Henry Su

Lab Experiment #5
12-1,3

May 8, 2003
CHE 331
Dr. Rahni

Determination of Optimum Flow Rate in Gas Chromatography

Resolution and Qualitative Identification of Hydrocarbons by Gas Chromatography
Purpose
The purpose of this laboratory experiment is to determine the optimum flow rate of
chloroform in gas chromatography, and also to measure the retention times of a homologous
series of hydrocarbons.
Theory
In order to have good separation of a given pair of components by gas chromatography,
the judicious selection of a column substrate, in both the solid and liquid phases, and the efficiency
of the overall GC system are taken into consideration. The relative position of the various
components in the sample on the chomatogram is affected by a solute-solvent type of interaction
with the column substrate. Solvent efficiency, or relative retention time, is expressed as a ratio of
the retention time of a solute to the retention time of a material that doesnt interact with the
liquid phase.
Most factors that affect column efficiency are evaluated by their effect on N, the number of
theoretical plates. The height of the theoretical plate is seen as H = L / N, where L is the length of
the column. N of a column can be determined as N = (4t R/Wb)2 . Losss in a number of theoretical
plates originates in three places:
1-Sample injection-The sample should be injected all at once in the column and should be
vaporized immediately. For this reason, some sample chambers are heated. The sample
should enter the packed column as a plug of gas without tailing.
2-Column characteristics-The column depends much on the proper flow rate. If flow rate
is increased, the effects of diffusional broadening will be diminished. At high temperatures,
partition equilibrium must also be considered.

3-Volume of Detector-One the band issues from the column, it should go immediately into
a small detector. This is especially important in the case of the sharp peaks that emerge
early from the column.
In order for a mixture to be separated successfully, the peaks from the individual components
must be resolved from each other. The extent of the separation of two adjacent, approximately
gaussian peaks, can be expressed in terms of the resolution R of a column.

Apparatus
The following materials will be needed in order to perform this experiment:

Material
Gas Chromatographer with Recorder
Tank of He (g) with pressure regulator
Timer
Soap bubble flow rate meter
Column: Dimethylsilicone SE-30
Syringe 10 ul

Quantity
1
1
1
1
1
1

Procedure
1-Connect the bubble flow rate meter to the gas exit port
2-Determine the flow rate by squeezing the soap bulb so that the soap goes above the gas inlet
side arm
3-Get two or three bubbles going up and use timer to check time it takes for bubble to go from 0
ml to 10 ml.
4-Set flow rate of the chromatograph
5-Obtain individual chromatograms of the pure hydrocarbons
6-Obtain chromatograms of unknowns
7-Obtain chromatogram of unleaded gasoline
Data and Calculations
None for this laboratory experiment.
Conclusion:
A theoretical view of gas chromatography has been discussed.
Discussion