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PRELIMINARY
1.1 Background
aromatic rings are composed by carbon and hydrogen atoms (Scott, 2015).
compound. Therefore, the above underlying this paper that contains PAH analysis
Ms?
1.3 Purpose
compounds.
3. To find out How aromatrik polycyclic hydrocarbon analysis using the Gc-
Ms.
CHAPTER II
DISCUSSION
media, including air, water, food, soil, sediment, industrial waste, animal or
human tissue. PAH is composed of two or more benzene rings in a linear array or
exist as a solid yellow-green, white or pale with a distinctive odor. PAH formed
mechanism of formation, PAHs are divided into two different categories. The
categories are pyrolitic and petrogenic form. Petrogenic PAH is their natural
organic materials, crude oil and its products (Arowojolu et al., 2018).
ground, coal mining, and the volcanic area. Another source of PAH are non-
smoking. Cigarettes contain tar levels are quite high and burning tar molecules
reactions of organic material into simple fragments (pyrolysis) and the formation
formed at a relatively low temperature, about 100-150 ° C, but with a much longer
time than the pyrolysis and pirosintesis. PAH is generally very hydrophobic
nature due to its structure which has many aromatic rings which are nonpolar
(Mauro, 2014).
low enough concentrations, whereas high molecular weight PAHs are generally
occurs only in invertebrate sea creatures such as mussels and oysters that are
and fish, PAH molecules in very low concentrations, it can be metabolized further
so as not to contaminate the meat derived from these animals (Mauro, 2014).
US Environmental Protection Agency's list of priority pollutants for PAH are the
They can also pose a potential threat to the marine environment. The effects of
PAHs are usually extensive and permanent in the environment. Most PAH have
phase of motion is usually in the form of an inert gas such as helium or un-
reactive gas such as nitrogen, and the stationary phase is a microscopic layer of
liquid or polymer which is inert and solid, in a glass or metal tube called a column
liquid. Sample flow or berjalanan through a column with a stream of helium gas.
The components in the sample are separated from each other for some time longer
to pass through the column than others. Mass Spectrometry (MS) is used as a
detector for GC. Samples out of the GC column is fragmented by ionization and
time (RT) so that the fragmentation pattern will be formed for a specific
semi-volatile compounds with great resolution, but can not identify it. MS can
provide detailed information about the structure of most of the compounds so that
the components in the sample can be identified correctly, but can not easily
pulses based on its volatility, then by flowing inert gas (mobile phase), which
carries the sample through the stationary phase column. So that would be
sample. These spectra are collected as they exit the column read by the detector
mass ratio (m / z). This spectrum can then be stored on a computer and analyzed
GC-MS consists of two parts, namely gas chromatography (GC) and mass
the compounds in the sample. Separation occurs in the column. The principle of
well as based on interactions with the stationary phase. In the column enacted and
compounds. Compounds that have been separated on the GC column, will enter
the MS. MS consists of three parts, namely the ion source, mass analyzer and
detector. Compounds that enter the MS will undergo ionization and fragmentation
into fragment ions. Ionization occurs because the electrons originating from the
Fragment ions to enter the mass analyzer and will be split based on the
value of m / z her. Fragment ions having m / z values smaller quicker detector will
enter dibandingakan fragment ions having m / z values are great. The output of
the detector in the form of a diagram the relationship between the value of m / z
with the relative intensities of the fragment ions of a compound. Each compound
spectra patterns that exist in the library (Syed and Maqbool, 2014).
2.2.2 Instrumentation
1. gas transporter
Typically the pressure of cylinder of 150 atm. Gas transporter must qualify that
should be inert, does not react with a trailer (trailer solvent and the material in the
detector, and the need to reduce gas diffusion. The gas that is often used is helium,
aargon, nitrogen, carbon dioxide, and hydrogen. Helium and argon is very good,
is not flammable, but very expensive. So sometimes gas that is often used is
carrier gas tube is equipped with output pressure regulator and pressure gauge.
Before getting into the chromatograph, there are accelerometers, gas and
molecular filter system for separating water and other gaseous impurities.
