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Chm510 GC

The document describes an experiment to optimize gas chromatography conditions for separating a mixture of methyl esters. It varied (a) carrier gas flow rate at 210°C from 30m/s to 50m/s to 70m/s, (b) column temperature at a flow rate of 70m/s from 170°C to 190°C to 210°C, and (c) identified individual methyl ester compounds under optimized conditions. It was found that a gas flow rate of 70m/s and a column temperature of 210°C provided the best separation and shortest analysis time for the methyl ester mixture.

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Aishah Sam
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62 views2 pages

Chm510 GC

The document describes an experiment to optimize gas chromatography conditions for separating a mixture of methyl esters. It varied (a) carrier gas flow rate at 210°C from 30m/s to 50m/s to 70m/s, (b) column temperature at a flow rate of 70m/s from 170°C to 190°C to 210°C, and (c) identified individual methyl ester compounds under optimized conditions. It was found that a gas flow rate of 70m/s and a column temperature of 210°C provided the best separation and shortest analysis time for the methyl ester mixture.

Uploaded by

Aishah Sam
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© © All Rights Reserved
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EXPERIMENTAL:

a. Isothermal elution was set up with condition of:


Injection port: split (40:1)Injection port temperature: 250°CColumn temperature: varies
(170°C, 190°C, 210°C)Carrier gas flow rate: varies (30m/s, 50m/s, 70m/s)Detector
temperature: 250°C
b. Effect of carrier gas flow rate on isothermal GC separation of methyl ester:
1.
The standard mixture was injected with 0.4μL at 210°C isothermally and
30m/s of gas flow rate.2.
For the second injection with 0.4μL volume of standard mixture, the gas
flow rate was increased to 50m/s with same temperature of 210°C.3. The same procedure
was repeated with 70m/s gas flow rate.4. The resolution of 3 different flow rates at the same
temperature was calculated and compared to determine which gas flow rate give the better
separation of the compounds in the standard mixture.
c. Effect of column temperature on the isothermal GC separation of methyl ester:
1. By using the best gas flow rate from the above procedure, the same
standard mixture with 0.4μL was injected into the column isothermally at
170°C and followed by 190°C.2. The resolution of each chromatogram was calculated and
was based on the resolution and the analysis time.
d. Identification of components in methyl esters mixture:
1.
The standard individual methyl ester compounds were injected with 0.4μL
volume using the optimized GC conditions.2. The standard individual methyl ester
compounds are methyl laurate,methyl myristate, methyl palmitate, methyl stearate and
methyl linoleate.

Discussion
The variation of the mobile phase flow rate will affect the retention time of the compounds in
which slow mobile phase flow rate will give better separation but very long analysis time. In
contrast, high flow rate will shorten the analysis time but will cause broadening due to the
mass transfer (C-term) in Van Deemter plot, because the solute does not completely interact
with the stationary phase. To reduce the analysis time and to produce better separation, the
optimum gas flow rate must be used. In this experiment, the optimum mobile phase flow rate
is 70m/s that give good resolution of 6.33 compared to the others that are far from the ideal
resolution value that is 1.5. The column temperature also affects the separation resolution
and the analysis time. High column temperature will give short analysis time but some of the
earlier peaks may be overlapped while low column temperature produces better separation
but will take very long analysis time. The optimum column temperature must be used in
order to separate each compounds adequately. In this case, 210°C of column temperature is
the best temperature to separate each of the compounds.Based on this experiment, the best
condition to separate the methyl ester mixture by using 70m/s gas flow rate at 210°C column
temperature which give adequate separation between compounds and shorter analysis time.
Optimum flow rate and optimum column temperature will produce better separation,high
efficiency, good resolution and short analysis time for the separation. Since the separation of
gas chromatography is based on the boiling point of the compounds, it can be concluded
that methyl laurate has lowest boiling

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