GAS CHROMATOGRAPHY – FLAME IONIZATION

DETECTOR (GC-FID)

Submitted to Submitted by
Mr.Ashit Ishwar Rizwan Ahmad
Office Incharge Student
(Instrumentation Lab) B.Tech(Food Tech.)
 INTRODUCTION

Gas Chromatography – Flame Ionization Detector or GC-FID is a very

common analytical technique that is widely used in the petrochemical,
pharmaceutical and natural gas markets.
An FID typically uses a Hydrogen/Air flame into which the sample is
passed to oxidize organic molecules and produces electrically charged
particles (ions). The ions are collected and produce an electrical signal
which is then measured.

As common with other GC techniques, a carrier gas is required with

low Water and Oxygen impurities since Water and Oxygen can interact
with the stationary phase and cause significant problems such as high
baseline noise and column bleed in the output gas chromatogram
which both reduces the analyzer sensitivity and decreases column
lifetime. The FID is also extremely sensitive to Hydrocarbon impurities
in the Hydrogen and Air supply for the flame. Hydrocarbon impurities
can cause increased baseline noise and reduce the detector sensitivity.
The routine calibration of the analyzer using a calibration mixture is
common.
 PRINCIPLE

The flame ionization detector (FID) is the automotive emissions

industry standard method of measuring hydrocarbon (HC)
concentration.
The sample gas is introduced into a hydrogen flame inside the
FID. Any hydrocarbons in the sample will produce ions when
they are burnt. Ions are detected using a metal collector which
is biased with a high DC voltage. The current across this
collector is thus proportional to the rate of ionization which in
turn depends upon the concentration of HC in the sample gas.
The ionization process is very rapid, so the slow time response
of conventional FIDs is mainly due to sample handling. A typical
slow analyzer might have a response time of 1-2 seconds.
The Gas Chromatography FID analyzers use conventional
detection principles and a unique patented sampling system to
give millisecond response times.
 INSTRUMENTATION WITH WORKING
1.Initialization of the GC
Turn on the Helium carrier gas and air and adjust the pressure
gauges on the instrument.
Turn on the column oven to a high temperature (typically 250
°C or above) to bake in the column. Do not exceed the
maximum temperature of the column. This will remove any
contaminants. Let it bake for at least 30 min before running a
sample.
2. Making a Methods File
In the software controlling the instrument, input all the desired
values for a methods file. First, set the AutoSampler settings.
Set the number of pre-run rinses, post-run rinses, and rinses
with sample. These rinses clean the column between different
samples.
An injector is used to inject the sample into the liner where it
gets evaporated. The amount injected is typically 1 µL. A split
ratio is usually set because injecting all of a sample might
overload the column.
Input the mobile phase parameters. The flow rate is controlled
by the pressure set. Faster flow rates lead to faster separations,
but there is less time for the analyte to interact with the
column(Retention Time).
Enter the temperature programming. For an isothermal
run(e.g.,Cholesterol), enter the temperature of the separation
and then a time for the separation. For a gradient
elution(e.g.,Fatty Acid), enter the starting temperature and hold
time, the ending temperature and hold time, and the ramp
speed in °C/min. An equilibration time is also set that allows the
column to cool back down the original temperature between
runs.
Enter the detector parameters. A detector temperature and
sampling rate will be entered. The detector must always be a
higher temperature than the column temperature so that no
analyte condenses on the detector.
3. Collection of GC Data
Turn on the hydrogen gas and make sure the pressure gauge is
set correctly. Light the flame of the FID.
On the autosampler rack, fill the wash vial with wash solvent,
like acetonitrile or methanol. Make sure the waste vial is empty.
Prepare the sample. If there is any chance of particulates in the
sample, filter the sample. Because plastic residues can
sometimes be seen with GC, use only glass syringes and glass
vials to prepare your sample.
Fill the vial at least half way with sample so the autosampler
syringe is ensured to pick up the sample. Autosampler vials are
typically 2 mL, but if sample volume is limited, vial inserts are
available to reduce the sample volume needed.
Load the sample vial(s) into the autosampler rack. Keep track of
what position each sample is in. Hit the “start” button and make
a file.
Data is typically analyzed with a software program. Parameters
that can be measured include retention time, peak height, peak
area, and number of theoretical plates.

APPLICATIONS
The flame ionization detector (FID) is one of the most used
Detectors for gas chromatography. The application area Is wide.
For example, petrol for airplanes, kerosene, are Carefully
analyzed with the FID as a routine control. The Composition of
the kerosene is of great importance for The energy conversion.
A completely different area is the Packaging of food. Your take-
away hamburger comes in An insulating polystyrene box. During
the processing of Polystyrene, different hydrocarbons are added
to create The end-product. When polystyrene is used within the
food Industry, it is crucial that the product is analyzed for any
Residues of the hydrocarbons, since they can influence the
Quality of the food and harm your health.