GAS CHROMATOGRAPHY

DR MD NAZMUS SAQIB
Department of Nutrition and Food Engineering
Daffodil International University
WHAT IS GAS CHROMATOGRAPHY? (GC)

Gas chromatography (GC) is an analytical technique applicable to gas, liquid, and solid samples
(components that are vaporized by heat). If a mixture of compounds is analyzed using GC system,
each compound can be separated and quantified.

Overview of GC Analysis

When a mixed solution sample is injected into the GC system, the compounds contained in
the sample, including the solvent components, are heated and vaporized within the sample
injection unit.
With GC system, the mobile phase, referred to as the carrier gas, always flows in sequence
from the sample injection unit to the column, and then to the detector. The target
components that were vaporized in the sample injection unit are transported by the carrier
gas to the column. Once in the column, the mixture of compounds is separated into the
various components, and the amount of each compound is then measured by the detector.
The detector converts the amount of each compound into an electrical signal, and sends
these signals to a data processing unit. The data obtained enables determination of the
compounds contained in the sample, and in what amounts.
Overview of GC Analysis
 GC SYSTEM CONFIGURATION
There are three main GC system components
•the sample injection unit, which heats the liquid sample and vaporizes it;
• the column, which is used to separate each compound; and
• the detector, which detects the compounds and outputs their concentrations as electrical
signals.
As shown in Figure , the GC consists of a fow control section, a
sample injection port, a column, a column oven, and a detector
in which is connected to a data processor. Carrier gases such as
helium (He), nitrogen (N ) or hydrogen (H ) are preferred to be
2 2

supplied at a constant fow rate to the sample to the injection

port. A separation tube called a column is connected between
the sample injection port and the detector, all three parts are
maintained at an appropriate temperature. The sample injected
into the sample injection port instantaneously vaporizes and
fows into the column with the carrier gas. In the column, a
liquid stationary phase (for example, silicone polymers) is
chemically bonded or coated, the vaporized sample is
repeatedly dissolved and vaporized in the liquid stationary
phase and travels downstream with the carrier gas.
 GC SEPARATION PROCESS

The sample containing multiple compounds is

injected into the column together with the mobile
phase. (In GC, the mobile phase is a gas referred to as
the carrier gas. He is frequently used.) Both the
sample and the mobile phase travel through the
column, but the rate of progression within the column
differs depending on the compound. Accordingly,
differences arise in the times at which the respective
compounds arrive at the column outlet. As a result, a
separation between each compound occurs.
The row of peaks drawn when the electrical signals
output from the GC detector are plotted on the
vertical axis and the elapsed time after sample
injection is plotted on the horizontal axis is called a
chromatogram.
The components passing through the column are
transported by the mobile phase (gas phase) while
being partitioned from and adsorbed into the
stationary phase (liquid phase and solid phase).
GC CHROMATOGRAM
A typical chromatogram is shown here. The horizontal axis shows the time until the component
reaches the detector. The vertical axis shows the signal intensity. The part at which nothing is
detected is called the baseline, and the part where a component is detected is called a peak. The
time from when the sample is injected into the system until the peaks appear is called the retention
time. As the elution times for each component differ, each component can be separated and
detected.
WHAT CAN BE ANALYZED BY GC
Compounds Suitable for GC Analysis
• Components that can be analyzed with GC have the following three main features.
• Compounds with a boiling point up to 400 °C
• Compounds that are not decomposed at their vaporization temperature
• Compounds that decompose at their vaporization temperature, but always by the same
amount. This is called pyrolysis GC.
Compounds That Cannot Be Analyzed or Are Difficult to Analyze with GC
• Compounds That Cannot Be Analyzed
• Compounds that do not vaporize (inorganic metals, ions, and salts)
• Highly reactive compounds and chemically unstable compounds
(hydrofluoric acid and other strong acids, ozone, NOx and other highly reactive compounds)
• Compounds That Are Difficult to Analyze
• Highly adsorptive compounds (compounds containing a carboxyl group, hydroxyl group,
amino group, or sulfur)
• Compounds for which standard samples are difficult to obtain (Qualitative and quantitative
analyses are difficult.)
.
CARRIER GAS
Carrier gas is an inert gas used to carry samples. Helium (He), nitrogen (N2), hydrogen (H2), and
argon (Ar) are often used. Helium and nitrogen are most commonly used and the use of helium is
desirable when using a capillary column. Carrier gas always fows into the detector, therefore it is
necessary to use one with a high purity (99.995 % or higher). In capillary columns, He is preferred
due to its ability to maintain the separating
resolution at high linear velocity (the speed at which sample travels through the column).
Requirements of a carrier gas
• Inertness
• Suitable for the detector
• High purity
• Easily available
• Cheap
• Should not cause the risk of fire
• Should give best column performance
THE COLUMN
Two types of columns are used in gas chromatography:
• packed columns and
• capillary columns.

