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Principles and
Instrumentation
CDB 3093: ANALYTICAL CHEMISTRY
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Introduction
GC is is widely used for the determination of
organic/volatile compounds.
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Two types of gas chromatography (GC):
i. Gas-solid (adsorption) chromatography (GSC)
ii. Gas-liquid (partitioning) chromatography (GLC)
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The basic components of a typical instrument for
performing GC are:
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Instrumentation of GC
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Principles Operation of GC
Volatile liquid or gaseous sample is injected through a
septum into a heated port, in which it rapidly
evaporated.
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The sample is automatically detected as it emerges
from the column using a variety of detectors
whose response is dependent upon the composition
of the vapor.
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By measuring the retention time and comparing this
time with that of a standard of the pure substance, it
can identify the peak.
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Detector
Column
Sample Injection
GC Operation
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Modern Gas Chromatography System
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Carrier Gas System
The mobile-phase gas in GC is called carrier gas and
must be chemically inert.
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Carrier Gas System / Gas Supply
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Sample Injection System
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Sample Injection System
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• To achieve high column efficiency, the sample must
be of a suitable size.
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Autosampler
Syringes
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GC Columns
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GC Columns
Two types of columns used in GC are:
i. Packed column
ii. Capillary column (open tubular)
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i) Packed Column
The column contain a fine solid support coated with a
nonvalatile liquid stationary phase (partitioning
chromatography); or the solid itself may be the
stationary phase (adsorption chromatography).
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Small particle size of fine solid decreases the time
required for solute equilibration improve column
efficiency, but higher pressure required to force
mobile phase through the column.
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Glass Packed GC Column
Stainless Steel GC
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ii) Capillary Column (Open Tubular)
Most widely use.
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Compared with packed columns, open tubular
columns offer:
i. Higher resolution
ii. Shorter analysis time
iii. Greater sensitivity
iv. Lower sample capacity
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Capillary Columns
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Columns placed in the Oven
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Capillary Fused Silica Stationary Phases
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GC Detectors
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GC Detectors
After the components of a mixture are separated in
the chromatography column, they must be detected at
the outlet so that they can be identified and
measured.
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Thermal Conductivity Detector (TCD)
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Thermal Conductivity at 273 K , 1 atm
Molecular
Weight
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Eluate from the column flows over a hot filament.
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Flame Ionization Detector (FID)
Relies on the creation of ion/charged particles
produced from the sample/compound when they are
burnt by temperature in a flame.
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FID Detector
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In the absence of organic solutes, the current is
almost 0.
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Other Detectors
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Comparison of Gas-Chromatographic Detectors
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Characteristics of the Ideal Detector
Adequate sensitivity.
Non destructive.
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Quantitative Analyses based on
GC Chromatogram
1) Analyses based on Peak Areas (or Peak Height)
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Recall:
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2a) Analyses based on Internal Standard Method (single
point)
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Example
When 1.06 mM of pentanol and 1.53 mM of hexanol were
separated by gas chromatography, they gave relative
peak areas of 922 and 1570 units, respectively.
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Solution
F = 1.18
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1.18
[x] = 0.468 mM
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Exercise
A standard solution containing 6.30 x 10-8 M
iodoacetone and 2.00 x 10-7 M p-dichlorobenzene (an
internal standard) gave peak areas of 395 and 787,
respectively, in a gas chromatogram. A 3.00-mL
unknown solution of iodoacetone was treated with
0.100 mL of 1.60 x 10-5 M p-dichlorobenzene and the
mixture was diluted to 10.00 mL. Gas chromatography
gave peaks areas of 633 and 522 for iodoacetone and
p-dichlorobenzene, respectively. Find the
concentration of iodoacetone in the 3.00 mL of
original solution.
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2b) Analyses based on Internal Standard Method
(calibration curve)
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Construct a calibration curve of the ratio of the
Ethanol/Propanol area vs ethanol concentration and
calculate the unknown concentration.
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Correlation, y = 12.029 x + 0.0128, by substitution of
y = 1.72 into the equation, concentration of unknown,
x = 0.142 % wt/vol
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3) Area Normalization method
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Solution
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Temperature Selection
The proper temperature selection in gas
chromatography depends on several factors.
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The detector temperature must be high enough
prevent condensation of the sample components.
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Example: GC analysis results for the same mixture
using different temperature-programmed
Temperature
Program:
50 °C -100 °C,
10 ° C/min
Temperature
Program:
60°C - isothermal
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Effect of temperature on gas
chromatography:
(a)Isothermal at 45 °C
(b)Isothermal at 145 °C
(c)Programmed at
30 °C to 180 °C
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Method Development in Gas
Chromatography
Order of decisions:
1. Goal of analysis
- what is require?
- qualitative or quantitative?
- need high resolution?
2. Sample preparation
3. Choosing the detector
4. Choosing the column
5. Choosing the injection method
- split/splitless/on-column injection
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End of GC topic
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