PPT KA II KROM.GAS SUSI
GAS CHROM ATOGRAPHY (GC)
By: Susila Kristianingrum
susila.k@uny.ac.id
Basic Competencies:
Students can describe the separation of GC,
interpretation chromatograms, and apply this
separation method for the analysis of a sample
USAGE GC
•
•
•
•
•
•
The oil (pet roleum)
The field of essent ial oils
The field of medicine
Chemist ry / research
Pest icide
Environment / pollut ion
BENEFITS OF USE GC
Fast
Operat ion is simple
Sensit ive (order of ppm, ppt ), mL, mg
The separat ion (resolut ion) high
Qualitat ive and quant itat ive analysis
High repeatabilit y
ANALYSIS OF CHROM ATOGRAPHY
GAS-LIQUID: PARTITION
GAS-SOLID: ADSORPTION
Qualitat ive analysis: based on chromat ogram
peak t hat appears
Quant itat ive analysis: a high peak areas or
peak chromat ogram
Gas-Solid Chromatography (GSC)
•
•
M obile phase: gas
Stat ionary phase: non-volat ile solids ,
stable
For example: spheron (Grafit e-coal),
linden (molecular sieves) porapak,
polypak, chromosorb
•
Basic work: t he separat ion of molecules
based on size
Gas-Liquid Chromatography (GLC)
•
Terms of t he solid support :
1. Stable at high t emperat ures
2.Inert , not react ing w it h samples &
stat ionary phase
3.The large surface area (grain)
4. Ideal sit uat ion (same size)
•
Examples of solid support :
Diat oport , cilit e, chromosorb (G, P, W)
•
Working basis:
separat ion based on part it ion bet ween mobile
phase and stat ionary phase
Gas-Liquid Chromatography (GLC)
• M obile phase: gas
• Stat ionary phases: liquid, t he condit ion:
1. Non volat ile
2. Inert & stable
3. Very viscous
4. Spread & bound t o a solid support
5. Soluble in organic solvent (et her)
Gas-Liquid Chromatography (GLC)
This t ype of stat ionary phase: polar, semi polar,
non polar
Examples of polar stat ionary phases:
carbowax 20M , PEGA, DEGS,
cast orwax, amine 220, versamid 900,
PDEAS
Examples of semipolar stat ionary phases:
dionilftalat , SE-52 (OV-17)
Examples of non-polar stat ionary phases:
apiezon, Squalane, SE-30
Classificat ion of compounds
POLAR
water
Glycol, glycerol
alcohol
Oksim
Hydroxy acids
ester
etc.
Classificat ion of compounds
SEM I POLAR
et her
ketone
aldehyde
tert iary amine
etc.
• NON POLAR
CHCl3
CH2Cl2
aromat ic hydrocarbons
olefin hydrocarbons
CH3CHCl2
etc.
BASIC SEPARATION
Rule: like dissolves like
Compounds
nat ure
Polar
Stationary
Phase
Polar
Soluble
Non polar
Non polar
Soluble
Polar
Non polar
insoluble
Non polar
Polar
insoluble
CHROM ATOGRAM
GAUSS CURVE
1. Eddy diffusion and molecular
2. The balance of slow
3. Price K is not fixed
IDEAL chromat ogram
1. Quickly balance
2. No diffusion
3. uniform column
INSTRUM ENTS GC
COM PONENTS INSTRUM ENTS GC
Carrier gas tank (+ regulat or)
Place t he sample inject ion
column
det ect or
Amplifier + Recorder
Carrier gas tank (+ regulator)
Place t he sample inject ion
column
Detector
•
•
•
•
FID
TCD
FPD
ECD
FID Detector
• Basic work: sample + burner gas (H2 + air/O2)
burned
Ionization occurs: positive ion to
negative electrode, negative ion to positive
electrode
• On electrodes occurs: Change Voltage (V)
Change of voltage forwarded to the recorder and
produce chromatogram.
• Advantages: highly sensitive (1000xTCD).
• Disadvantages: damaged samples, detecting
water insoluble, CS2, O2, N2, CO2, and the
noble gases.
TCD Detector / Chatarometer
• Conditions: t he t emperat ure of t he det ect or
must be higher t han column t emperat ure
• Basic principles: Component s w hich have been
separat ed from t he column carried by t he
carrier gas on t he filament . Change of filament
t emperat ure causes filament resistance .
Resistance filament s changed by Wheat st one
bridge become current . Change current arus
forwarded t o t he recorder and t hen convert ed
become chromat ogram.
TCD Detector / Chatarometer
• Advantages:
1. Does not dest roy t he sample
2. All kinds of compounds can be det ect ed.
• Disadvantage:
less sensit ive.
