SIC2022
LAB REPORT ANALYTICAL CHEMISTRY 1
EXPERIMENT 6
TITLE INTRODUCTION TO GAS CHROMATOGRAPHY
NAME SITI SARAH BINTI ABD SAMAD
ID NUMBER 23005996
DATE OF EXPERIMENT 18 DECEMBER 2024
INSTRUCTOR AP DR MUGGUNDHA RAOOV
PARTNER’S NAME NUR ALIAH BINTI ABDUL JALIL (23005941)
Experiment 6
INTRODUCTION TO GAS CHROMATOGRAPHY
Introduc�on
Chromatography involves separa�ng a mixture of analytes according to their par��oning between a
sta�onary phase and a mobile phase. Gas chromatography (GC) is a very powerful and one of the most
common instrumental analysis techniques in use. When properly u�lised, it provides both qualita�ve
(i.e., what is it?) and quan�ta�ve (i.e., how much?) informa�on about individual components in a
sample. The mobile phase of GC is an inert carrier gas (e.g. nitrogen, helium, hydrogen, etc) and the
sta�onary phase is found in the column. The gas chromatograph used in this experiment is equipped
with a capillary column.
The sample (dissolved in organic solvent) is injected onto the GC through a septum into a heated
injec�on port. The temperature of the injector is selected so as to vaporize the sample upon injec�on.
The sample vapour is then carried through the column by the carrier gas. As they interact with the
sta�onary phase to varying degrees, they are separated. With nonpolar sta�onary phases, the
principal determining factor as to rela�ve reten�on �mes on the column is the vola�lity of the
analytes. Therefore, the elu�on order is o�en es�mated using the boiling points of the analytes. The
detector temperature is chosen to be at least 20°C higher than the highest boiling point, in order to
ensure all analytes are detected as gases. To get a beter and more efficient separa�on of analytes,
temperature programming is o�en employed. The temperature of the column is raised during the
course of the analysis.
BTEX refers to benzene, toluene, ethylbenzene and xylenes. BTEX are an important class of vola�le
environmental contaminants, and are frequently analyzed in environmental and drinking waters.
Regula�ons o�en require that all waste entering the municipal sewer system contain no more than 1
mg/L. In this experiment, BTEX will be quan�fied using the external standardiza�on technique.
Objec�ves
1. To separate the components of standard BTEX, toluene, p-xylene, o-
xylene and ethylbenzene via gas chromatography.
2. To determine the concentra�on of each component of BTEX in an
unknown sample by using standard calibra�on curves.
Results and Discussions
Table 1: Concentra�on BTEX standard solu�on (ppm) and the volume used of BTEX stock
solu�on (ppm)
Concentra�on of BTEX standard solu�on Volume used of BTEX stock solu�on (𝜇𝜇𝜇𝜇)
(ppm)
10 20
20 40
30 60
40 80
50 100
To calculate the volume used of BTEX stock solu�on, use the formula of:
M1V1 = M2V2
A) Determina�on of Calibra�on Curves for Each Components of Standard BTEX via Gas
Chromatography
Table 2: Concentra�on and peak area of toluene
Concentra�on (ppm) Peak Area
10 2114
20 2794
30 3967
40 5941
50 7033
Figure 1: The linear graph of peak area against concentra�on for toluene
Toluene
8000
7000
6000
Peak area
5000
4000
3000 y = 129.85x + 474.3
R² = 0.9749
2000
1000
0
0 10 20 30 40 50 60
Concentration (ppm)
Table 3: Concentra�on and peak area of ethylbenzene
Concentra�on (ppm) Peak Area
10 2367
20 2919
30 4288
40 6240
50 7284
Figure 2: The linear graph of peak area against concentra�on for ethylbenzene
Ethylbenzene
8000
6000
Peak area
4000
y = 131.55x + 673.1
2000
R² = 0.9722
0
0 10 20 30 40 50 60
Concentration (ppm)
Table 4: Concentra�on and peak area of p-xylene
Concentra�on (ppm) Peak Area
10 2452
20 3155
30 4353
40 6435
50 7332
Figure 3: The linear graph of peak area against concentra�on for p-xylene
p-xylene
8000
7000
6000
5000
Peak area
4000
3000 y = 130.4x + 833.4
2000 R² = 0.9723
1000
0
0 10 20 30 40 50 60
Concentration (ppm)
Table 5: Concentra�on and peak area of o-xylene
Concentra�on (ppm) Peak Area
10 2059
20 2698
30 4361
40 6338
50 7250
Figure 4: The linear graph of peak area against concentra�on for o-xylene
o-xylene
8000
7000
6000
5000
Peak area
4000
3000 y = 140.22x + 334.6
2000 R² = 0.9754
1000
0
0 10 20 30 40 50 60
Concentration (ppm)
Based on the experiment, four calibra�on curves of each component of standard BTEX, toluene,
ethylbenzene, p-xylene, and o-xylene are ploted. The y-axis of the calibra�on curve is peak area while
the x-axis is the concentra�on of the standard BTEX. The peak area of each component of BTEX is
obtained from gas chromatography.
