1.gc basic
TRANSCRIPT
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GC BASIC
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Contents
Basic Theory Configuration Carrier gas Injection port Column Detector
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Flow Chart for Analysis
Sample collection Sample collection
PreparationPreparation
InjectionInjection SeparationSeparation DetectionDetection
IntegrationIntegration
ReportReport
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Chromatography
LCSFCGC
LSC LLC
Column TLC
LSCAbsorption
IECIon exchange
SEC LLCPartition
BPCPartition
ICIon exchange
GPCSize exclusion
GFC IPCIon pairing
GSCAbsorption
GLCPartition
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GC or LC
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Advantages of GC
Fast Analysis Time High Resolution High Sensitivity Easy interface with MSD, AED Reproducibility Small injection volume Economic price
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Analysis Flow of GC
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System Configuration
Carrier Gas
Injection port
Column
Detector
Data system
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Carrier Gas
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Carrier Gas
Used for carrying vaporized sample to the column
Necessities : Inert, pure, dry Type : H2, N2, He, Ar
→ Different depending on detector
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Recommended Carrier Gas
Best sensitivityN2
Best sensitivityN2ECD
Best Linear Dynamic rangeAr/CH4
Generally usedN2FID
Can be usedH2,He
Optimum HeNPD
Only use HeHePDD
Used for analysis of H2 N2
High sensitivity H2
General
Detector
N2IRD
MSD Mass Range 10-800 m/z
Must use HeHeMSD
Generally used He
TCD
Special
Detector
RemarkCarrier GasDetector
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A : Moisture trap B : Hydrocarbon trap
C : Indicating Oxygen trap
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Injection Port
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Injection Port
Purpose - Vaporize sample - Transfer sample to the column
with accuracy and reproducibility
Sample type - Liquid or Gas
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Injection Port
Injection port for packed column
Injection port for capillary column- Split
- Splitless
- Cool On Column
Sample preparation System - Headspace, Purge & Trap, Valve, Pyrolyzer etc.
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Columns for Injection port
Packed Injection port - Packed column
- Wide bore capillary column(0.53 mm I.D.)
Capillary Injection port - Capillary column(0.25 ~ 0.53mm I.D.)
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Packed Injection Port
Traditional sample injection method High resolution is not necessary Gas analysis using GSC(gas-solid chromatography) Simple design, Whole carrier gas transfer to the column Sample is transferred to the column after vaporization, the possibility of contamination from non volatile compounds is low
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Packed Injection Port
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Capillary Injection Port Split/Splitless
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Split Injection
Developed for capillary GC Sample is vaporized at the injection port
by high temperature. Some part of sample
are transferred to the column and others
are vented Can be used in most of samples No limitation of solvent Good peak shape
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Automated Pneumatic Control System (Split mode)
To Detector
Split Vent
Septum Purge
Carrier Gas
Flow Sensor FS
Pressure Sensor PS
Septum Purge Regulator
Trap
On/off valve V
Proportional Valve PV2
Proportional Valve PV1
Capillary inlet
High Flow Rate
Low Flow Rate
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Split Ratio
Set up oven temperature Set up column pressure Set up septum purge flow
(3-5ml/min)
Set up split vent flow
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Splitless injection port
All carrier gas goes to the column without venting
All sample is transferred to the
column after vaporizedThe sample is fully used into the
column : high sensitivity
high reproducibility
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Automated Pneumatic Control System (Splitless mode)
To Detector
Carrier Gas
Flow Sensor FS
Pressure Sensor PS
Septum Purge Regulator
Trap
On/off valve V
Proportional Valve PV2
Proportional Valve PV1
Capillary inlet
Septum purge
Split Vent
Low Flow Rate
High Flow Rate
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Splitless Injection
Have to optimize some conditions such as oven temperature comparing with split mode injection to reduce the band broadening
Can be used with high b.p solvent
Use with large capacity liner
Can be used with high column flow rate
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Demerits of Splitless mode
Quantitation result depends on injection skill
Pay attention to select sample solvent
Possible to cause the column degradation rapidly
The component eluted at the tail of solvent peak depends on boiling point, polarity and injection volume of solvent
Optimizing analytical condition needed
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Flow control for split/splitless
Length 0.25mm ID
0.32mm ID
0.53mm ID
15m30m60m105m
6psi12psi24psi40psi
4psi8psi
16psi30psi
1psi3psi6psi
10psi
Injector pressure set up
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Split/splitless liner(I)
Have to use non activated Glass liner
if the sample has high activity Liner cleaning
- Rinse with MeOH/Acetone
- Do not use Acid and Base
- Do not use soap and detergent
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Split/splitless liner(II)
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Optimum injector condition
Standard Condition
- Injector temperature(general) : 250 ℃
- Volatile sample : 150 200∼ ℃ex) VOCs
- High b.p sample : 275-300℃ex) steroids, triglycerides or surfactants
Check the maximum temp. of septum installed
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Contaminable parts of injector
Tubing used for carrier gas
Septum
Liner
Gold seal (split/splitless injector)
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Contamination of septum
Contaminated septum After replace the septum
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Oven temperature Setup
