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GC Analysis
GC Analysis
Introduction
Figure 1.
Our laboratory setup is presented in Figure 2.
Figure 2.
Figure 3.
The effluent from the column is mixed with hydrogen and air, and ignited.
Organic compounds burning in the flame produce ions and electrons that can
conduct electricity through the flame. A large electrical potential is applied at
the burner tip, and a collector electrode is located above the flame. The
current resulting from the pyrolysis of any organic compounds is measured.
FIDs are mass sensitive rather than concentration sensitive; this gives the
advantage that changes in mobile phase flow rate do not affect the detector's
response. The FID is a useful general detector for the analysis of organic
compounds; it has high sensitivity, a large linear response range, and low
noise. It is also robust and easy to use, but it destroys the injected
sample.
After detection, a signal is sent to the recording device. You will see
the development of the curve on the computer screen (Figure 4.)
Figure 4.
The time between sample injection and an analyte peak reaching a detector
at the end of the column is termed the retention time (tR ). Each analyte in a
sample will have a different retention time. The time taken for the mobile
phase to pass through the column is called tM.
Laboratory procedure
Make sure that you read and understand the lab procedure.
Follow the safety procedure for the work in the lab.
Turn GC on. Let it warm up for about 15 minutes
Open up the valves on two rightmost reservoirs with compressed air
and Hydrogen.
Ignite the flame in FID by pushing and holding “Flame Ignite” bottom
on GC. You can see if it works by bringing a stainless steel surface (or
a mirror) into the contact with FID outlet. The surface will get foggy.
Make sure that the temperature is programmed to increase from 40 to
90 degrees.
Rinse the syringe in acetone and then in distilled water several times.
Be very careful. The syringe is very fragile and very expensive.
Start testing lower concentration of one-component liquids first. Then
go to higher concentrations, change to other compound and then to
mixtures.
Insert the needle into the testing vial through the lid. Don’t open the
vial.
Withdraw some liquid. Discard this liquid in the wastewater beaker.
Insert needle into vial again. Slowly withdraw 4 µl of liquid. Make sure
that you don’t have any air bubbles inside the syringe. The volume
must be precise.
Make sure that GC thermometer indicates it is at about 40 oC.
Start a new file.
Click on “0” bottom on the screen of the computer for Autozeroing.
Press “space” on the keyboard to start the run.
Inject testing fluid into Injector 2.
Wait 6-7 minutes.
Review the output curve. Click “results” at the bottom of the screen.
Write down type of the pollutant tested, concentration of the sample
and area under the curve calculated by the computer.
Save the file in the new folder.
Repeat the procedure for other samples.
When finished, close valves on air and hydrogen reservoirs. Turn GC
off.
Using Excel, draw the calibration curve.
Calibration curve:
C1 * V1 = C2 * V2
The final volume should be 25ml, so you have to get this amount of water
(i.e. 458 µl) out from the vial with pipette, and then add this amount of
toluene water back into the vial.
References
www.umd.umich.edu
www.shu.ac.uk