FACULTY OF APPLIED SCIENCES

CHM 571 - BASIC INSTRUMENTAL ANALYSIS

LAB REPORT

NAME: MOHAMAD SAIFUL BIN MOHD RAFFIAH

STUDENT ID: 2021459156
CLASS GROUP: AS239 4A
EXPERIMENT 2: GAS CHROMATOGRAPHY (GC)
LECTURER: DR. NORAINI BINTI KASIM
DATE OF EXPERIMENT: 12th APRIL 2022
DATE OF SUBMISSION: 14th JULY 2022
Tittle : Gas Chromatography

Objective
1. To determine the retention time of each compound individually
2. To identify the components present in a standard mixture
3. To identify the components present in an unknown sample
4. To investigate the effect of column temperature on the retention time
5. To study the effect of column temperature on the peak areas

Introduction
The group of analytical separation techniques used to analyse volatile compounds in the
gas phase is known as gas chromatography. By dividing the sample between two phases which
is a stationary phase and also a mobile phase. In gas chromatography, the components of a
sample are dissolved in a solvent and vaporized to separate the analytes. The analyte molecules
are transported through the heated column by the mobile phase, which is a chemically inert gas.
One of the only types of chromatography that does not use the mobile phase to interact with the
analyte is gas chromatography.
Gas chromatography's ability to efficiently separate substances depends on how quickly
the substances move along the column. There are few aspects that affect the way the GC system
performs. Volatility of the chemical is one of the considerations. The more volatile the component
is, the more rapidly it will elute compared to compounds with high boiling points. The GC column
temperature is the next topic. The chemical in the stationary phase separates more quickly the
higher the column's temperature. The separation is also impacted by the carrier gas flow rate; as
the carrier gas flow increases, the compound will move through the column more quickly. The
migration time of the analyte in a column increases with its length and increases the time required
for elution. The separation is also affected by the carrier gas flow rate; as the carrier gas flow
increases, the compound will move through the column more quickly. The migration time of the
analyte in a column increases with its length and increases the time required for elution. A longer
column however, will provide better separation.

Materials Provided
- 2-propanol, n-butanol
- Standard mixture; 2-propanol : n-butanol (50 : 50 v/v)
- Sample mixture with unknown quantities
Instrument
Gas chromatography (Agilent Technologies 6890N) equipped with flame ionization detector (FID)
and 30 m x 250 µm x HP5-MS capillary column

Procedures
1. The sample was prepared for calibration with various compositions. The amount of
isopropanol, n-butanol, standard mixture and unknown were fix equal to 0.4 L into the
instrument.
2. The instrument was set to 100 °C for each compound. Then, each of the compound were
injected individually and the retention times were recorded. For standard mixture the
temperature was set into two temperature which is 80°C for 6 minutes and 130°C for 2 minutes.
The chromatography of the standard mixture with different temperature were observed and
compared.
3. The sample should be volatile, thermally stable such as 2-propanol, n-butanol, standard
mixture and unknown solution. The sample was injected into the Gas Chromatography FID-
ECD (6890N- Agilent) until it vaporised.
4. The carrier gas must be chemically inert. The commonly used gases is nitrogen, helium, argon
and carbon dioxide. The inert gas goes through a glass column packed with silica that is coated
with a liquid. It contains a molecular sieve to remove water and other impurities.
5. The sample injection port is where a micro syringe is used to inject sample through a rubber
septum into a flash vaporiser port at the head of the column. It provides the means to introduce
a sample into continuous flow of carrier gas. The column can be packed or capillary. Packed
column contains finely divided, inert, solid support material and use carrier gas flow 10 - 40
mL/min.
6. The capillary column has internal diameter a few tenths of millimetre, it also has high resolution
time. The column temperature must be controlled to within tenths of a degree. The optimum
column temperature is dependent upon the boiling point of the sample.
7. The column temperature is increased as separation proceeds. The detector is very selective
to almost every compound that elutes from the column and it can be sensitive to a particular
type of compound. It is then interpreting in the computer.
Results
Data
Column Temperature 100°C
Retention time (min) Average Area
Sample Average
1 2 (min) 1 2
Isopropanol 1.833 1.831 1.832 11008.7 10336.1 10672.4
n-butanol 2.434 2.419 2.427 11252.8 11067.5 11160.2
The Retention Time and Area of Sample in 100°C Column Temperature

