Title

Determination of
microextraction

accelerants

in

fire

debris

using

solid

phase

Objective
To determine which accelerants used to fire the wooden chip by using solid
phase microextraction.

Introduction
The use of several techniques to detect accelerants at fire scenes
has attracted a lot of attention from forensic researchers in recent years.
The basic techniques that are currently used to isolate residual accelerants
from fire debris samples collected at fire scenes have been reviewed. The
most commonly used accelerants are petrol, kerosene,thinner and diesel .
These accelerants are generally complex mixtures of hydrocarbon
molecules which have similar chemical properties. However their boiling
points vary and cover a wide range of values. This variation causes the
accelerants to alter their composition during the evaporation process.
Solid phase microextraction (SPME) is a rapidly developing new
technology which is simple, solventless extraction procedure in which a
phase-coated fused silica fiber is immersed in a liquid sample or exposed
to the headspace above a solid or a liquid sample. Analytes adsorbed to
the phase are then desorbed in the injection port of a gas chromatograph
and transferred to a capillary column. Methods developed for the analysis
of organic compounds by SPME-GC have been reviewed. So far, SPME has
been applied to the extraction of organic compounds from different
matrices including air, water and soil. Studies on the forensic applications
of SPME however, are not many and have included extraction of drugs
from blood, detection of ethanol and methanol in body fluids and analysis
of accelerants from aqueous solutions . This work reports on the
application of the SPME technique to the analysis of gasoline and diesel by
their direct extraction from fire debris.

Reagents and Solvents

Accelerants: Kerosene, unleaded petrol, paint thinner and diesel.

Apparatus

SPME holder with 100mm polydimethylsiloxane (PDMS) fiber

Glass vial with septum
Sample
Wood chips

Instruments
Gas Chromatography (Agilent Technologies 6890N) equipped with Flame
ionization detector (FID) and 30 m x 250 m x 0.25HP5-MS capillary
column.

Analytical Procedure
1. Instrument Set-up:
Injector temperature: 250oc
Detector temperature: 280OC
Carrier gas flow rate: 30.0mL/s (nitrogen)
Column Temperature: 60oC to 170oC at 10oC/min

2. Sample Preparation
a. Wood chips were placed into 25 ml conical flask and unknown
accelerants were poured to cover the chip completely. The flask
was capped and leaves the chips to soak for about six hours.
b. After soaking the chips, the excess accelerants were poured out
the flask into a waste container.
c. The wood chips were placed in the glass container. Set fire to the
wood chips (to be done outdoor) and allow to burn until most of
the chips surface was burnt. Extinguish the fire using water
immediately and transfer the semi-charred wood chips into a
glass vial for SPME extraction procedure.

3. Solid Phase microextraction procedure

a. Condition the fiber (100 m polydimethylsiloxane (PDMS) in a GC

injection port at 250oC for the least 10 minutes to remove
contaminants.
b. The sample was heat to 40OC
c. The SPME fiber was exposing to the headspace of the vial for 20
minutes.
d. The fiber was withdraw into the sample, pull out from the vial and
inject into GC-MS immediately with a desorption time 80 seconds.

Identification of accelerants in fire debris

Record chromatograms of several accelerants using SPME method.
Compare the profile of the major components in your fire debris sample to
the profile of the accelerants and identify the accelerant in the fire debris.

Results

Accelerants

Retention Time (minutes)

Kerosene

4.801

Gasoline

4.025

Diesel

9.628

Thinner

1.242

Table 1: Retention time of accelerants

Sample

Retention Time (minutes)

Unknown 3

9.573

Table 2: Retention time of sample

Discussion
The resulting chromatograms obtained by the SPME extraction
method and those from the standard sample injections are compared. GC
Profiles of fire debris samples SPME extracts of the simulated fire debris
samples produced acceptable and identifiable chromatograms.
This
experiment was conducted to identify the type of accelerants used to burn
the sample. The sample used is wooden chip which labeled as Unknown A,
Unknown B, Unknown C and Unknown D. We used Unknown C to be
identified. All the four accelerants which are kerosene, gasoline, thinner
and diesel was heated for 10 minutes at 50 0c. The headspace technique
was used to obtain as many as desired analyte from the accelerants. The
accelerant used to burn the wood chip can be identifying by comparing the
retention time between the sample and the accelerants. Through
chromatogram that obtained, we can conclude that the wooden chip for
Unknown C was burned by using diesel since the retention time is close to
each other. The determination of the type of accelerant present in fire
debris is of great importance in arson cases. This is useful in ascertaining
whether a fire has been started deliberately or not and if so, which type of
accelerant has been used.

Conclusion
We can conclude that the Unknown C is diesel which act as accelerants
that used to fire the wooden chip by using solid phase microextraction.

References
Umi K. Ahmad and Chin K. Voon. (2000). Detection of Accelerants in Fire
Debris using
Headspace Solid Phase Microextraction-Capillary Gas Chromatography.
Malaysian Journal
of Analytical Sciences, Vol. 7, No. 1 (2001) 57-63. Retrieved November
6, 2012, from
http://pkukmweb.ukm.my/mjas/v7_n1/10-umiKahmad.pdf

Experiment 5 and 6:
DETERMINATION OF ACCELERANTS IN FIRE
DEBRIS BY USING SOLID PHASE
MICROEXTRACTION (SPME) AND GAS
CHROMATOGRAPHY-FLAME IONIZATION DETECTOR
(GC-FID)

Name : Nur Zuraihan Binti Abd Wahab (2011856974)

Normahani Binti Ramli (2011603842)

Group : ASB3Ag

Name of Lecturer : Miss Anis

Date of Experiment :

/ 2012