Faculty of Engineering

Cairo University

Chemical Engineering department

1stYear

Report on

“Gas Chromatography”

Prepared by:
1. Ahmad Yousry Muhammad
2. Ameer Anass Muhammad
3. Hazem Mohamed Aly
4. Khaled Abdalnasser Mahmoud
5. Muhammad Salem Hamed
6. Tony Adel Nassif

Submitted to: Dr/ Shakinaz El-sherbiny

 Abstract
Have you ever tried to separate iron filings, salt and sand? You can use a magnet, water and a filter
paper to make this separation process. Generally, materials are separated according to differences in
their physical properties. So iron attraction to the magnet and salt solubility in water will allow us to
make the separation.

So how could we separate a mixture of methanol and methyl benzene?

In this report we will discover a technique of separation of components of complex mixtures (samples)
with the purpose of obtaining information about their molecular compositions and amounts. With the
difference in physical properties of the components of this mixture “Gas Chromatography” can be
applied to separate them qualitatively and quantitatively.
 TABLE OF CONTENTS

Abstract ………………………………………………………………………………………………………………………………….………. i

List of figures ………………………………………………………………………………………………………………………………...…iii

Introduction ………………………………………………….……………………………………………………………………………….… 1

GC Samples ………………………………………………..………………………………………………………………….………………..…2

The main components of GC.......................................................................................................................................…...2

GC Analysis Cycle..……...……………………………….…………………………………………………………………………….……….4

GC Limitations.……………………………………………………..………………………………………………………………….…………5

GC Advantages…………………………………………………………………………………………………………………………………...6

REFERENCES…………………………………………………………………………………………………………………………………….…7

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 LIST OF FIGURE

Figure 1 components of GC …………………………………………………………………………………………………………………..2

Figure 2 the injection port……………………………………………………….................................................................................2

Figure 3 the Column…………………………………………………………………………………………………………………………..…..3

Figure 4 the Detector……………………………………………………………………………………………………………………………..3

Figure 5 data system……………………………………………………………………………………………………………………………....3

Figure 6 Column separation…………………………………………………………………………………………………………………...4

Figure 7 Data analysis (Chromatogram)…………………………………………………………………………………..………….....5

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 INTRODUCTION

"Chromatography” is like a horse race on a muddy track. Some horses are better "mudders" than
others. Just as all the horses start together at the starting line, the horses that know how to run on a
muddy track pull ahead of the others, and the horses become separated.

“Chromatography”, quite simply, is a broad range of physical methods used to separate and (or) to
analyze complex mixtures. The mixture is dissolved in a fluid called the mobile phase, which carries it
through a structure holding another material called the stationary phase. The various constituents of
the mixture travel at different speeds, causing them to separate.

“Gas Chromatography” is the most common popular analytical technique in the world, virtually; all
major companies have GCs available for research and quality control, it’s a kind of Chromatography
by using gas as a carrier in the mobile phase. The fundamental limitation of GC is simple volatility; GC
samples must be able to be vaporized within the temperature limits of the GC heated zones so that
they can be carried by the gas chosen to be the carrier in the mobile phase.
GC samples:
The GC is used to analyze samples from many different industries for quality control and for research,
it can be applied on many kinds of samples; Solids, Liquids or Gasses.
 Gasses: Natural gas, Petroleum gas, Air quality and Inert gasses.
 Liquids: Solvents, Gasoline, Alcohols and Glycols.
 Solids: Solvents from tablets and trace solids dissolved in solvents.

The GC sample must be volatile so it’s able to be vaporized and swept to the column by the carrier
gas flow.

The main components of GC:

Figure1 components of GC

1. The injection port:

The sample is injected here. From this injection port the
sample passes into the column which is kept in a
temperature-controlled oven.

2. Carrier gas: Figure 2 the injection port

From a pressure rise cylinder or a gas generator the carrier

gas is pumped, typically carrier gasses are; Helium, Hydrogen (with safety precautions),
Nitrogen or Argon. It’s preferred to be inert or very stable gas to avoid any reaction with the
mixture sample or the stationary phase in the column. The components of the mixture are
carried by a stream through the column by “the carrier gas (mobile phase).