Compounds are onlyduplicated by Retention time
IsothermalTemperature
program
Yes No
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Isothermal(a) and temperature program(b)
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Isothermal condition setup Set up oven temperature
50 → 10 /min → Max. temperature of column ℃ ℃ Check the retention time and temperature of last
eluted compound Analyze sample at the below 20 of temperature for ℃
last eluted compound If the compounds are not separated, analyze again
on the decreased temperature Change the condition to the temperature program or
the column
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Temperature program setup
1st step temperature program setup
50 → 10 /min → Max. temperature of column(30min)℃ ℃ After injection, check the chromatogram
Set up initial temperature and time
Set up increasing rate
Set up final temperature and time
Confirm optimum condition
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Optimum oven temperature
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Split injection mode
Splitless injection mode
(oven temp.: 25°~210°)
Splitless injection mode
(oven temp.:60°~210°)
Splitless injection
(Solvent : Methanol)
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Column
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Column
Separates the mixed compounds to individual components
Type
- Depending on I.D. : Packed, Capillary
- Depending on stationary phase : GSC, GLC
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Packed / Capillary column
Packed column - Large inside diameter / short length - Large sample capacity - Low Resolution
Capillary column - Small inside diameter / long length - Small sample capacity - High Resolution
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Comparison
Packed Capillary
Length (m)
ID (mm)
Flow rate (ml/min)
Pressure drop (psi)
Theoretical plate
Theoretical plate/length
Capacity
Film thickness (um)
1-6
2-4
10-60
10-40
5000(2m)
2500(2mm ID)
10ug
1-10
5-105
0.2-0.75
0.5-15
3-40
180000(60m)
3000(0.25mmID)
50ng(0.25mmID)
0.1-7.0
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Packed Column
Traditional packing
..
Porous layer bead
Bead column
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Capillary Column
Wall coated column
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Chromatogram of plant extract
Packed column
Capillary column
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Capillary column with high resolution
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Van Deemter Curve
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Optimum flow rate for carrier gas
Packed
Capillary
Column ID Optimum gas flow rate
Optimum gas linear velocity
1/4"1/8"
530 um (mega bore)320 um (wide bore)200 um (narrow bore)100 um (high speed)
50-60 ml/min20-30 ml/min
3-5 ml/min1-3 ml/min0.5-1 ml/min0.2-0.5 ml/min
2.6 - 3.2 cm/sec4.2 - 6.3 cm/sec
22 - 38 cm/sec20 - 62 cm/sec26 - 53 cm/sec42 - 106 cm/sec
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Comparison of GSC / GLC
GSC GLC
Mobile Gas Gas phase
Stationary Porous polymer Solid support phase +Liquid phase
Separation Absorption/Desorption Partition
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Gas Solid Chromatography
Carrier gas
Carrier gas
• Packed column
• Capillary column
packing material (GSC)
- Porous
- Large surface area
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Gas Liquid Chromatography
Carrier gas
• Packed column
• Capillary columnSolid support :
Porous support
with large surface
area
Liquid phase
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Capillary column selection
Sample type (Like dissolves likes)
Stationary phase type
Film thickness
Column Inside diameter
Column length
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Column selection according to polarity
Polarity
• Non polar(HP-1, HP-5) : boiling point• Intermediate (HP-50+) : boiling point
hydrogen bond• Polar (HP-INNOWax, HP-Wax) :
interaction of functional group
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Column selection guide
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Non polar column
HP-1 (HP-101) - 100% Dimethylpolysiloxane - Phenol, Amines, Hydrocarbons, PCBs, Pesticides, Sulfur compounds - DB-1, BP-1, SPB-1, GB-1, CP-Sil 5, OV-1, SE-30
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Non polar column
HP-5 - 5% Diphenyl / 95% dimethylpolysiloxane
- Fatty acid, Drugs, Methyl esters, Alkaloids,
Halogenated compounds
- DB-5, BP-5, SPB-5, CP-Sil 8, SE-52,
OV-5
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Medium-polar column
HP-35 - 35% Diphenyl / 65% dimethylpolysiloxane
- Pesticides, Drugs, Amines
- DB-35, RTX-35, SPB-35, AT-35, Sup-Herb
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Medium-polar column
HP-1701 - 14% Cyanopropylphenyl /
86% dimethylsiloxane
- Aroclors, Herbicides, Pesticides, TMS sugars
- DB-1701, SPB-1701, OV-1701, CP-Sil 19
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Polar column
HP-FFAP - Acid modified Polyethylene glycol
- Acids, Alcohols, Aldehides, Nitriles,
Ketones
- DB-FFAP, OV-351, Stabilwax-DA
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Chromatograms of gasoline by capillary column with varying on film thickness
Film thickness
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Column ID 0.20mm 0.25mm 0.32mm 0.53mm 0.75mm
Sample
capacity(ng)5 - 30 50 - 100 400 - 500
1,000 -2,000
10,000 -15,000
Number of TP
(N/m)5000 4170 3330 1670 1170
Optimum
Flow rate
(He, 20cm/min)0.4 0.7 1.4 2.5 5
Column selection guide
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Resolution according to length
Column length : Resolution : Retention time :
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Column selection Guide
Select same polarity with sample Use the column ID 0.32mm
- Small ID(0.25mm) column : complex sample- Large ID(0.53mm) column : simple sample
Use the column length 30m - The higher resolution needed,the longer column you
select
Use the column 0.25 ㎛ film thickness- Thick film : volatile compounds- Thin film : non volatile compounds
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Column cutting
Wrong column cutting
Right column cutting
Cutting tools
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Installation method for column(at injector-side)
① Insert column nut to the column at first and
then insert ferrule.
