COURSE CODE: CHM510

NAME: NURUL HUSNA BINTI IBRAHIM

NO MATRIC: 2018226626
TITLE EXPERIMENT: EXPERIMENT 4: ANALYSIS OF
HYDROCARBONS IN COMMON FUELS USING SOLID-PHASE
MICROEXTRACTION (SPME) AND GAS
CHROMATOGRAPHY-MASS SPECTROMETRY (GC-MS)
LECTURER’S NAME: MADAM ZARILA
LABORATORY PARTNER’S NAME:
1. HUSNA AFIFAH BINTI RAZALI (2018801414)
2. NUR AMIRAH BINTI AHMAD (2018801966)
3. FATIMAH AZZAHRAH BINTI MOHD FAIRUZ
(2018414328)
INTRODUCTION
Solid-phase microextraction (SPME) is a solid phase extraction sampling technique that
involves the uses of a fiber coated with an extracting phase, which can be either liquid or a
solid. SPME can extracts different kinds of analytes including both volatile or non-volatile
from different kinds of media, that can be in liquid or gas phase. SPME is an alternative to
the conventional liquid-liquid extraction (LLE) technique. It is rapid, inexpensive and
solventless technique for the isolation of organic compounds from gaseous, liquid or aqueous
and solid samples. In the analysis the solid-phase microextraction (SPME) and capillary gas
chromatography or mass spectrometry (GC-MS) was developed for the identification of
volatile compounds (hydrocarbon) in fuel. The sample used was unleaded petrol, diesel, paint
thinner and unknown. Factors effecting the SPME performance are the coating material, pH
sample, thickness of fiber, salt addition and extraction procedure.
OBJECTIVE
The objective of the experiment is to identify the major chemical constituents in petrol,
diesel, thinner, and unknown compound using solid phase micro extraction and gas
chromatography mass spectrometry detector.
APPARATUS
1. Micro reaction vials (5ML)
2. Glass dropper
3. Beaker 100ML
EQUIPMENT

1. Solid Phase Micro Extraction Holder

2. Solid Phase Micro Extraction Fiber – PDMS 100 UM
3. Hot plate
4. Thermometer
5. Steel rod and clamp
SAMPLE
- Unleaded petrol
- Diesel
- Paint thinner
- Unknown
INSTRUMENT
Gas chromatograph (Agilent Technologies 5890 Series II) equipped with HP5971A mass
spectrometry detector (MSD) and 30 m × 250µm × 0.25µm HP5-MS capillary column
PROCEDURE
A. Instrument set-up (may vary depending on instrument)

Injection temperature: 250°C

Detector temperature: 300°C
Column temperature: 60°C to 170°C at 10°C min-1
Carrier gas flow rate: 30 cm sec-1

B. SPME Procedure

i. PDMS fibre in a GC injection is set at 250°C (10 minutes) to remove

contaminants
ii. 2.0 mL of sample is added in a glass vial with septum and the vial is placed in
a water bath (in beaker) on a hot plate. The sample is heated to 50°C. The
sample is agitating by using the magnetic stirrer.
iii. The SPME fibre is exposed to the headspace of the vial for 20 minutes.
iv. The fibre is withdrawn into the needle, the vial is pull out and is injected
immediately into the GC-MS with a desorption time of 80 seconds
v. The major compound in each sample and unknown is identify by using the
mass spectra in NIST library.
DATA AND RESULTS
A. Major compound presence in petrol sample

Retention time/ Area/ % Quality Compound

min
8.901 0.94 74 Benzene 1-methyl-2-(2-
propenyl)

9.445 0.57 87 Azulene

 2.876 29.98 70 Toluene

11.037 0.33 97 Naphthalene 1-methyl

B. Major compound in diesel sample

Retention time/ min Area/ % Quality Compound

13.627 8.79 89 Pentadecane

14.378 4.31 97 Naphthalene. 2,3,6-trimethyl

14.931 1.22 96 4,6,8 trimethylazulene

12.318 8.73 95 Tetradecane

C. Major compound in thinner sample:

Retention time/ min Area/ % Quality Compound

2.689 100.00 94 Toluene

D. Compound in unknown sample:

Retention time/ min Area/ % Quality Compound

2.592 11.94 83 Toluene (in thinner, petrol)

14.318 0.96 98 4,6,8 trimethylazulene (in diesel)

13.561 3.42 93 Pentadecane (in diesel)

6.332 5.36 90 Benzene 1,2,3-trimethyl

 12.818 6.52 95 Naphthalene 2,6-dimethyl (in petrol)

12.262 3.38 93 Tetradecane

11.699 0.93 95 Naphthalene 1,2,3,4-tetrahydro-1,4-

dimethyl

DISCUSSIONS
In this experiment, we need to identify the main components in petrol, diesel, thinner and the
unknown compound using solid-phase micro extraction and gas chromatography mass
spectrometry detector. Based on the results that we obtained, we can conclude that there are 4
major compounds contains in petrol are benzene 1-methyl-2-(2-propenyl), azulene, toluene
and naphthalene 1-methyl which lies between minutes 2 until minutes 11 of retention time. In
the 12th minutes until 14th of retention time in diesel compounds indicates the major
compounds which are pentadecane, naphthalene 2,3,6-trimethyl, 4,6,8-trimethylazulene and
tetradecane. For thinner, unlike the others its only contain one major compound which is
toluene at 2.689 min. In order to analyse the unknown sample, we need to compare from all
the 3 individuals. The unknown sample shows major compounds such as toluene, 4,6,8-
trimethylazulene, pentadecane, benzene 1,2,3-trimethyl, naphthalene 2,6-dimethyl,
tetradecane and naphthalene 1,2,3,4-tetrahydro-1,4-dimethyl. Therefore, we can conclude that
the unknown sample is a mixture of petrol, diesel and also thinner because it contains toluene
at 2nd retention time, which also can be found in petrol and thinner. The major compound
4,6,8-trimethylazulene also found at 14.318 in diesel. It is the same for pentadecane in the
unknown sample that also found in diesel. Naphthalene 2,6-dimethyl also found at 12.818
retention time which confirmed that the compound is present in petrol.
CONCLUSION
The identification of major compounds in each sample has been identified based on the
results that we obtained. Benzene 1-methyl-2-(2-propenyl), azulene, toluene and naphthalene
1-methyl are the major compound that is found in petrol while in diesel we found
pentadecane, naphthalene 2,3,6-trimethyl, 4,6,8-trimethylazulene and tetradecane. While for
thinner, it only contains toluene. Therefore, we can conclude that the unknown sample is a
mixture of petrol, diesel and also thinner because there are some similarities of compounds
appear in the sample.
REFERENCES
1. Zhu, H., Zhu, J., Wang, L., & Li, Z. (2015). Development of a SPME-GC-MS method for
the determination of volatile compounds in Shanxi aged vinegar and its analytical
characterization by aroma wheel. Journal of Food Science and Technology, 53(1), 171–
183. doi:10.1007/s13197-015-2035-5 

2. http://fareastzareul1994.blogspot.com/2018/05/experiment-4-analysis-of-
hydrocarbons.html
3. Frauenhofer, E., Cho, J., Yu, J., Al-Saigh, Z. Y., & Kim, J. (2019). Adsorption of
hydrocarbons commonly found in gasoline residues on household materials studied by
inverse gas chromatography. Journal of Chromatography A, 1594, 149-159.