Introduction:

When dealing a situation in experimenting a certain analyte from a compound,

chromatographic method is used to obtain the desired analyte from the rest.
Chromatography is done by dissolving a sample in a mobile phase which is either liquid or
gas which is forcefully passes through a stationary phase. The mobile and stationary phase
has difference in polarity since it can attract an analyte with certain degree of polarity to
either phase. Thus, difference in retention time is resulted on how long an analyte stay inside
the system. If it more soluble in mobile phase, thus the retention time is much shorter since
the analyte exits the system quicker. In gas chromatography, the mobile phase utilizes gas
carrier as the mobile phase. The sample is injected in small amount into the system, which
turned into gaseous form by the high temperature of the injection port. The gas carrier mixes
with the gaseous sample which is passes through the long column. The gas used for the
mobile phase is inert to ensure no reactivity happen between the gas carrier and the analyte,
thus preventing loss of analyte. In partitioning a compound, there are two ways done in gas
chromatography; temperature programming or isothermal elution. Normally, temperature
programming is preferred due to better resolution of the peak. The mixture of gaseous
sample and gas carrier is passed through the column, where the analyte would or not sticks
to the surface of the column due to the polarity. Analyte with or no polarity would stay longer
or shorter due to the condition of the stationary phase or mobile phase, thus affecting the
time taken for the analyte to expel out from the system to the detector which it detects the
amount of analyte over a set period. From this detection, the peak is given.

In this experiment, a GC-FID (Flame Ionization Detector) is used which it good at detecting
organic compounds. The FID uses a mixture of hydrogen and air as a fuel to burn the
effluent from the column. The effluent is ignited which is then produces ion which needed in
conducting electricity for the detector to detect.
Purpose:

To determine the retention time of naphthalene in lubricant oil (Petronas and Shell oils)

Procedure:

Standard Preparation

About 5mg of naphthalene is weighed and dissolved in a small amount of dichloromethane

in a beaker. It is then transferred into a 50mL volumetric flask and diluted to the calibrated
mark with dichloromethane. The mixture is injected into a small vial by usage of syringe with
0.5 millipore filter attached to it.

Sample Preparation

There are two sample used; 2T oil (Shell oil) and lubricant oil (Petronas oil). Each sample is
prepared from each stock solution about 10mg of respective oils which are dissolved in
dichloromethane in 100mL volumetric flask (100ppm solution). From these stock solutions,
1ppm solution is prepared by pipetting 0.5mL of each stock into 50mL volumetric flask and
filled to the calibrated mark with dichloromethane solution. Again, they are injected into small
vial by the usage of syringe with millipore filter attached to it.
Setting:

Initial temperature 40oC

Hold time 2 Minute
Ramping temperature 20oC per Minute
Final temperature 200oC
Hold time 5 Minute
Index setup
Mode Splitless
Injection temperature 250oC
Flow 1.6 mL/min

Data:

Sample Retention time, TR

(min)
Standard Naphthalene 1.687
Naphthalene in Petronas Oil 1.479
Naphthalene in Shell Oil 1.503

Discussion

The experiment starts with the preparation of standard which made from 5mg of naphthalene
which is dissolved in dichloromethane in 50mL volumetric flask. Small amount of the solution
is injected through the millipore filter to filter out any fine un-dissolved particles, to prevent
column damage. It is tested with the GC-FID device which the data and peak for the
naphthalene is obtained for the comparison with sample oils. The naphthalene peak is
observed at the retention time of 1.687 minutes, thus is set aside for the sample testing.

The samples involve Petronas and Shell oils since naphthalene exists in fractionation of
crude petroleum oil. In its preparation, 10mg of respective oil are dissolved in
dichloromethane in 100mL volumetric flask which marked as 100ppm solution. From this
solution, 1ppm solution is made by pipetting 0.5mL of each stock into 50mL volumetric flask
and filled to the calibration mark with dichloromethane. It is then tested and the compared
with the standard data.

From the comparison of these sample oils with the standard naphthalene, the naphthalene
in Petronas oil have retention time of 1.479 minutes while in the Shell oil, 1.503 minutes. The
reason of such difference is may lies in the temperature programming setting since the oils
has several components in it which affects the separation of analyte with the rest of the
chemicals in the oil. The other reason is that different oils made by different companies
which have certain rule or specification on the composition of the chemicals inside the oil,
thus the content of naphthalene within are differ from the rest of the samples. Therefore
qualities of these oil samples are largely different, specifically in fuel burning efficiency in
motorized vehicles.

Conclusion

The retention time for the naphthalene in Petronas and Shell oils are 1.479 and 1.503
minutes respectively.

References

1. Notes of Petroleum Industries, CMT 307 by Mdm Faridah Hanum Hj Badrun

2. Notes on Gas Chromatography, CHM 260 by Mdm Faridah Hanum Hj Badrun
3. Notes on Instrumental Analysis, CHM 312
4. Flame Ionization Detector, http://en.wikipedia.org/wiki/Flame_ionization_detector
5. Gas Chromatography, http://en.wikipedia.org/wiki/Gas_chromatography
6. Explanation on GC-FID, http://www.shsu.edu/~chm_tgc/primers/FID.html