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3. The Column:
The column is the heart of the GC, it’s temperature-controlled in an
oven, and it contains a very viscous liquid that’s called a “Stationary
phase” that’s used to separate the sample by physical properties
(Solubility-Boiling point). Some columns are over 30 meters long,
but the column is wound spirally to save space. The properties of

the column and its filling are chosen for the particular Figure 3 the Column
separation that is to be carried out.

4. The Detector:
The detector detects each component of the mixture as
it comes out of the column and also measures its
amount. There’re many types of detectors, each type of
detectors responds differently to compounds.
Examples:

1- FID: detects all organic compounds. Figure 4 the Detector

2- NPD: detects nitrogen and phosphorus compounds.

5. Data system:
A computer station is used to measure the amount of
each sample component as it passes through the
detector (Quantitative) and also to identify these
components based on “Retention time” (Qualitative).
Retention time (RT) is a measure of the time taken
for a solute to pass through a chromatography
column. It is calculated as the time from injection to
detection. Qualitative analysis relies on comparing
the retention times of each component in the unknown
Figure 5 data system
sample with those of known standards. If the retention
time of a component in the unknown sample is the same as the standard then a positive
identification can be made.

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GC analysis cycle:

1. Sample preparation:
It’s often the most time consuming step. Before beginning the separation, the operator must set the
flow rate of the carrier gases and the temperature of the oven. The temperature of the inlet port is
also set in a level that ensures the sample is fully vaporized and the detector must be lit.

2. Injection:
It involves rapid vaporization of the sample with mixing with the carrier gas to be introduced to the
column. Most commonly, liquids are analyzed by injecting them into the heated GC column through
the injection port using (5 to10) µl syringe. Gas can be injected using gas sampling valve. Solids can
be analyzed by extracting chemicals that are in the solid with a liquid solvent; (Think of making
coffee).

3. Column separation:
When the components of the mixture
are carried through the column in the
mobile phase, the more volatile the
component and the less it interacts
with the stationary phase, the faster it
travels through the column.

Figure 6 Column separation

4. Detection:
After the separation of the components, they’re individually measured in the GC detector that
converts some chemical or physical properties into electrical signals to by analyzed using a PC data
system.

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 5. Data analysis (Chromatogram):

The data system is used to receive signals from the GC

and use mathematical calculations to determine peak
areas, peak heights and retention times.
The retention time for each component is simply the
time between the point of injection and its peak.
The peak area is used to represent the concentration
of each component. Twice the concentration, twice the
peak area. Figure 7 Data analysis (Chromatogram)
The components of the mixture will reach the detector at varying
times due to differences in volatility. The first peak represents the most volatile component in the
mixture which is more abundant in the mobile phase.
Retention time is used for qualitative analysis, while peak height or area is for quantitative analysis.

GC limitations:
1. Samples must be volatile, as it’s limited to be vaporized in the oven temperature
limits.

2. “Dirty” samples require a clean up to avoid blocking or destroying the column.

3. We must use another instrument (e.g. Mass Spectrophotometer) for confirmation

of identity.

4. Some experience is necessary to obtain good results.

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GC advantages:

1. High resolution:

Many compounds can be resolved nicely, for example, Gasoline is been resolved to 300 different
peaks of very complex petroleum sample.

2. High speed:

Analysis takes few minutes to analyze the sample quantitatively and qualitatively. In the last few
years it can take few seconds.

3. High sensitivity:

We see both; rapid analysis as well as high sensitivity. In very small time interval, GC detects more
than one component, and detects very small amounts of components reaches to (a part per
billion).

4. High accuracy:

When we do quantitative analysis we get very good results.

5. Easy, Well known:

GC is widely one of the most used instruments today with very simple technique.

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 References

1- “Gas Chromatography” Blumberg 2012.

2- (1962) Gas Chromatography, Purnell H

3- Analytical Gas Chromatography (Second Edition)

Author(s): Walter Jennings, Eric Mittlefehldt and Philip Stremple

4- C. F. The Essence of Chromatography. Amsterdam, 2003 , POOLE

5- Principles and Practice of Modern Chromatographic

Methods.. Robards K, Haddad PR and Jackson PE (1994)

6- “Intermediate Chemical Experimentation”, MIT open courseware. No. (5.32), Spring

2003.

Instructor(s):

Dr. Mircea Gheorghiu (Laboratory Director).

Prof. Alexander Klibanov.