Thermo Electron LLS India pvt., Ltd.

Presentation on
GAS CHROMATOGRAPH
By
N.Balamurugan
 Presentation - Structure
• Basics
• Types of Phases
• Carrier Gas Selection
• Column Selection
• Types Of Sample
• Injectors
• Detectors
• Schmatic Diagram - GC
• GC – Specification
• Chemito – GC Models
 Chemito Technologies
BASICS
Chromatography is the separation science
used to separate various components in a
homogenous mixture of organic components

CHROMATOGRAPHY

 PAPER CHROMATOGRAPHY
 THIN LAYER CHROMATOGRAPH
 GAS CHROMATOGRAPHY
 GAS LIQUID CHROMATOGRAPHY
 GAS SOLID CHROMATOGRAPHY
 LIQUID CHROMATOGRAPHY
 Types Of Phases

 MOBILE PHASE
Gas

 STATIONARY PHASE
Liquid
Solid
 Types Of Phases

• Mobile phase is the gas under

pressure with constant flow to
push the Sample.

• The sample through the column –

Stationery phase up to detector
 Mobile Phase

MOBILE PHASE  CARRIER GAS (Inert Gas)

HELIUM
ARGON
HYDROGEN
NITROGEN

SELECTION OF CARRIER GAS DEPENDS ON

» AVAILABILITY
» INERTNES
» SAFETY
» ECONOMY

Hence now a days generally nitrogen is used as carrier

gas especially with destructive detectors like
FID, NPD, TID, FPD etc.
 Stationary Phase

• Stationery phase is a phase where

separation takes place.

• Separation takes place due to difference

in adsorption co efficient of individual
component with respect to column
materials – Stationery phase.
 Stationary Phase

STATIONERY PHASE
COLUMNS

Packed Capillary

Copper Glass SS Teflon Wide bore capillary
   
¼” D 1/8” D 1/8” D 0.53 mm 0.25 mm

Even Glass Lined SS Packed Columns are also

available.
 Packed Columns

• Packed columns are packed with solid

materials.
• Example – molecular sieve, porapack q
etc.,
• Coated with liquid phase with solid
support
• Example – SE- 30, Carbowax 20 m on
chromosorb, OV 101 etc..
 Columns Selection

HOW TO ARRANGE / SELECT COLUMNS

• Selection parameters
• Column materials
• Length column
• Diameter of column
• Material of construction
• Column materials depends on analysis –
sample, internal standards (adsorption co
efficient)
 Columns Selection

Length and Dia Depends on No. of

Components – Resolution Efficiency In
Turn Depends on No. of Theoritical
Plates.

N.T.P.  LENGTH OF COLUMN

1/ DIA OF COLUMN
 Columns Selection

The methods were developed and

standardized for most of analysis
required / being done by various
organizations like

• ASTM
• British Pharma copia
• Indian Pharma copia
• BIS etc
 Pneumatics

To regulate mobile Phase – carrier gas we need

pneumatics like

• Carrier pressure regulators – SS metal diaphragm

• Splitter – “ T “
• Differential flow controllers / pin index flow controller
• Pressure reducers
• Pressure gauges / digital pressure readout
• Electronic pressure controller / auto flow controller /
digital pressure controller for capillary carrier.
• Mass flow controller for packed - carrier
 Column Oven

• To house stationery phase and also to vary

the temperature of column, we need oven
with heater to heat entire oven with fan to
have uniform heat throughout oven with
PRT to monitor and maintain required
temperature.

• With sufficient space to accommodate

columns like packed / capillary / combination
with or without switching valves.
 Types Of Samples

Sample can be
• Gas
• Liquid
• Solids
• In order to carry the sample through
column we have to convert the sample
state to gaseous state before introducing
the sample into column.
 Types Of Samples

• Solid sample to be dissolved in a solvent

and to be made as liquid sample.

• If not possible, esterifies the same

and analyze the esters and electroplate
the results of esters into sample or using
pyrolyser.
 Injectors

Liquid sample / converted liquid samples

have to get convert in to gaseous form
for which these liquid to be vapourized
before entering into column. Hence we
need injector.