Retention Time (min) Area

Sample
Peak 1 Peak 2 Peak 1 Peak 2
Standard
1.831 2.427 46474.6 63992.9
Mixture 1
Standard
1.817 2.406 44107.8 60878.0
Mixture 2
Average 1.824 2.417 45291.2 62435.5
The Retention Time and Area of Standard Mixture 1 & 2 in 100°C Column Temperature

Retention Times (mins) Area

Sample
Peak 1 Peak 2 Peak 1 Peak 2
Unknown 1.828 2.425 22406.3 67648.8
Unknown 1.824 2.416 20760.2 63236.0
Average 1.826 2.421 21583.3 65442.4
The Retention Time and Area of Unknown Solution in 100°C Column Temperature

Column Temperature 80°C

Retention Time (min) Area
Sample
Peak 1 Peak 2 Peak 1 Peak 2
Standard
2.243 3.472 39926.7 58525.8
Mixture 1
Standard
2.237 3.462 45552.3 63456.1
Mixture 2
Average 2.240 3.467 42739.5 60991.0
The Retention Time and Area of Standard Mixture 1 & 2 in 80°C Column Temperature
 Column Temperature 130°C
Retention Time (min) Area
Sample
Peak 1 Peak 2 Peak 1 Peak 2
Standard
1.602 1.840 39087.4 49293.2
Mixture 1
Standard
1.602 1.844 45447.8 63692.3
Mixture 2
Average 1.602 1.842 42267.6 56492.8
The Retention Time and Area of Standard Mixture 1 & 2 in 130°C Column Temperature

Discussion
1. How do you determine the identity of the components in the sample mixture ?
- A GC system scans the samples continuously throughout the separation and ultimately the
chromatogram shows the retention times. The chromatogram peak is analyzed by the mass
spectrometer which leads to the identification of the separated components.
2. What is the effect column temperature on the retention times ?
- The column temperature increase will cause the retention times of the compounds that are
separated to decrease. This is due to the inlet pressure increase that accelerated the elution
of compounds because of a large pressure gradient between the column inlet and column
outlet.
Conclusion
The retention times of n-butanol and isopropanol in this experiment can be identified to be 2.427
min and 1.832 min respectively. Furthermore, by contrasting the retention time, tr the component
present in the standard mixture can be detected. The presence of the components was then
determined by comparing the tr of the unknown mixture to the tr of the standard mixture. The
retention time shown in the graph, when n-butanol and isopropanol were present in the
combination since the retention time was almost identical which can be used to determine the
current variable. Also, the temperature value has an impact on the solution's resolution Rs, with a
temperature reduction leading to an increase in Rs.
Reference

1. How Does Gas Chromatography Identify Compounds? (2021, April 6). AZoM.com.
https://www.azom.com/article.aspx?ArticleID=20279#:~:text=A%20GC%2FMS%20syste
m%20scans
2. Idroes, R., Muslem, Mahmudi, Saiful, Idroes, G. M., Suhendra, R., & Irvanizam (2020).
The effect of column and temperature variation on the determination of the dead
 time in gas chromatographic systems using indirect methods. Heliyon, 6(2), e03302.
https://doi.org/10.1016/j.heliyon.2020.e03302
3. Temperature Programmed GC: Why Are All Those Peaks So Sharp? (n.d.).
Chromatography Online. https://www.chromatographyonline.com/view/temperature-
programmed-gc-why-are-all-those-peaks-so-sharp-1