• The GC user chooses the column based on certain attributes

such as; the target compounds, the number of components
and the instrument configuration.
• A smaller diameter and longer column is suitable if higher
resolution is needed, while a larger diameter column can be
used if higher resolution is unnecessary.
 THE COLUMN
Packed Column Stainless steel or glass
tube filled with particulate packing
material (an adsorbent material, or a
support material coated or impregnated
with a solid phase).
 THE COLUMN
Capillary Column A typical capillary
column is a thin, fused silica glass tube,
lined with a liquid phase or adsorbent
material or having a chemical bonding
layer. Thin metal tubes are also
sometimes used as capillary columns.
The outside is coated by polyimide resin to
increase the intensity. The column with 0.25
mm internal diameter and 30 m length is
frequently used.
THE COLUMN TYPE AND EFFECT ON SEPARATION

• Packed columns produce broad peaks and capillary columns

produce sharp peaks.
In addition, capillary columns produce taller peaks, which
allows the detection of lower concentrations (high detection
sensitivity). This is the advantage of capillary columns.
Sharper peaks provide better separation but also shorter
analysis times.
GENERAL GUIDE TO COLUMN SELECTION
General Guide to Selecting Polarity
•Selecting columns with polar properties that are close to the polarity of the
target compounds
•Analysis of non-polar compounds → Non-polar column
•Analysis of polar compounds → Strongly polar column
•Selection by analytical objective
•Large difference in boiling point between analytical target compounds
→ Non-polar column
•Isomers or other compounds with little difference in boiling points →
Strongly polar column

Guide to Selection of Internal Diameter, Length, and Coating Thicknes

•Selection based on required separation
•High-resolution separation required → Internal diameter: Thin, Length:
Long
•Adequate separation with shorter analysis time → Internal diameter: Factors Which Affect Separation in a GC
Thick, Length: Short, Coating thickness: Thin Column
•Selection by analytical objective
•Analysis of low boiling point compounds → Length: Long, Coating
thickness: Thick
•Analysis of high boiling point compounds → Length: Short, Coating
THE DETECTORS

They are broadly divided into general-purpose detectors

and selective, high-sensitivity detectors. General-purpose
detectors can analyze a wide range of compounds, of
which the flame ionization detector (FID) is the most
common because it can analyze almost all organic
compounds. In contrast, selective, high-sensitivity
detectors are only capable of detecting specific types of
compounds selectively and with high sensitivity.

Factors Which Affect Separation in a GC

Column
Features of GC Detectors. This table serve as a rough indication, it may be different depending on the compound chemical
structure and analytical condition

*The detection limits are approximations. Actual values will vary depending on the compound structure and analytical conditions.
FLAME IONIZATION DETECTORS (FID)
The FID is the most common detector used in gas
chromatography. The FID is sensitive to, and capable of
detecting, compounds that contain carbon atoms (C), which
accounts for almost all organic compounds. However, the FID is
not sensitive to carbon atoms with a double bond to oxygen,
such as in carbonyl groups and carboxyl groups (CO, CO2,
HCHO, HCOOH, CS2, CCl4, etc.).
Main Applications
•Organic compound analysis
Schematic Diagram of the FID
The FID creates a hydrogen flame by burning air and hydrogen
supplied from below. The carbon in a sample carried into the
detector on carrier gas is oxidized by the hydrogen flame,
which causes an ionization reaction. The ions formed are
attracted by a collector electrode to an electrostatic field,
where the components are detected.
SAMPLE INJECTION
Sample Injection Methods
Hot Injection
•Split: Most of the sample is eliminated as only a portion is injected
into the column.
•Splitless: Not split, but only for 1 to 2 minutes after injection
•Total volume injection (Direct injection): There is no splitting
mechanism.