Injector is the place where we inject the

sample either in gaseous form / liquid
form.
 Injectors

• Injector is heated at a particular

temperature normally more than
250 deg c. Setting of temperature
depends on sample of interest.

• Sample is heated / vapourised and

then get entered into column due to
presence of carrier gas.
 Injectors

• Gas Sample - MGSV / AGSV

GC SAMPLING VALVE

SAMPLE SAMPLE

CARRIER CARRIER

LOAD INJECT
 Types Of Injectors

INJECTOR

• PACKED

• CAPILLARY
SPLIT / SPLITLESS
 PACKED INJECTOR

PACKED INJECTOR / On Column Injection

• Complete carrier gas and sample

will be allowed to enter into column.
 CAPILLARY INJECTOR

CAPILLARY INJECTOR

• Portion of sample and carrier gas will be entering into

capillary column depends on our setting of split - ratio
and balance will be purged out using split purge
attachment.
• Split ratio can be set depending on analysis can be
varied
• From 1:1 to 1:200.
• Output of capillary column i.e. separated components
with carrier is very less and hence not sufficient to be
carried into detector. Hence we need to have make up
gas arrangement.
 DETECTORS

• The separated components has to be detected

using detectors by using optimum detectors.
• Various available detectors are :
• Thermal conductivity detector
• Flame ionisation detector
• Electron capture detector
• Nitrogen phosphorous detector
• Thermionic detector
• Flame photometric detector
 DETECTORS

• Thermal conductivity detector

• Universal detector used for general
purpose detector for analysing organic
samples, inorganic gases.

• Micro TCD for analysing low

concentration analysis
 DETECTORS

• Flame ionization detector / NPD/TID/FPD

• Are destructive detectors where sample are let into fire
and get destructed.
• Detectors due to its own principle of operation
generate electronic signals interms of micro volts which
are amplified using amplifier and out put of amplifier is
fed in to
a) recorder
b) integrator
c) Computer based data processor.
Due to scarcity of samples and need to be detected
using FID and TCD, or FID – ECD or TCD – ECD. we can
have detectors in tandem.
 Schematic Diagram

• In general schematic diagram of gas

chromatograph is

Carrier gas  pneumaticsinjectorcolumn

ovendetectoramplifierintegrator/
software

electronic modules

• Electronic module can be of microprocessor

controlled / solid state type.
 Schematic Diagram

BLOCK DIAGRAM OF GAS CHROMATOGRAPH

INJECTOR COLUMN DETECTOR RECORDER

 Electronic Module
Itis used for
• Injector temperature setting / controlling
• Oven temperature setting / controlling / programming
• Setting & controlling temp – cooling
• Detector temperature setting / controlling
• Detector functioning / amplifier functioning
• Transfer of signals – to data processor
• Storing various methods and retrieving and using the
same
• Self diagnostic
• Controlling / functioning various accessories like AGSV,
ALS, PTV, PYROLYSER / HSS, METHANISER / CSV/ BFV.
 Electronic Module

• Safety functions setting and controlling like

Maximum operating temperature cut off
Maximum temperature factory cut off
H2 cut off – controlling when no flame
Instrument cut off – when no carrier
Instrument cut off – when leak
• Chronometers – time events for values
• Carrier – pressure control / programming
• Mass flow controller for carrier, fuel, oxidants
 General Specifications

General specifications
• Gas chromatograph with packed – dual column with
• Temperature range for oven ambient – 400 deg c
• Detector and injector ambient – 400 deg c
• Temperature programme with 3 iso thermal & dual
ramp
• Temperature heating range 0 – 40 deg c/min
• Temperature cooling rate 300 deg c – 70 deg c in 10
min
• With temperature accuracy +/- 0.1 deg c
• Fid and tcd, data processor
• Optional / specific requirements
 General Specifications

• Capillary attachment, special detectors

• Temperature range ambient to 450 deg c / 500
deg c
• AGSV / MGSV – CSV – ALS
• Head space sampler
• Methanator
• PTV
• Fast cooling within 7 minutes using atmospheric
air