CHROMATOGRAPHY
MMS 3201
AQUATIC METHODOLOGY AND
INSTRUMENTATION
Izwandy Idris, Blue Cabin,
ext. 3467, izwandy.idris@umt.edu.my
Introduction
What is Chromatography?
GAS CHROMATOGRAPHY
GC analytical technique
2.
Separation processes
i. Different adsorption with column packing
materials.
ii. Different Boiling point (Temp programming
System).
iii. Different in weight (Molecular weight)
Sample injected
(A, B &C)
B
C
A
Carrier (inert) gas Initial column temp set at 60oC
The boiling points for
A=70oC
Peak
height
Time, min.
INJECTION PORT
GC SEPARATION
TYPES OF GC COLUMN
(0.01 0.053cm)
(0.3-0.4cm)
TYPES OF GC COLUMN
(0.01 0.053cm)
(0.3-0.4cm)
Comparison Of column
Capillary column
Packed column
stable
Injection of Sample
1. Sample must be volatile.
2. The analyte must be present at an
appropriate concentration.
3. Injected sample must not be degradable
in the column.
DETECTORS FOR GC
1.
DETECTORS FOR GC
2.
DETECTORS FOR GC
3. Electron Capture Detector (ECD)
consists of a beta emitter (electron) such as 63Ni.
Emitting electrons ionize the mobile phase (usually
N2), production of additional electrons electric
current
OM
OM
/Hydrocarbons
H2 + O2
N2
Example of Chromatogram-Petroleum
Hydrocarbon Analysis
Petroleum hydrocarbons are extracted from sea
water and fractionated into
1. Aliphatic hydrocarbon &
2. Aromatic hydrocarbon fractions using
Column Chromatography.
GC-FID with capillary column (30 m) and
temperature programming 20 min (70 oC),
increase to 300oC with a rate of 8oC/min and hold
at 300 oC for 30 min
Aliphatic Hydrocarbons
FID2 B, (JOHNSON\SIG11155.D)
pA
C27
C18
150
C29
C19
C28
C23
C24
C26
C21
200
C22
250
10
20
C32
C20
C16
C10
C9
C8
50
ISTDi
C17
100
30
40
50
60
70
min
Polyaromatic Hydrocarbons
FID2 B, (JOHNSON\SIG11026.D)
pA
120
BkF
100
Pyr
80
60
ISTDI
ISTDII
20
10
20
30
40
BbF
IP
ISTDIII
BaA
40
50
60
70
min
3.
4.
C32
C29
C28
C27
C26
C24
C23
C22
C21
C19
C8
300
C18
C16
400
C17
C13
500
C14
C12
C30
C20
C25
C9
600
C11
pA
C15
C10
FID2 B, (JOHNSON\SIG11151.D)
200
100
10
20
30
40
50
Ace
Acy
Na
FID2 B, (JOHNSON\SIG11032.D)
450
400
350
300
250
Flu
200
10
20
30
40
BbF
dBahA
BghiP
50
BkF
BaP
IP
Pyr
100
BaA Chyrs
AnPh
FI
150
50
2.
3.
4.
GC MS(Shimadzu 2010)
GC MS 3D VIEW
Organic + oO2
600 C
CO2
Infrared Analysis
TOC
https://www.youtube.com/watch?v=08YWhLTjlfo