Environmental Chemistry (ENE-213)

Course Instructor: Dr. Sofia Baig

Lab Report-11

Gas Chromatography

Submitted To: Engr. Muhammad Irfan

Submitted By: Group-01

Arafat Abdullah Rehman

Faras Ahmad Shahbaz
Muhammad Momin
Haniya Zainab Siddique

National University of Sciences &Technology (NUST)

School of Civil & Environmental Engineering (SCEE)
Institute of Environmental Sciences & Engineering (IESE)

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Contents
Objective ................................................................................................................................... 3
Theory ....................................................................................................................................... 3
Principle .................................................................................................................................... 6
Environmental Significance .................................................................................................... 6
Apparatus and Chemicals Used.............................................................................................. 6
Procedure .................................................................................................................................. 6
Precautions……………………………………………………………………………………7
Note............................................................................................................................................ 7
Conclusion ................................................................................................................................ 7
References ................................................................................................................................. 7

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Title: Gas Chromatography

Objective:

The main objective to perform this experiment is to understand the concepts regarding gas
chromatography. We will be able to know how to find and analyze the components of a
mixture. Different applications of gas chromatography will be studied along with their
environmental importance. Presentation of results after the experiment is also one of the
objectives of this experiment.

Theory:

Chromatography
Chromatography’ is an “Analytical Technique” commonly used for separating a mixture of
chemical substances into its components, so that the individual components can be thoroughly
analyzed.

Types:
Types of chromatography are:

 Liquid chromatography
 Gas chromatography
 Ion-exchange chromatography
 Affinity chromatography

Gas Chromatography:
“Gas chromatography is an analytical technique used to separate the chemical components of
a sample mixture by using a gaseous mobile phase.”
It involves a sample being vaporized and injected onto the head of the chromatographic
column. The sample is transported through the column by the flow of the inert, gaseous mobile
phase. The column itself contains a liquid stationary phase which is adsorbed onto the surface
of an inert solid.

Types of Gas Chromatography:

The two major types of gas chromatography:

 Gas-solid chromatography:
Here, the mobile phase is a gas while the stationary phase is a solid. Used for separation of low
molecular gases, e.g., air components, H2 S, CS2, CO2, rare gases, CO, and oxides of nitrogen.

 Gas-liquid chromatography:
The mobile phase is a gas while the stationary phase is a liquid retained on the surface as an
inert solid by adsorption or chemical bonding.

Rf Value:
In chromatography, the retardation factor (R) is the fraction of an analyte in the mobile phase
of a chromatographic system. In planar chromatography, in particular, the retardation factor
RF is defined as the ratio of the distance traveled by the center of a spot to the distance
traveled by the solvent front.

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Mobile phase or carrier:
Solvent moving through the column.
Stationary phase or adsorbent Substance:
It is the substance that stays fixed inside the column.
Eluent Fluid:
It is the fluid entering the column (Carrier Gas).
Eluate Fluid:
It is the fluid exiting the column (that is collected in flasks).
Elution:
It is the process of washing out a compound through a column using a suitable solvent.
Analyte Mixture:
It is the mixture whose individual components have to be separated and analyzed.

Carrier gas:
The cylinder/ gas tank is fitted with a pressure controller to control the pressure of the gas, a
pressure gauge that indicates the pressure, a molecular sieve to transfer filtered dry gas, and a
flow regulator to ensure a constant rate of flow of mobile phase to the column.
It should meet the following criteria:
 Should be chemically inert,

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 Should be cheap and readily available,
 Should be of high quality and not cause any fire accidents,
 Should give best possible results,
 Should be suitable for the sample to be analyzed and for the detector.
Sampling unit:
 A sampling unit or injection port is attached to the column head.
 Since the sample should be in the vaporized state, the injection port is provided with an
oven that helps to maintain its temperature at about 20-500 C above the boiling point of
the sample.
 Gaseous samples may be introduced by the use of a gas-tight hypodermic needle of 0.5-
10 ml capacity.
 For Liquid samples, micro syringes of 0.1-100µL capacity may be used.
Column unit:
Columns are of different shapes and sizes that include: “U” tube type or coiled helix type. They
are mainly made of copper, stainless steel, aluminum, glass, nylon, and other synthetic plastics.
Support material:
Its main function is to provide mechanical support to the liquid phase. have a large surface
area, chemically inert, An ideal support should get uniformly wet with the liquid phase, should
be thermostable. Commonly used solid phases are diatomaceous earth, glass beads, porous
polymers, sand, etc.
Types of columns:
The types of columns are:
1. Packed columns:
In GLC, they are densely packed with finely divided, inert, solid support material (
diatomaceous earth) coated with a liquid stationary phase. In GSC, the columns are packed
with adsorbents or porous polymers. Length- 1.5 - 10m and internal diameter- 2 - 4mm.

