CHM 510 Exp 1
CHM 510 Exp 1
CHM 510 Exp 1
CHM510
STUDENT ID 2022855638
GROUP MEMBERS
1) NUR AMIRAH BALQIS BINTI MOHD KOSIM
(2022800388)
2) AINUL SYARAFANA BINTI SHAMSUL HAYAT
(20224942820)
3) NURATHIRAH NABIHAH BINTI SAIRI (20224942820)
4) NUR HIDAYAH MOHD NAJIB (2022
CLASS AS2452S1
Gas chromatography is a method of separating chemical compounds that uses variations in the
partitioning behaviour between a flowing mobile phase and a stationary phase to do so. For
hydrocarbons like butane or hexane, the flame ionisation detector (FID) is the most sensitive
gas chromatographic detector.
The sample solution is injected into the machine and then enters a gas stream that carries it into
a separation tube called a "column," according to the gas chromatography principle. The so-
called carrier gas is either nitrogen or helium. Inside the column, the different parts are divided.
The detector counts the components as they leave the column. An injection of a standard sample
with a known concentration into the instrument is necessary to measure a sample with an
unknown concentration. To determine the concentration, the test sample's peak retention time
and area are compared to the standard samples.
Compounds have to pass through the column at various rates in order for the GC to separate
them effectively. Considering the sample broadly is always the first step in developing a
method. Determining whether conditions are suitable or appropriate for the required analysis
is the process of developing a method. The volatility of the compound, the column temperature,
the velocity of gas flow through the column, the length of the column, column polarity, and the
polarity of the compound are some of the elements that affect GC separation. However, the
first four elements are the main focus of this experiment. Below are specifics for every aspect.
1. Volatility of compound
2. Column temperature
b. Objectives
To study the volatility of compound, the effect of the length of the column, the effect of column
temperature and flow rate by carrier gas through the column
c. Apparatus
b. Standard mixture of methyl laurate (0.20 mg mL-1), methyl myristate (0.20 mg mL-1) and
methyl palmitate (1.0 mg mL-1), methyl stearate (0.70 mg mL-1) and methyl linoleate (0.35
mg mL-1).
Instrument
Gas chromatograph (Agilent Technologies 6890N) equipped with flame ionization detector
(FID) and 30 m x 250 µm x 0.25 µm HP5- MS capillary column
Analytical Procedure
methyl esters.
1. 0.4 μL standard mixture was injected isothermally at 210˚C at carrier gas flow rate of
30 cm sec-1.
2. The flow rate was increased to 50 cm sec-1.
3. A few minutes for the system was allowed to equilibrate and the standard mixture was
injected again.
4. The same procedure was repeated at flow rate of 70 cm sec-1. Which flow rate is most
suitable for this separation?
190˚C, at the optimal carrier gas flow rate. The effect of column temperature was evaluated on
the separation, resolution, and analysis time.
2.. Methyl esters was separated using column temperature programming. Standard mixture was
injected at the optimal carrier gas flow rate using a linear temperature ramp from 100˚C to
290˚C at optimal flow rate. Comment on the separation of the compounds. If the resolution is
not adequate for your needs, attempt a modification to the temperature programming in order
to improve the resolution of the compounds.
3. Components in methyl esters mixture were identified. Each methyl ester was injected
individually to identify the various compounds in the standard mixture using the optimized GC
condition
D. Data and results
Calculation
2 (t R2 − t R1 )
Rs =
W1 + W2
Condition of 30cm sec-1 gas flow rate at 2100C
2 (6.120−4.385)
First injection: 𝑅𝑅𝑅𝑅 = = 21.7828
0.0683+0.0910
2 (6.142−4.401)
Second injection: 𝑅𝑅𝑅𝑅 = = 21.3227
0.0738+0.0895
21.7828−21.3227
Average 𝑅𝑅𝑅𝑅 = 2
= 21.5528
e. Discussion
As shown by the findings above, this can be used to show how changes in the mobile phase
flow rate at constant column temperature will impact the analytes' retention times in the
standard combination. Due to the carrier gas's diffusion, slower flow rates will result in better
analyte separation but relatively lengthy analysis times. While the analysis will be shortened at
larger flow rates, a broad peak will result from mass transfer as predicted by Van Deemter
theory. This occurs as a result of the analytes' incomplete interaction with the stationary phase.
In this experiment, the best separation is achieved at a flow rate of 70 m/s, which results in a
resolution of 21.5528. However, this resolution needs to be improved more till it is nearly at
the 1.5 acceptable resolution.
The retention period of the analytes in the standard mixture will also change depending on the
column temperature. Even if the mixture's analytes are better separated at lower temperatures,
analysis takes longer. The experiment's analysis time will be shortened and the peaks'
resolution will be closer to 1.5 if a higher temperature is employed. The best separation and
quickest analysis times in this experiment were achieved at a column temperature of 210oC.
Additionally, if the temperature is higher than the analytes' boiling points, the resolution will
be too low, which will result in overlapped analyte peaks in the mixture.
Based on the results of this experiment, a flow rate of 70 m/s and a column temperature of
210˚C were found to be the optimal conditions for running the analysis on the standard mixture.
It is known as optimum condition
f. Conclusion
A carrier gas flow rate of 70 m/s and a column temperature of 210˚C are ideal for the separation
of methyl esters. Methyl laurate is the first peak on the chromatogram, followed by methyl
myristate and methyl palmitate.
g. Reference
• Gas Chromatography- Definition, Principle, Parts, Steps, Uses
https://microbenotes.com/gas-chromatography/
• Gas Chromatography
https://chem.libretexts.org/Bookshelves/Analytical_Chemistry/Supplemental_Module
s_(Analytical_Chemistry)/Instrumentation_and_Analysis/Chromatography/Gas_Chro
matography
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