Gas Chromatography

Chromatography

A separative technique
Physical separation of
components:
Gas, Liquids, Solids
Organics and Inorganics
 Chromatography: qualify and
quantify

• Which
(are the components)
and
• How much (of the single
component)
 History
• 1850-Foundation of chromatography were laid
around when organic chemistry flowered in to a
separate science

• 1906-Tswett described the use of glass columns

packed with adsorbent for separation

• 1941-Martin and Synge- Gas could replace liquid as

mobile phase

• 1952- First GC- Martin and James

 History- contd..

• 1954-Ray-Thermal conductivity detector

• 1955-First Commercial GC

• GC-Powerful analytical tool in modern laboratory

 Basics Of Chromatography

• Definition
• Separation of components achieved by transporting
through static medium by moving carrier gas
• Types of chromatography
• classified based on the nature of static (stationary)
medium and carrier (mobile phase)
• LLC - Liquid Liquid Chromatography
• LSC - Liquid Solid Chromatography
• GLC - Gas Liquid Chromatography
• GSC - Gas solid Chromatography
 Basics Of Chromatography

• Main components
• Carrier Gas - normally nitrogen , helium , hydrogen
etc.. Carrier gas continuously flows through the column.
• Sample - can be gas (<0.5 ml) or liquid (1 micro Liter)
periodically injected by specially designed sample
injection valve. Liquid samples must vaporize after
injection and pass through the system.
• Column - the component separation is done inside the
column.
• Detector - components separated then passed through
the detector , where it is converted into electric
current/voltage
 Basics Of Chromatography

The sample volume , column and detector response

are temperature dependent hence all these
components are installed in a temperature controlled
enclosure called “Oven”
Sample In Sample Out

Detector Vent

Sample Loop
Column

Isothermal Oven
Peak Height

Carrier Gas

Time
 How Separation Takes Place ?

• Different components dissolve to different extent in

same liquid.
• Dissolving capacity depends on pressure and
temperature.

Consider the column as closed compartment in which

static phase as liquid and sample injected as gas.
 A B C D

Sample
(gas)

liquid

Gas started Equilibrium Some more Equilibrium

dissolving in reached gas is added. reached
liquid Dissolving
started

Using above phenomenon lets understand what happens

while gas phase (sample) is moving with the carrier
 Carrier Flow

Sample

Static
Medium

A B C

D E F
 For 21 compartments
n
concentratio

For 10 compartments

For 5 compartments

compartments
 Retention time (tr)

A peak is characterised by the retention time (selectivity)

and its shape (efficiency)
 EFFICIENCY

• Is not quality of a separation

• Ability to transmit the sample component(s) from inlet

to outlet without appreciable band broadening
 Resolution
Resolution
(measure of the
separation
between two R =  t/Wb2
consecutive
peaks) depends
on the system’s
selectivity and
efficiency
 Electronic Card Case
Display Keypad

Regulator / Gauge

Air
Carrier
Flow
Adjustment
Vent

Column
LSV
CP Valve
Sample Line
 Purging System

• GCs have X-purge system installed at the top of the GC as

separate box.
• When GC is switched on and purge air inlet pressure is
healthy the power to the GC will be turned on after 5.3
minutes.
• The GC will be immediately switched of if the pressure
inside the GC goes below…….
• The GC power will be disconnected if the ex-proof purging
box is opened.
• There is a bypass switch , when pressed the power is
given to GC without purge pressure being healthy.
 Filters and Regulators

• The carrier gases , makeup gas , air etc.. Comes to the

regulator block.
• These gas connection have filter / restrictors at the inlet
on regulator block.
• The regulator block have number of pressure gauges ,
regulators and associated tubing.
 Carrier Gases

• Carrier gases are to be selected depending on the detector

used and the composition to be measured.
• For FID/FPD combustible carrier gas (like hydrogen ,
helium) will be used.
• For TCD detector gases which have distinct thermal
conductivity compared to composition gas will be
used as carrier gas.
• Also depend on the length of column and speed of analysis
required.
 Carrier Gases
• The carrier gas should be highly purified
• The purity level should be 99.999%
• The impurities like Oxygen , moisture and hydrocarbon
should be less than 10 ppm in total.

