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Chromatography
Monroe L. Weber-Shirk
Gas Chromatograph:
an overview
What
is chromatography
History of chromatography
Applications
Theory of operation
Detectors
What is Chromatography
color writing
the separation of mixtures into their constituents by
preferential adsorption by a solid (Random House College
Dictionary, 1988)
Chromatography is a physical method of separation in
which the components to be separated are distributed
between two phases, one of the phases constituting a
______________ of large surface area, the other being a
stationary
bedor along the stationary bed.
______ that percolates
through
(Ettre & Zlatkis, 1967,
The Practice of Gas
fluid
Chromatography)
History of Chromatography
1903
chromatography
1930s -
solid chromatography
Gas Chromatography
Applications
Compound must exist as a ____gas
at a temperature that can be
produced by the GC and withstood by the column (up to
450C)
Depending on the column
Alcohols in blood
Aromatics (benzene, toluene, ethylbenzene, xylene)
Flavors and Fragrances
Permanent gases (H2, N2, O2, Ar, CO2, CO, CH4)
Hydrocarbons
Pesticides, Herbicides, PCBs, and Dioxins
Solvents
Advantages of Gas
Chromatography
Requires only very small samples with little
preparation
Good at separating complex mixtures into
components
Results are rapidly obtained (1 to 100 minutes)
Very high precision
Only instrument with the sensitivity to detect
volatile organic mixtures of low concentrations
Equipment is not very complex (sophisticated oven)
Chromatogram of Gasoline
1. Isobutane
2. n-Butane
3. Isopentane
4. n-Pentane
5. 2,3-Dimethylbutane
6. 2-Methylpentane
7. 3-Methylpentane
8. n-Hexane
9. 2,4-Dimethylpentane
10. Benzene
11. 2-Methylhexane
12. 3-Methylhexane
13. 2,2,4-Trimethylpentane
14. n-Heptane
15. 2,5-Dimethylhexane
16. 2,4-Dimethylhexane
17. 2,3,4-Trimethylpentane
18. Toluene
19. 2,3-Dimethylhexane
20. Ethylbenzene
21. m-Xylene
22. p-Xylene
23. o-Xylene
Theory of Operation
Velocity
Carrier gas
Detector
(flame
ionization
detector or
FID)
Air
Hydrogen
Column
Oven
front view
Flame
Ionization
Detector
Coaxial cable
to Analog to
Digital
Ionsconverter
Flame
Platinum jet
Air
Hydrogen
Capillary tube (column)
Why do we need
hydrogen?
Responds
all
organic compounds
Little
Linear
Peak
time (s)
Other Detectors
Thermal
Conductivity Detector
Difference
Capture Detector
Specific
methane
time
ECD
output
Mixture containing
lots of methane
and a small
amount of TCE
FID
output
TCE
time
Mass Spectrophotometer
Uses the difference in mass-to-charge ratio (m/e) of
ionized atoms or molecules to separate them from each
other.
Molecules have distinctive fragmentation patterns that
provide structural information to identify structural
components.
The general operation of a mass spectrometer is:
mass-to-charge ratio
N2
Trap