DATASHEET EXPERIMENT 5

GAS CHROMATOGRAPHY (GC)

Name and Student ID 1. Nurul Ain Binti Azni (2020847984)

2. Nurul Ashikin Adila binti Nor Katini (2020817628)
3. Syaura Nurmizan Qistina Binti Sumadee (2020826604)
4. Amirah Sofiya Binti Anis (2020815282)

Date 30/11/2022

Group A4AS1205_13 (C)

Name and Model Gas Chromatography - Flame Ionization Detector

instrument Agilent / 7890b

Temperature (°C) Compounds Retention time, tR (min)

70 Standard mixture 2.985 6.471

70 2-Propanol 3.011

70 n-butanol 6.670

70 Unknown sample 6.670 -

100 Standard mixture 2.273 3.258

140 Standard mixture 1.957 2.216

Unknown number: 1
INTRODUCTION

Complex compound combinations are separated by chromatographic analysis. Chromatography,

which was first applied in the early 1900s, gained its name from the fact that it was used to
separate various mixes of coloured substances. Chemists began to use chromatography more
frequently in the 1930s when they discovered that it could be used to separate mixtures of
colourless chemicals. There are two phases in any chromatographic system: a mobile phase and a
stationary phase. A sample is transferred through a solid stationary phase by a liquid or gas
known as the mobile phase. Due to variations in the mixture's affinities for the stationary phase
and solubilities in the mobile phase, the compounds will separate as the sample in the mobile
phase passes through the stationary phase.

The eluted compounds in chromatographic analysis are identified by their retention times,
or tR. Determining the tR of analytes and comparing them to the tR of standards are steps in
qualitative analysis. Comparing the areas of the analyte peaks with those of standards allows for
quantitative analysis.

OBJECTIVES

1. To determine the retention times tR of n-butanol and 2-propanol.

2. To identify the components present in a standard mixture based on the tR.
3. To identify the component(s) present in an unknown sample.
4. To determine the effect of temperature on tR and Rs.
PROCEDURE

A. Experimental
GC instrument turned on and the GC instrument was set using the following conditions: Initial
oven temperature: 70°C, final oven temperature: 70°C, injection temperature: 180°C, and
detector temperature: 180°C. The component samples then were injected and the retention time
of each component was determined. Next, the standard mixture was injected and each
component present was identified by comparing the retention time of each component with the
retention time of each single component determined previously. Lastly, the unknown sample was
injected and the component(s) present in the unknown was identified.

Next, the column temperature changed as follows: Initial column temperature: 100°C,
final column temperature: 100°C. The standard mixture was injected and the effect of reducing
the temperature on the retention time and Rs of the components were observed. Lastly, the oven
temperature also changed as follows: Initial column temperature: 140°C, final column
temperature: 140°C, and then the standard mixture injected and the effect of increasing the
temperature on the retention time and Rs of the components were observed.

B. Operation of the GC
Instrument: Agilent 7890
Firstly the ‘File’ icon was clicked, followed by ‘Load’, and ‘Method’. Next, ‘Run control’ icon
was clicked, ‘viol location’ icon chosen and the location changed into ‘Viol 101’ for standard
mixture at 140°C. The sample name was changed into ‘Standard Mixture’ and comment changed
into ‘To determine the retention time of standard mixture at 140’. After that, the ‘Run’ button
clicked followed by the ‘print’ button. Then, the sample in the right location was injected by the
instrument syringe and waited for 8 minutes for the chromatograph. Step 2-4 were repeated for
the next samples; Viol 102 for 2-propanol, Viol 103 for n-butanol, and Viol 104 for unknown
sample.

RESULTS
PRE-LABORATORY QUESTIONS

1. Define the volatile compound, retention time, resolution.

Volatile compound is a compound that has a high vapor pressure and lower water
solubility. Retention time is the time that a solute spends in a column. Resolution is a
measure of the separation of two peaks of different retention time, t in a chromatogram.

2. Find the boiling points of n - butanol and 2-propanol.

n-butanol : 117.7 C

2-propanol : 82.5 C

3. Predict which compound, n-butanol and 2-propanol will elute first in a GC analysis.
Explain your answer.

2-propanol will elute first because it has a lower boiling point than n-butanol. This is
because the 2-propanol takes less time and heat in order to convert to gas which is
necessary for its effective analysis through gas chromatography.

QUESTIONS

1. State the types of compounds which are suitable for analysis using GC.

Halogenated, organic and inorganic compounds.

2. Why is FID a suitable detector for this analysis?

FID is a suitable detector for this analysis because it is a general detector for organic
compounds. The compounds that have been used in this experiment are n-butanol and
2-propanol. FID able to detect at the nanogram level.
 3. List two factors which can increase the efficiency of a GC column.

The two factors that can increase the efficiency of a GC column are column packing and
the particle size of the absorbance.

DISCUSSION

A gas chromatography analysis has been conducted to measure the compound in a

sample. Each of the compound in the sample has their own retention time depending on its
chemical composition. Retention time is the period of time a substance remains on the column
after it has been injected. The detector will measure the quantity of compounds that exits the
column. One of the factors that will affect the retention time is the column temperature. The
higher the temperature, the shorter the retention time.

There are four chemicals that have been tested with a different temperature. The
chemicals used in this experiment are 2-propanol, n-butanol, an unknown sample and a standard
mixture of 2-propanol and n-butanol. At 70°C the retention time is between 2.985 and 6.471 min.
For the 100°C, the retention time is 2.273 and 3.258 min and lastly for the 140°C, the retention
time is 1.957 and 2.216 min. Based on the data obtained from the chromatograms of the
standard mixture at 70, 100 and 140 °C, it can be interpreted as the higher the temperature, the
shorter the retention time between the two peaks.

Next, the 2-propanol and n-butanol have been analyzed at the same temperature which is
70°C. These two compounds will act as a batch mark when comparing the result of an unknown
sample. The retention time for 2-propanol is 3.011 min while n-butanol is 6.670 min. At the
unknown sample, it has been determined that the components present in an unknown sample is
n-butanol because it has the same retention time with the compounds. In the chromatograms
obtained, there are some of them that have another short peak except the sample used. This may
have occurred due to the sensitivity of the detector when reading the sample.

The detector that has been used in chromatographic analysis is flame-ionization detector.
It works for organic compounds and has high sensitivity with a large dynamic range. The
possibilities of that may cause an error in the result is when handling the sample. To solve the
problems, the samples must be handled carefully.

CONCLUSIONS

The retention time of n-butanol is 6.670 (min) meanwhile 2-propanol is 3.011 (min). The
components that are present in the standard mixture are n-butanol and 2-propanol. The
component that is present in an unknown sample is n-butanol because the unknown sample has
the same retention time with n-butanol.
As the temperature increases, the retention time will decrease and the resolution will also
decrease.

REFERENCES

Aryal, S. (2022, March 1). Gas Chromatography- Definition, Principle, Parts, Steps, Uses.

Microbe Notes. https://microbenotes.com/gas-chromatography/

Mathias, J. (2019, January 14). A Beginner’s Guide: How to Interpret Gas Chromatography

Mass Spectrometry Results. Innovatech Labs.

https://www.innovatechlabs.com/newsroom/1841/how-to-interpret-gas-chromatography-

mass-spectrometry-results/