2. injection site
and steam can be entered directly. However, most organic compounds and solid
form of a solution. Thereby compounds in the form of liquids and solids are first
Injection site is always set temperature. The first rule for setting this
temperature is that the temperature of the injection site is about 50 ° C higher than
the boiling point of the mixture of footage which has a high boiling point. Footage
entered into the column by injecting through the injection site. This can be done
by using a hypodermic needle which is often called "a gas tight syringe".
3. Column
There are two types of columns used in GC are boxed column and
capillary column. Column container in the form of a tube made of glass or inert
solids steinnstless suatau berisis packaged neatly. This column has a length of 1.5
to 10 m with a diameter of 2.2 to 4 nm. While the capillary columns are typically
made of silica with a layer of polyamide. Columns of this type usually has a
4. column oven
The column is located inside an oven in the instrument. Oven temperature
should be set and slightly below the boiling point of the sample. If the temperature
is too high, liquid stationary phase can be evaporated, too little sample can be
dissolved in a high temperature and can flow too fast in the column.
5. ion source
In the ion source, the product will be ionized prior to analysis in the mass
spectrometer. Ion source will change into a sample of gas phase ions.
6. mass analyzer
electromagnetic fields.
7. Detector
The detector will detect ion beam emerging from the mass analyzer and
converted into a signal that can be used. The detector is an important element of
mass spectroscopy which produces a signal from ions that are reinforced by
Sediment by GC-MS.
sediment samples from the industrial port in southern Taiwan's Kaohsiung Harbor
of 16 PAH vary. PAH concentration is relatively high in the area of the river
mouth, and gradually decreases towards the harbor area. Diagnostic ratios indicate
that the likely source of PAHs in the industrial port area could come from the
various levels of PAHs exceed the observed effects range median (ERM), and
thus can cause acute biological damage. The results can be used for regular
various industries.
Sampling
Dredge fishing with a boat ride. Immediately after collection, the samples were
scooped into a glass bottle, which was washed with n-hexane and stored in the
refrigerator. Then the samples were transported to the laboratory for analysis. In
the laboratory, the samples were freeze-dried for 72 hours, the soil, filter 0.5 mm
C in glass bottles that had been washed with n-hexane and covered with
benzo [b] fluoranthen (BBF), benzo [k] fluoranthen (BKF), benzo [a] pyrene
(BAP), indeno [1,2,3-cd] pyrene (IP), dibenzo [a, h] anthracene (DA), and benzo
[g, h, i] perylene (BP) in a mixed solution of 80 mg / L obtained from
"AccuStandard Chem. Co. (New Haven, CT, USA) ". Deuterated internal standard
Chrysene 12, and perylene-d 12) at 4,000 mg / L and the replacement standard
AccuStandard Chem.
sample preparation
d 14) solution. Prepared empty tube following the same procedure without adding
sediment samples. Created the standard used for quality control by adding
until homogenised for 1 minute. PAH used for the extraction of ultrasonic
equipment for 15 minutes. Sample tubes were then centrifuged at 2000 rpm for 10
compounds were sucked out with a Pasteur pipette, and the sediment was re-
acenaphthene-d 10, phenanthrene-d 10, Chrysene-d 12, and perylene-d 12) was
added to the extract which was then analyzed using gas chromatography with
Transfer line and ion source temperature of 280 ° C and 200 ° C. The column
using a mass spectrometry (EI) and selective ion monitoring mode (SIM). The
following table picture of the ion monitoring GC-MS conditions at the scheduled
time:
Figure 2. Ion monitoring on GC-MS
result
target compounds were tested with the standard mix of 16 PAH. Figure 3a shows
the total ion chromatogram for this analysis. Identity 16 PAH is confirmed by
properties and the retention time, five internal standard isotope used to monitor
the 16 PAHs. Naphthalene-d8 with a retention time of 7.021 minutes used for NA.
Acenaphthene-d10 with a retention time of 10.495 min is used to ACY, ACE, and
retention time of 15.250 minutes used for PAH in the retention time range 13,50-
21.50 min. Chrysene-D12 is used for CH and baa. Perylene-D12 is used for the
remaining PAH. Figure 3 (b, c) shows the selected ion chromatogram illustrating
how internal standards and standards effective replacement cover 16 PAHs. The
CLOSING
3.1 Conclusion
3.2 Suggestion
from sources more reliable material. And the reader is expected to provide input