From the Figure 1 un�l 4, it shows the peak area is directly propor�onal to its concentra�on. Meaning
that, as the concentra�on of the substance is increased, the peak area obtained from the gas
chromatography will increase. This is because in high concentra�on, more molecules will enter the
detector per unit �me which will result in larger peak areas.
Chromatograms of the analysis of 10 ppm, 20 ppm, 30 ppm, 40 ppm and 50 ppm standard
BTEX solu�on
Figure 5: Chromatograms of the analysis of 10 ppm standard BTEX solu�ons
Figure 6: Chromatograms of the analysis of 20 ppm standard BTEX solu�ons
Figure 7: Chromatograms of the analysis of 30 ppm standard BTEX solu�ons
Figure 8: Chromatograms of the analysis of 40 ppm standard BTEX solu�ons
Figure 9: Chromatograms of the analysis of 50 ppm standard BTEX solu�ons
The chromatograms obtained from the gas chromatography explains the first peak shown indicates
the substance in a compound that has much lower boiling point compare to the others. As we know,
BTEX contains of four components such as toluene, ethylbenzene, p-xylene and o-xylene. Compound
with lowest boiling is toluene (110.60 ℃), followed by ethylbenzene (136.00 ℃), p-xylene (138.40
℃)and o-xylene (144.40 ℃). Thus, first peak shows the toluene, second peak is for ethylbenzene, third
peak is p-xylene and the last peak is o-xylene.
B) Determina�on of The Peak Area for Each Components of BTEX in the unknown C sample.
Table 6: Peak Area and concentra�on of each component of BTEX in the unknown C sample.
Component Concentra�on (ppm) Peak Area
Toluene 24.8802 3705
Ethylbenzene 23.2223 3728
p-xylene 21.8604 3684
o-xylene 24.2861 3740
Figure 10: Chromatograms of the analysis for unknown C
Calcula�on:
Concentra�on of toluene
Based on Figure 1,
y = 129.85x + 474.3
When y = 3705,
3705 = 129.85x + 474.3
x = 24.8802
∴ Concentration of Toluene in BTEX is 24.8802 ppm
Concentra�on of ethylbenzene
Based on Figure 2,
y = 131.55x + 673.1
When y = 3728,
3728 = 131.55x + 673.1
x = 23.2223
∴ Concentration of ethylbenzene in BTEX is 23.2223 ppm
Concentra�on of p-xylene
Based on Figure 3,
y = 130.4x + 833.4
When y = 3684,
3684 = 130.4x + 833.4
x = 21.8604
∴ Concentration of p-xylene in BTEX is 21.8604 ppm
Concentra�on of o-xylene
Based on Figure 4,
y = 140.22x + 334.6
When y = 3740,
3740 = 140.22x + 334.6
x = 24.2861
∴ Concentration of o-xylene in BTEX is 24.2861 ppm
Gas chromatography is an analy�cal technique used to separate the component of a sample mixture
and to detect their presence and absence in the sample (Thet & Woo, 2020). The separa�on of the
component in a sample mixture depends on the differences in behaviour between a flowing mobile
phase and sta�onary phase (Helmens�ne, 2019). The mobile phase and the sta�onary phase of gas
chromatography are inert gas and liquid respec�vely. Gas chromatography consists of five components
which are sample injec�on unit, column, column oven, detector and data processing unit. There is a
lot of different types of detectors such as mass spectrometer (MS), flame ioniza�on (FID), thermal
conduc�vity (TCD), electron-capture (ECD), atomic emission (AED), chemiluminescence (CS), and
photoioniza�on (PID) (Menon, 2021). In this experiment, the detector used is FID. Figure 11 shows the
schema�c diagram of gas chromatography.