By: Susila Kristianingrum
susila.k@uny.ac.id
Basic Competencies:
Students can describe the separation of GC,
interpretation chromatograms, and apply this
separation method for the analysis of a sample
USAGE GC
•
•
•
•
•
•
The oil (pet roleum)
The field of essent ial oils
The field of medicine
Chemist ry / research
Pest icide
Environment / pollut ion
BENEFITS OF USE GC
Fast
Operat ion is simple
Sensit ive (order of ppm, ppt ), mL, mg
The separat ion (resolut ion) high
Qualitat ive and quant itat ive analysis
High repeatabilit y
ANALYSIS OF CHROM ATOGRAPHY
GAS-LIQUID: PARTITION
GAS-SOLID: ADSORPTION
Qualitat ive analysis: based on chromat ogram
peak t hat appears
Quant itat ive analysis: a high peak areas or
peak chromat ogram
Gas-Solid Chromatography (GSC)
•
•
M obile phase: gas
Stat ionary phase: non-volat ile solids ,
stable
For example: spheron (Grafit e-coal),
linden (molecular sieves) porapak,
polypak, chromosorb
•
Basic work: t he separat ion of molecules
based on size
Gas-Liquid Chromatography (GLC)
•
Terms of t he solid support :
1. Stable at high t emperat ures
2.Inert , not react ing w it h samples &
stat ionary phase
3.The large surface area (grain)
4. Ideal sit uat ion (same size)
•
Examples of solid support :
Diat oport , cilit e, chromosorb (G, P, W)
•
Working basis:
separat ion based on part it ion bet ween mobile
phase and stat ionary phase
Gas-Liquid Chromatography (GLC)
• M obile phase: gas
• Stat ionary phases: liquid, t he condit ion:
1. Non volat ile
2. Inert & stable
3. Very viscous
4. Spread & bound t o a solid support
5. Soluble in organic solvent (et her)
Gas-Liquid Chromatography (GLC)
This t ype of stat ionary phase: polar, semi polar,
non polar
Examples of polar stat ionary phases:
carbowax 20M , PEGA, DEGS,
cast orwax, amine 220, versamid 900,
PDEAS
Examples of semipolar stat ionary phases:
dionilftalat , SE-52 (OV-17)
Examples of non-polar stat ionary phases:
apiezon, Squalane, SE-30
Classificat ion of compounds
POLAR
water
Glycol, glycerol
alcohol
Oksim
Hydroxy acids
ester
etc.
Classificat ion of compounds
SEM I POLAR
et her
ketone
aldehyde
tert iary amine
etc.
• NON POLAR
CHCl3
CH2Cl2
aromat ic hydrocarbons
olefin hydrocarbons
CH3CHCl2
etc.
BASIC SEPARATION
Rule: like dissolves like
Compounds
nat ure
Polar
Stationary
Phase
Polar
Soluble
Non polar
Non polar
Soluble
Polar
Non polar
insoluble
Non polar
Polar
insoluble
CHROM ATOGRAM
GAUSS CURVE
1. Eddy diffusion and molecular
2. The balance of slow
3. Price K is not fixed
IDEAL chromat ogram
1. Quickly balance
2. No diffusion
3. uniform column
INSTRUM ENTS GC
COM PONENTS INSTRUM ENTS GC
Carrier gas tank (+ regulat or)
Place t he sample inject ion
column
det ect or
Amplifier + Recorder
Carrier gas tank (+ regulator)
Place t he sample inject ion
column
Detector
•
•
•
•
FID
TCD
FPD
ECD
FID Detector
• Basic work: sample + burner gas (H2 + air/O2)
burned
Ionization occurs: positive ion to
negative electrode, negative ion to positive
electrode
• On electrodes occurs: Change Voltage (V)
Change of voltage forwarded to the recorder and
produce chromatogram.
• Advantages: highly sensitive (1000xTCD).
• Disadvantages: damaged samples, detecting
water insoluble, CS2, O2, N2, CO2, and the
noble gases.
TCD Detector / Chatarometer
• Conditions: t he t emperat ure of t he det ect or
must be higher t han column t emperat ure
• Basic principles: Component s w hich have been
separat ed from t he column carried by t he
carrier gas on t he filament . Change of filament
t emperat ure causes filament resistance .
Resistance filament s changed by Wheat st one
bridge become current . Change current arus
forwarded t o t he recorder and t hen convert ed
become chromat ogram.
TCD Detector / Chatarometer
• Advantages:
1. Does not dest roy t he sample
2. All kinds of compounds can be det ect ed.
• Disadvantage:
less sensit ive.