• The regulators used should be of 2 stage SS diaphragm type.

• The impurities like moisture can ingress into the carrier
gas through rubber diaphragms.

• Purification traps (molecular sieve) can used to purify the

carrier gases.
 Oven
• Isothermal Oven
• To keep the temperature constant.
• To keep all the moving phase in gaseous form.
• Temperature controlled at +/- 0.05%
• heaters and vortex coolers are used
• Programmed Oven
• To change the oven temperature as per
application requirement.(heating and cooling)
• Used when the wide boiling range compositions
measurement.
 Temperature Zones

• The temperature zones are areas where temperature

is controlled by heating ( or cooling).

• The LSV , isothermal oven , air cleanup assembly

forms individual zones.
 Sample Injection

• Liquid Sample (Injection)

• Liquid Sample Valves (LSV) Used for injecting
liquid samples into the GC
• LSVs have the arrangement for selecting
sample size (normally 0.02 to 0.07 micro liter)
• LSVs Prevents liquid sample entry into the GC
with the help of seals.
• Also have temperature control to gasify the
liquid.
• The temperature is maintained at higher value
than isothermal oven.
• Mainly two types of valves are used namely
Reciprocating , Rotary
 Sample Injection
• Gas Injection
• There is no need of separate Valve.
• Gas sample directly goes into the GC.
• Sample is trapped into the Tube (Sample loop).
• Sample size is decided by the loop length of
the tube.
 Air Cleanup / Methaniser

• Air Cleanup
• Used for GCs with FID. Removes traces of Hydro
Carbon and moisture.
• Contains heater and molecular sieve.
• Temperature is of the order of 450 deg.
• Methaniser
• Used in TCD.
• Converts Methane into CO2 and measures as
Methane.
• Contains heater and molecular sieve.
 CP Valve
• Continuous Performance Valve
• This valve is used to switch the column . Detector and
vent etc.. Interconnections.
• There are two type of CP valves 10 port and 8 port.
• Pneumatically actuated.
• Contains slider with grooves.which sits on the moving
part.
• Slider connect the ports on the stationary part of the
valve.
• Failure chances are more as this is moving part.
 Columns
• Columns are used for separation of composition of
interest
• Also used to separate the heavier component to
enable backflush.
• Some columns are used to remove water.
• Columns are classified as Packed and Capillary
columns.
 Packed columns
• Packed Columns have molecular sieve filled inside
them and then the stationary phase is loaded.
• The column OD for these columns are normally 1/8”
and more. But the micropacked columns have the
OD of 0.95 mm.
• These columns have very high column capacity.
 Capillary Columns
• Capillary columns have stationary phase loaded on
the fused silica or SS tube.
• Fused silica enable to form thin tunes but are delicate
as compare to SS columns.
• These columns have less capacity as compare to
packed columns.
• These columns can give faster separation and high
carrier gas velocity.
• The ID of the capillary column vary from 0.1 to 0.53
mm.
 Columns
• Columns are identified by following factors
• Column length
• Column ID
• Stationary phase
• Molecular sieve (packed columns)
• Stationary phase thickness
• Column Material
• Column maxi allowed temperature.
• Example
0.32 mm X 30 m , MXT-Wax , 1 micron , 190 Deg , SS
 Columns
Significance of Column parameters

• Column Length
• Column length is instrumental in separating the
peaks from each other i.e more resolving power.
• Longer the column more will be the separation.
• Column length also determine the cycle time of the
chromatograph. Longer the column GC will have
longer cycle time and longer retention time.
• If the column length is doubled the Retention time will
double but the resolution will increase only by 40%.
• Longer the column costlier it will be.
 Columns
Significance of Column parameters
• Column ID
• More ID means more column capacity i.e.
column can take more sample inside it.
• If the sample is more than the column capacity
then the poor reproducibility , peak distortion
will result.
 Columns
Significance of Column parameters