Figure 11 shows the schema�c diagram of gas chromatography
By using gas chromatography, the concentra�on of the individual component is presented in electrical
signals. Then, the processor will convert the electrical signal into a chromatogram. The higher the
concentra�on of the component, the higher the peak presented in the chromatogram. Each of the
component of BTEX will produce a peak at different reten�on �me. Reten�on �me is the �me taken
for a component to pass through the chromatography column and it is depended on the boiling point
of the component. The boiling points of toluene, ethylbenzene, p-xylene and o-xylene are 110.60 ̊C,
136.00 C ̊ , 138.40 ̊C and 144.00 C
̊ . Therefore, the reten�on �me for toluene is the smallest while the
reten�on �me for o-xylene is the largest.
Based on Figures 5, 6, 7, 8 and 9, there is four peaks represent the each of the component of BTEX.
The peak at reten�on �me around 9.6 min to 9.9 min is the peak for toluene, at reten�on �me around
11.7 min to 12.1 min the peak is represented ethylbenzene, at reten�on �me around 11.9 to and 12.3
min the peak is for p-xylene and at reten�on �me around 12.4 to 12.8 min the peak represents o-
xylene. The components contain in the unknown sample is determined by comparing the reten�on
�me of the unknown sample with the reten�on �me of the standard.
From the analysis, total number of peaks shown was four indicates four components, so there is no
other compound or impuri�es that may cause extra number of peaks. However, the overall
chromatogram obtained shows the sample prepared was slightly dirty since it has rough surface. To
increase the quality of the experiment, some precau�on steps will be taken. First, the micropipete
used is always pointed downwards to prevent the chemical from flowing in the piston part and causing
damage. Second, before tested the BTEX next solu�on, the microsyringe is washed by solvent which is
hexane and rinse by using the sample first to obtain more accurate result by preven�ng any
contamina�on of the BTEX solu�on. Third, during the prepara�on, all the apparatus used are dried
and free of water to avoid the injec�on of BTEX solu�on into the gas chromatography contains any
water molecule that will interrupt the results.
Conclusion
The concentra�on of toluene, ethylbenzene, p-xylene and o-xylene in the unknown sample obtained
in this experiment are 24.8802 ppm, 23.2223 ppm, 21.8604 ppm and 24.2861 pm respec�vely.
Ques�on
Discuss the advantage of temperature program (ramping) over isothermal separa�on.
Advantage of temperature program (ramping) over isothermal separa�on are wide boiling point range.
Temperature programming is ideal for separa�ng mixtures with components that have significantly
different boiling points. Low-boiling-point compounds elute quickly at lower temperatures, while high-
boiling-point compounds are eluted as the temperature increases, improving resolu�on across the
range. Other than that, it can reduced the overlapping peaks. In isothermal separa�on, components
with close boiling points may co-elute if the temperature is not op�mized. Temperature ramping
minimizes this risk by allowing beter resolu�on of closely elu�ng peaks.
References
1. SIC2022 Basic Analy�cal of Chemistry, Lab Manual, Dept of Chemistry, Faculty of Science,
Universi� Malaya.
2. Helmens�ne, A. M. (2019, October 14). Gas chromatography - What it is and how it works.
Retrieved, December 01, 2021 from htps://www.thoughtco.com/gas-chromatography-
4138098
3. Menon, G. (2021, January 16). Detectors forgas chromatography. Retrieved, December 01,
2021 from htps://www.linkedin.com/pulse/detectors-gas-chromatography-
4. Thet, K. & Woo, N. (2020, August 16). Gas chromatography. Retrieved, December 01, 2021
from
htps://chem.libretexts.org/Bookshelves/Analy�cal_Chemistry/Supplemental_Modules_(Ana
ly�cal_Chemistry)/Instrumental_Analysis/Chromatography/Gas_Chromatography
