-scan Mass Spectrometer.

The high purity carrier gas flows into the injector, through
the column and then into the Mass Spectrometer.

A sample is introduced into the injector usually with a

syringe or an exterior sampling device.

 The vaporized solutes are transported into the column by

the carrier gas. The various solutes travel through the
column at different rates.

Each solute from the column enters the mass spectrometer

through interface.
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 INTERFACE

 Transports the effluent from the gas chromatography to mass

spectrometer.

 An ideal interface should:

 Quantitatively transfer all analyte.

 Reduce pressure/flow from chromatograph to level MS can

handle.

 Not cost an arm (or a leg).

No interface meets all requirements.

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 TYPES OF INTERFACE

1. Effusion separator

2. Membrane separator

3. Jet separator

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 EFFUSION SEPARATOR
To
vacuum
pump

From
To MS
GC

Sintered glass

Effluent from GC passes through ultrafine porous sintered glass

having average pore size of about 10 -4 .

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 MEMBRANE SEPARATOR
Vent From GC

Membrane

To MS

Dimethyl Silicon rubber used as a membrane generally

having thickness of 0.025 -0.040 mm.

Limitation –
Operates within temperature limit ( 80˚C – 220˚C). 13
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 JET SEPARATOR

 Effluent from GC pass through orifice where Expansion and

diffusion of Helium occurres while sample in gas stream travels
directly forward to second jet or orifice.
 All Glass jet separator is frequently used for packed column
operation.
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 TYPES OF IONIZATION

 Electron impact and chemical ionization are the two

methods most widely used in GC/MS work

• Electron impact (EI) - most common.

• Chemical ionization (CI) - a modification of EI which

results in ‘softer’ ionization
- less fragmentation.

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 DIFFERENT TYPES OF
ANALYSER

Ion trap mass spectrometer.

Magnetic sector mass spectrometer.

Time of flight (TOF).

Linear Quadrupole Mass Analyser.

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Linear Quadrupole Mass Analyser-

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Limitations of GC/MS Strengths of GC/MS
Analysis Analysis

Sample must either be volatile or capable Identification of organic components by

of being derivatized to be volatile separating complex mixtures

Very Expensive Quantitative analysis

Trace-level determination of organic

contamination low to mid-ppb level for
liquids and low nanogram level for solids
(Dynamic Headspace Analysis)
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 GENERAL APPLICATIONS

• Identification and quantitation of volatile and semi volatile

organic compounds in complex mixtures.

• Determination of molecular weights and (sometimes) elemental

compositions of unknown organic compounds in complex
mixtures.

• Structural determination of unknown organic compounds in

complex mixtures both by matching their spectra with reference
spectra and by a prior spectral interpretation.

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 APPLICATIONS
 Environmental Monitoring and Cleanup.

 Criminal Forensics.

 Law Enforcement.

 Security.

 Food, Beverage and Perfume Analysis.

 Astrochemistry.

 Separation of degradation products.

 Diagnosis of disease states.

 Antibiotic metabolites. 20
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• Environmental Monitoring and Cleanup-
GC-MS is being the tool of choice for tracking organic
pollutants in environments.

• Criminal Forensics-
GC-MS can analyze the particles from a human body in order
to help link a criminal to a crime.

• Law Enforcement –
GC-MS is increasingly used for detection of illegal narcotics.

• Security-
Explosive detection systems run on a host of technologies,
many of them based on GC-MS.

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• Food, beverage and perfume analysis -
GC-MS is extensively used for the analysis of these compounds
which include esters, fatty acids, alcohols, aldehydes, terpenes. It is
also used to detect and measure contaminants from spoilage or
adulteration which may be harmful and which is often controlled by
governmental agencies, for example pesticides.

•Astrochemistry-
GC –MS is used to analyze atmosphere.

•Separation of degradation products-

Separation & identification of degradation product of organic and
organometallic compounds to help in elucidation of their structure.

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•Diagnosis of disease states-
1)GC –MS is to determination of changes in the biochemical
composition of the cell and body fluids.

2) Determination of clinical disease state.

•Antibiotic Metabolites-
GC-MS is used in investigation of choramphenicol,
thiamphenicol and other such broad spectrum antibiotics.

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 REFERENCES
1) Hobart H.Willar , Lynne L.Merritt Jr., John A. Dean, Frank A. settle, J
Instrumental methods of analysis, Seventh Edition,Wadsworthpublishing
company,U.S.A,465.

2) Skoog D.A, Holler J. F, Neiman T. A., Principles of Instrumental Analysis,5th

Edition, Harcourt Brace College Publishers, NY, 300-324.

3)Ronald A. Hite ,Gas Chromatography Mass Spectrometry Indiana University

School of Public and Environmental Affairs and Department of Chemistry.

4) Ian A. Fowlis , Gas Chromatography, Second Edition, University of

Northumbria at Newcastle.

5)G.A. Eiceman, Instrumentation of gas chromatography , New Mexico State

University, Las Cruces,USA.
6)Thomas Steger-HartmannaChapter 25 Chromatography Software
Schering AG, Experimental Toxicology, Müllerstrasse 178,
13342 Berlin, Germany. 24
7) Harris, Daniel C. , "24. Gas Chromatography", Quantitative chemical
analysis (Fifth ed.), W. H. Freeman and Company, pp. 675--712, ISBN 0-
7167-2881-8, 1999.

8) Gohlke, R. S. ,"Time-of-Flight Mass Spectrometry and Gas-Liquid

Partition Chromatography". Analytical Chemistry 31: 535.
doi:10.1021/ac50164a024,1959.

9) C. Eric Boswell,Efficient volatiles analysis by Purge and Trap GC/MS,

National Air and Radiation Environmental Laboratory, Mixed Waste
Analytical Program,540 South Morris Avenue, Montgomery, AL 36115
(334) 270-7071.

10) Gohlke, R; McLafferty, Fred W., "Early gas chromatography/mass

spectrometry". Journal of the American Society for Mass Spectrometry 4:
367. doi:10.1016/1044-0305(93)85001-E, 1913.

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10) M. L. Vincent and D. G. Peters, Journal of Electroanalyical Chemistry
Interfacial Electrochemistry, 327(1992), 121–35.

11)Journal of the American Society for Mass Spectrometry

Volume 4, Issue 5, May 1993, Pages 367-37

13) http://orgchem.colorado.edu/hndbksupport/GC/GC.html

14)http://www2.chemistry.msu.edu/faculty/reusch/VirtTxtJml/Spectrp y/
MassSpec/masspec1.htm

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THANK YOU