• Stationary phase
• The separation of particular component is decided by
the stationery phase inside the column.
• The stationary phase also decides the interaction
between stationary and moving phase and hence the
retention time of the components of interest.
• Stationary phase have the temperature limitation
above which it should not be used.
• Stationary phase also decides which solution to be
used for rinsing the column if required.
 Columns
Significance of Column parameters
• Molecular Sieve (packing)
• packing provides the more area for interaction
between the mobile and stationary phase.
• It also decides the conditioning time of the
column.
• Also influence the column bleeding.
 Columns
Significance of Column parameters

• Stationary phase thickness

• It effects the retention time of the components.
• Also have effect on the elution temperature
(oven temperature)
• It also have effect on column bleeding.
 Columns
Significance of Column parameters

• Column Material
• It gives the mechanical strength to the column.
• It decide the flexibility and inertness of the
columns
 Columns
Significance of Column parameters
• Max column operating temperature
• Above which stationary phase may get
damaged or deteriorate.
 Adjustment Valve

• There are adjustment valves for different flows (e.g

backflush , splitter etc.) The list is attached on the GC
indicating valve number and corresponding flow.
• These valves are at right side when you are facing the
GC
• The adjustment to be done with screw driver during flow
measurement.
 Adjustment Valve

• There are adjustment valves for different flows (e.g

backflush , splitter etc.) The list is attached on the GC
indicating valve number and corresponding flow.
• These valves are at right side when you are facing
the GC
• The adjustment to be done with screw driver during
flow measurement.
 Carrier Flows

• Selector vent : when the final separation of the

components are in progress , the lighter components
(unwanted) are sent to selector vent rather than to
detector. Once the lighter components are out , the
column is connected to detector.
• Analytical Flow : this is the carrier gas flow which
goes into detector. Normally there are more than one
analytical flow.
 Carrier Flows
• Make up flow : this flow is required for GC with FID /
FPD detector. This flow is added to carrier gas flow to
optimise the detector sensitivity.

• Dilution flow : This flow is required for GCs with FID /

FPD detector. This is generally the Nitrogen gas used
for dilution of carrier gas.This is required for
optimising the detector sensitivity.

• Air Flow : The Air flow is essential to flame ignition in

FID and FPD detectors
 Detectors

• FID / TCD / FPD are the detectors which are used in

most of the applications.

• The detector selection are based on the type of

composition to be measured and the concentration
range of the component(sensitivity required).
 Electronic Cards
• Power Supply Card
• It distribute the 100VAC input power to all parts
of GC.
• The input power is brought into the card
through filter (choke).
• The card has a switch which could be used to
switch off the power supply. GC does not loose
any data.
• CPU Card
• It works as the nerve system of the GC
• It has a reset switch on it. After the CPU
resetted all the tables in RAM will disappear.
 Electronic Cards

• Chromaboard
• It takes the input from detector.
• It also take / give digital signals (configurable
through the digital table)
• Analogue output board
• This board gives the analogue out for
measured components.
• This board also have one mount on board , on
the analogue board , for each out put.
 Electronic Cards

• Digital Output Card

• This board gives digital output in the form of 5V
or 0V.
• The digital output can be configured as
Normally close (5V) or Normally open (0V).
• VistaNet communication card
• This card is essential if the GC required to be
connected to PC or Modbus Interface Unit via
digital communication.
 Electronic Cards
• TCD / FID / FPD amplification board
• This board amplifies the detector output and give the
output to chromaboard.
• The board will be different for different type of
detectors.
• Display and Com board
• This display board sits on the front panel and
responsible for keyboard operation and LCD display.
• The com board sits on display board and is
responsible for communication between display
board and CPU.
 Electronic Cards
• DTC backplane board
• This board acts as the digital temperature
controller.
• This board also responsible for taking control
parameter form tables in CPU.
• This board accepts the input from temperature
zone cards and give the heater on of commands.
• Temperature Zone Card
• This small board is dedicated for one zone.
• This board actually switch the heater on/off and
also takes the input form zone temperature sensor.
 Electronic Cards
• VAC conditioning assembly
• This board gives the power to DTC and zone
cards.\
• This board handles large quantity of power as
the number of heaters receive power from this
board.
• Solenoid Driver Card
• This card switches the solenoid (stream
selection , CP valve , LSV etc..) on and off.
Electronics Panel Layout
Electronics Cards Layout
Thank you