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Submitted to: Ma’am Hina

Submitted by: Nimra Shabbir


Registration no: 19-Arid-1309
Subject: Organic Chemistry
Subject code: BCH 302
Group no 7
Analysis of hydrocarbon in common fuels is done
by SPME (Solid phase Micro extraction) and
Gas chromatography.
 SPME:

 Sample used were petrol, diesel, thinner and


unknown.
 It is basically a solid phase extraction sampling
technique.
 Solid-phase microextraction, or SPME, is solid
phase extraction sampling technique that involves
the use of a fiber coated with an extracting phase,
that can be a liquid (polymer) or a solid which
extracts different kinds of analytes (including
both volatile and non-volatile) from different kinds
of media, that can be in liquid or gas phase.
 The quantity of analyte extracted by the fibre is
proportional to its concentration in the sample as
long as equilibrium is reached or, in case of short
time pre-equilibrium, with help of convection or
agitation.
 The advantage of SPME is that the extraction is fast
and simple.
 It can be done usually without solvents, and
detection limits can reach parts per trillion (ppt)
levels for certain compounds.
 SPME also has great potential for field
applications, on-site sampling can be done even by
nonscientists without the need to have gas
chromatography-mass spectrometry equipment at
each location.
 When properly stored, samples can be analyzed
days later in the laboratory without significant loss
of volatiles.
 After extraction, the SPME fiber is transferred
to the injection port of separating instruments,
such as a gas chromatography and mass
spectrometry where desorption of the analyte
takes place and analysis is carried out.
 The fiber was conditioned in the GC injection
port at 2500 degree Celsius for at least 10
minutes to removed contaminants.
 The sample is added in a glass vial and then
vial is placed on a hot plate and sample was
heated to 500 degree Celsius while agitate it by
using magnetic stirrer.
 Then the SPME fiber was exposed to the
headspace of the vial for 20 minutes.
 After that the fiber was withdraw into the
needle and pulled out from the vial and
immediately injected into GC with desorption
time 80 seconds.
 After desorption period, the needle was
withdrawn from the injection port and
chromatography process continued.
 After the chromatogram was obtained, the
major compounds in each sample were
identified using the mass spectra library.
 For instance, if unleaded petrol was used as
sample the results obtained will give the
concentration of Toluene, Ethyl benzene and P-
Xylene.
 It is a process of separating components from
the given crude drug by using a gaseous
mobile phase.
 It involves a sample being vaporized and
injected onto the head of the chromatographic
column. The sample is transported through the
column by the flow of inert, gaseous mobile
phase. The column itself contains a liquid
stationary phase which is absorbed onto the
surface of an inert solid.
 Gas-solid chromatography
(stationary phase: solid)
 Gas-liquid chromatography

(stationary phase: immobilized liquid)


Advantages of Gas Chromatography:
 The technique has strong separation power and
even complex mixture can be resolved into
constituents.
 The sensitivity of the method is quite high.
 It gives good precision and accuracy.
 The analysis is completed in a short time.
 The cost of instrument is relatively low and its
life is generally long.
 The technique is relatively suitable for routine
analysis.

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