2. Capillary columns-
Its length ranges from 10-100 m and its inner diameter is usually 0.1-0.5 mm. It is mainly of
two types:

 Wall-coated columns:
It consists of a capillary tube whose walls are coated with a liquid stationary phase.

 Support-coated columns:
The inner wall of the capillary is lined with a thin layer of support material such as
diatomaceous earth, onto which the stationary phase has been adsorbed. It is also known as
PLOT (porous-layer open tubular columns). SCOT columns are generally less efficient than
WCOT columns. Both types of capillary columns are more efficient than packed columns.
Detectors:
The eluted solute particles along with the carrier gas exit from the column and enter the
detector. The detector then produces electrical signals proportional to the concentration of the
components of the solute. The signals are amplified and recorded as peaks at intervals on the
chromatograph.

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Principle:
The principle of separation in GC is “partition.” The mixture of the component to be
separated is converted to vapor and mixed with the gaseous mobile phase. The component
which is more soluble in the stationary phase travels slower and is eluted later. The
component which is less soluble in the stationary phase travels faster and eluted out first.
No two components have the same partition coefficient conditions. So the components are
separated according to their partition coefficient. The partition coefficient is “the ratio of
solubility of a substance distributed between two immiscible liquids at a constant
temperature.’

Environmental Significance:

 It is used for determining trace organic compounds in environmental samples.

 Nowadays, gas chromatography (GC) continues to play an important role in the
identification and quantification of ubiquitous pollutants in the environment.

Apparatus and Chemicals Used:

 Carrier gas He (common), N2, H2, Argon
 Sample injection port microsyringe
 Columns
 Detectors
 Electron capture detector(ECD)
 Flame Ionization Detector (FID

Procedure:
 Fill the syringe with the sample.
 Record the setting i.e., column temperature, detector temperature, and injection port
temperature.
 Introduce the sample into the injection port by completely inserting the needle into the
rubber septum. Note down the injection time.
 The sample gets vaporized due to the higher temperature of
 the injection port and is swept into the column by the carrier gas.
 These sample components now get distributed between the gas and stationary liquid phase
depending upon their solubilizing tendencies.
 The components with minimal solubility move faster and those with maximum solubility
travel slowly.

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 The components leaving the column activate the detector and recorder to give a plot.

Precautions:
Specific precautions for working with gas chromatographs include:
 Perform periodic visual inspections and pressure leak tests of the sampling system
plumbing, fittings and valves.
 Turn off and allow heated areas such as the oven, inlet and detector, as well as connected
hardware, to cool down before touching them.
 Turn off the hydrogen gas supply at its source when changing columns or servicing the
instrument.
 To avoid electrical shock, turn off the instrument and disconnect the power cord at its
receptacle whenever the access panel is removed.

Note: No observations & calculations because we didn’t performed it in laboratory.

Conclusion:

We can conclude that this experiment has much greater significance because this can be used
for both qualitative & quantitative analysis. One of its working is for pharmaceutical purposes
in Quality control & analysis of drug products like antibiotics, antivirals etc. Major applications
also include analaysis of food, pollutants, dairy products along woith separation &
identification of volatile materials.

References:

 https://link.springer.com/article/10.1007/BF00323092
 https://www.researchgate.net/publication/223157069_The_application_of_gas_chromato
graphy_to_environmental_analysis
 https://www.labmanager.com/lab-health-and-safety/11-gas-chromatography-safety-tips-
19204
 Ravi Shankar, textbook of pharmaceutical analysis
 Skoog. D.A, Holler. F.J; principles of instrumental analysis