Cold Injection
•Cold on-column injection (OCI)
•Programmed temperature vaporization (PTV)
Syringes
When injecting samples into a GC unit, a microsyringe is used for
liquid samples whereas a gas-tight syringe is used for gas samples.
SAMPLE INJECTION

Direct injection

Split injection

Cold injection
INDUSTRIAL APPLICATION OF GC
APPLICATION OF GC IN FOOD INDUSTRIES

1.Flavor Analysis: Identifying and quantifying volatile compounds for improved sensory
attributes.
2.Quality Control: Detecting contaminants like pesticides and additives to ensure food
safety.
3.Fatty Acid Analysis: Assessing nutritional content and quality of oils and fats.
4.Aroma Compounds in Spices: Analyzing spices for flavor profile enhancement.
5.Food Safety: Verifying compliance with regulatory standards for overall food safety.
6.Beverage Analysis: Characterizing and ensuring the quality of beverages through
ingredient analysis.
7.Residue Analysis: Detecting residues from processing or packaging, ensuring product
integrity.
8.Shelf Life Studies: Monitoring changes in food composition over time for shelf life
determination.
9.Authentication of Food: Verifying the authenticity of food products by analyzing
specific markers.
10.Process Optimization: Enhancing efficiency in food production processes through
analytical insights
GC VS HPLC
High-Performance Liquid
Aspect Gas Chromatography (GC) Chromatography (HPLC)
Separates non-volatile and semi-
Principle of Separation Separates volatile compounds.
volatile compounds.
Gaseous (usually inert gases like Liquid (commonly a mixture of water
Mobile Phase
helium). and organic solvents).
Usually a thin layer of liquid on a solid
Stationary Phase Solid particles or porous material.
support.
Example: Analysis of non-volatile
Example: Flavor analysis, detection
Application in Food Industry compounds like vitamins,
of volatile compounds in spices.
preservatives, and pesticides.

Well-suited for volatile and small Ideal for non-volatile, polar, and
Suitability for Compounds
molecular weight compounds. thermally unstable compounds.

Generally slower analysis time

Speed of Analysis Typically faster analysis time.
compared to GC.
High sensitivity for volatile High sensitivity for a wide range of
Sensitivity
compounds. compounds.
Requires samples to be in a gaseous Accepts liquid or solid samples
Sample State
state. dissolved in a solvent.
GC VS HPLC
Higher initial equipment cost, especially
Cost Generally lower initial equipment cost.
for high-pressure pumps.
Maintenance costs can be higher due to
Maintenance Cost Often lower maintenance costs.
complex instrumentation.
Provides high selectivity for a broad range
Selectivity Offers excellent separation for volatile compounds.
of compounds.
Sample preparation can be more complex,
Sample Preparation Generally simpler sample preparation.
especially for non-volatile compounds.

Well-suited for quantitative analysis of volatile Effective for quantifying a wide range of
Quantification
compounds. compounds in various matrices.

Robust for a broader range of compounds

Robustness Generally robust for volatile compound analysis.
but may require careful optimization.
Longer run times, especially for complex
Analysis Time Typically shorter run times.
samples.
Higher consumption of liquid mobile
Mobile Phase Consumption Lower consumption of mobile phase in gas form.
phase.
Column life may be shorter, especially in
Column Lifetime Generally longer column life.
the analysis of complex samples.
Lower solvent usage, potentially more Higher solvent usage may have a greater
Environmental Impact
environmentally friendly. environmental impact.
QUESTION ?

Video Reference
1. https://youtu.be/4Xaa9WdXVTM?feature=shared
2. https://youtu.be/UycPljfrnWo?feature=shared
3. https://youtu.be/X7J570KByC4?feature=shared
Reference
Basics & Fundamentals Gas Chromatography , application
Note Shimadzu Corporation