Result and Discussion
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Transcript of Result and Discussion
Result and Discussion:
In SPME process, there are some factors that
need to be considered such as the thickness of
fibre, agitation method and the conditioning of
fibre. Longer extraction time needed with the
use of thicker fibre but it provide better
recoveries. The extraction time and the relative
number of analytes extracted are independent of
the concentration of the analytes (Vas and
Vékey, 2004). The extraction time can be
reduced with use of proper agitation method
such as stirring, ultrasonics and heating. With
the use of proper agitation, the extraction time
depends on the geometry of the fibre and the co-
efficiency of the analyte diffusion in the fibre.
Before the extraction proceeded, the PDMS
fibre needs to be conditioned in a GC injection
port. In this experiment, the PDMS fibre was
conditioned at 250˚C for 10 minutes (Dr.
Nor'ashikin et al, 2012). This step is necessary
as it can remove any contaminants at the fibre.
The chromatograms obtained from the
experiments concerning the influence of type of
accelerant are shown in Figures 2 – 4.
Figure 1: GC-MS chromatogram of blank cotton cloth sample.
Figure 2: (Top) Chromatogram of a petrol standard. (Bottom) Chromatogram of a petrol fire debris sample
Figure 3: (Top) Chromatogram of a diesel standard. (Bottom) Chromatogram of a diesel fire debris sample
Figure 4: (Top) Chromatogram of a kerosene standard. (Bottom) Chromatogram of a kerosene fire debris sample
SPME extracts of the simulated fire debris samples produced acceptable and identifiable
chromatograms. However, it is difficult to characterize petrol and kerosene in fire debris based
on the chromatogram only because the chromatogram obtained was not identical to the standards
and too complex. The complexity of the chromatogram in Figure 2 indicates that petrol is
composed of a wide range of different compounds. Petrol was seen to be composed of aliphatic
and aromatic hydrocarbons. The chromatograms obtained for diesel standard remain
recognizable, but differ slightly for fire debris samples.
For each accelerant, five major volatile compounds with high quality were selected based
on the library search of mass spectrometry. The different volatile organic profiles characterized
the accelerants are presented in Table 1 – 7.
Table 1: Volatile profile of blank by SPME-GC-MS
Retention time (tR)
Volatile Compounds
Area (%)
Quality (%)
9.474 Benzoic acid 6.55 90
9.726 Naphthalene 5.83 93
12.449 Biphenyl 6.24 93
14.064Phenol, 2,4-bis (1,1-dimethylethyl)
13.34 97
17.290 Phenanthrene 3.93 96
Unsoaked cotton cloth was set as a blank in this analysis to ensure that materials other than the
material being analysed do not contribute to the identification. Table 1 simplify the five major
compounds found in blank fire debris.
Table 2: Volatile profile of standard petrol by SPME-GC-MS
Retention time (tR)
Volatile Compounds
Area (%)
Quality (%)
4.109Benzene, 1,3-dimethyl
1.06 97
5.952Benzene, 1-ethyl-2-methyl
0.71 95
6.189Benzene, 1,3,5-trimethyl
4.73 94
12.650Naphthalene, 2,6-dimethyl
1.81 97
16.5831,4,5,8-Tetramethyl
naphthalene0.67 93
Table 3: Volatile profile of fire debris sample soaked in petrol by SPME-GCMS
Retention time (tR)
Volatile Compounds
Area (%)
Quality (%)
4.835Benzene, 1,3-dimethyl
0.75 97
6.214Benzene, 1-ethyl-2-methyl
2.95 94
6.500Benzene, 1,3,5-trimethyl
0.70 91
12.794Naphthalene, 2,6-dimethyl
0.63 97
16.0211,4,5,8-Tetramethyl
naphthalene0.13 97
In the chromatograms of petrol fire debris, signals of alkyl derivate of benzene were
observed to have high peak area. This is similar to the standard petrol as shown in Table 2. The
volatile compounds found in standard petrol have large area compared to one in fire debris. It
can be said that some of the compound has been used up for combustion.
Table 4: Volatile profile of standard diesel by SPME-GCMS
Retention time (tR)
Volatile Compounds
Area (%)
Quality (%)
6.210Benzene, 1,2,2-trimethyl
0.56 90
7.889 Undecane 2.40 95
12.214 Tetradecane 4.72 94
13.510 Pentadecane 3.52 96
14.988 Hexadecane 1.13 94
Table 5: Volatile profile of fire debris sample soaked in diesel by SPME-GCMS
Retention time (tR)
Volatile Compounds
Area (%)
Quality (%)
6.722Benzene, 1,2,2-trimethyl
0.18 95
8.370 Undecane 1.11 93
12.667 Tetradecane 4.88 89
13.926 Pentadecane 3.22 94
15.093 Hexadecane 2.30 94
Major volatile compound found in diesel fire debris are alkanes such as Undecane,
Tetradecane, Pentadecane and Hexadecane as listed in Table 4. Examination of fire debris
revealed the presence of residual diesel in different relative amounts and retention time as
compared to the standard diesel oil.
Table 6: Volatile profile of standard kerosene by SPME-GCMS
Retention time (tR)
Volatile Compounds
Area (%)
Quality (%)
4.038 o-Xylene 3.20 95
4.412Benzene, 1,3-dimethyl
1.31 97
6.100Benzene, 1,2,4-trimetyl
2.67 90
6.182 Decane 3.38 78
7.332Benzene, 1,2,4-trimetyl
1.81 91
Table 7: Volatile profile of fire debris sample soaked in kerosene by SPME-GCMS
Retention time (tR)
Volatile Compounds Area (%) Quality (%)
4.735 o-Xylene 0.49 89
5.089 Benzene, 1,3-dimethyl 0.19 68
6.892 Benzene, 1,2,4-trimetyl 4.66 43
6.892 Decane 4.66 55
12.574Decahydro-4,4,8,9,10-pentamethyl
naphthalene1.07 97
For kerosene, differences in quantitative ratios of alkyl derivates of benzene can be observed.
This can be explained by the influence of fire conditions or, more probably, by changes in
kerosene composition. Still, the characteristic pattern of alkyl derivates benzene, considered
being kerosene’s ‘fingerprint’, thats enabling identification.