② Keeping the column length 3 cm from the ferrule, insert the column to the adaptor and then hand-tighten the nut.
③ Loosen the column nut
④ Cut the column remaining 5 mm from the ferrule
⑤ Connect the column nut to the capillary adaptor again
⑥ Hand-tighten the nut and then tighten ¼ turn using wrench
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Effect from wrong column connection
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Ferrule Selection
Graphite(100%)
- ~450 ℃ - general, reusable
- FID, NPD, ECD
- can not be used for MSD
Vespel(100%)
- 280 ℃ - reusable
- for isothermal condition
Graphite/ vespel
- GC/MSD interface
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How to connect the column at a detector side
Column end has to be located on the 2mm below of jet orifice
(Insert the column to the end of detector inside and then pull out around 2mm)
Installation method for nut and ferrule is same
with injection port.
In case of ECD, measure 72mm from the
ferrule and cut the column
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Column Conditioning
Thermal conditioning
- Do not connect to the detector
- Set the carrier gas flow
- Conditioning as below
100℃
1 hr
2~3 /min℃
Max. temp. -30 ℃
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Thermal conditioning
Column conditioning is essential like idling for car!
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Solvent rinsing can remove soluble contaminants inside of bonded capillary column
Cleaning using solvent
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Solvent volume and pressurefor cleaning
Column I.D.SolventVolume
ReservoirPressure
0.18mm 10ml 50 psi
0.25mm 15ml 40 psi
0.32mm 25ml 30 psi
0.53mm 50ml 15 psi
* Do not rinse the non-bonded column
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Detector
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Detectors Types
- TCD : Thermal Conductivity Detector
- FID : Flame Ionization Detector
- ECD : Electron Capture Detector
- NPD : Nitrogen Phosphorous Detector
- FPD : Flame Photometric Detector
- PDD : Pulsed Discharge Detector
- MSD : Mass Selective Detector
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Selection Guide
Non active gasFormaldehyde
START
Simple chemicalHigh concentration
CompoundContaining
halogen
Compound Containing
Nitrogen/phosphorus
CompoundContaining
Phosphorus
CompoundContaining
Sulfur
TCD
ECD
NPD
YY
YY
N
NN
N
N
Y
FID
N
Y
FPD
PDHID
PDHID
PDECD
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Characteristics of detectors
Detector type Analytes MDL Linearity
FID S have to ionized 5pg C/sec 10 (*7) on the H2/Air flame
TCD G All compounds 400 pg/ml carrier 10 (*6) (low sensitivity)
ECD S Halogen containing 0.1pg Cl/sec 10 (*4) compounds
NPD S N, P containing 0.4 pg N/sec 10 (*3) compounds 0.2 pg P/sec
FPD S P, S containing 20 pg S/sec 10 (*3) compounds 0.9 pg P/sec 10 (*
4)
MSD G All compounds 10 pg –10ng 10 (*5)
S: Selectable G : General
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Sensitivities
TCD
ECD
FID
NPD
PDHID
FPD
PDECD
10-15
1ppt
10-12
1ppb
10-9
1ppm
10-6
0.1%
10-3 g
100%
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TCD
Non destructive General detector
Measure the differences between sample and carrier
4 Filaments
Linearity : 106
Gas purity, Natural gas
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FID
Measure the current of ionized sample by the H2/Air flame
Linearity : 107
Organic solvent, organic compounds, food, flavor, etc.
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ECD
Respond to the compounds
have high electro negativity
Halogen, Nitro group, Organometalic, Oxygenated compound
Linearity : 104
Pesticides, PCBs, VOCs
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NPD
Similar structure to FID. Bead(Alkali salt) increase the ionization of the compounds which contains N and P
Ionization of compounds which do not contain N and P is not allowed.
Linearity : 104
Pesticides, Pharmaceutical
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FPD
Principle- Compounds containing S
and P : material that produces chemical emission is generated
- Produce the light of specific wavelength
- Amplify the light of specific wavelength (S:393nm, P:525nm)
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PDD PDHID/PDECD Mode HID mode - Electron is produced by He discharge - Produced electron collides with He in the discharged area, and produce He** - He** collides with sample to ionize the sample
ECD mode - Xe(Dopant gas) is ionized to produce free electron - Standing current is formed by produced electron - When the sample is introduced, standing
current is decreased