EXPERIMENT NO 5

GAS CHROMATOGRAPHY (GC)

MOHD IZWAN IBRAHIM

2011453154
OBJECTIVES
1. To determine the retention time tR of n-butanol and 2-propanol.
2. To identify the components present in a standard mixture based on tR.
3. To identify the component(s) present in an unknown sample.
4. To determine the effect of temperature on tR and Rs.

INTRODUCTION

Chromatographic analysis is used to separate complex mixtures of compounds. First used in

the early 1900s chromatography got its name because it was used to separate different mixtures of
coloured compounds. All chromatographic system have two phases, a mobile phase and a stationary
phase.

The mobile phase is a liquid or gas that carries a sample through a solid stationary phase. As
the sample in the mobile phase passes through the stationary phase the compounds in the mixture
will separate because of differences in their affinities for the stationary phase, and differences in
their solubilities in the mobile phase.

In chromatographic analysis, the eluted compound are characterizes by retention times, tR.
Qualitative analysis involves determination tR of analytes and comparing them with tR standards.
Quantitative analysis is accomplished by comparing the area of the analyte peaks with those of
standard.

APPARATUS

1. Syringe.
2. Beaker.
3. Dropper.

CHEMICALS

1. 2-propanol.
2. N-butanol.
3. Standard mixture of 2-propanol and n-butanol (1:1 ratio).
4. Unknown sample.

PROCEDURE

A. Sample Handling
1. The syringe is rinsed before filled with the sample. After that, the syringe is rinsed again with
small amount of the sample.
2. The plunged is pull to 1microliter. Make sure no air bubbles present in the syringe by press
plunged hard and fast several time before pulled to desire measurement.
 B. Operation of GC
1. The oven temperature is set up at first at:
a. Initial temperature: 70 C
b. Final oven temperature:70 C
c. Injection temperature: 180 C
d. Detector temperature: 180 C
2. Wait until the program in the computer turn to ready.
3. The sample was injected at back injector unit and press start button quickly. After that the
syringe is removed from back injector unit.
4. Wait until retention time is completed then run for 2-propanol, 100 C 2-propanol 140 C
2propanol 100 C n-butanol, 140 C n-butanol,100 n-butanol and unknown sample.

DISCUSSION

In gas chromatography only volatile compound can be used. Volatile compound as

mentioned by Art, 1993 said that Hydrocarbon compounds that have low boiling points, usually less
than 100C, and therefore evaporate readily. Some are gases at room temperature. Propane,
benzene, and other components of gasoline are all volatile organic compounds.

Flame Ionic Detector (FID) are suitable in this analysis because (FID) is the most sensitive gas
chromatographic detector for hydrocarbons such as butane or hexane. With a linear range for 6 or 7
orders of magnitude (106 to 107) and limits of detection in the low picogram or femtogram range, the
FID is the most widely and successfully used gas chromatographic detector for volatile hydrocarbons
and many carbon containing compounds.

The efficiency of a GC column can be increase by lengthen the column and reducing the
column diameter.

Firstly, in the beginning of experiment we run and obtained standard chromatogram of 2-

propanol and n-butanol. From this chromatogram we are able to identify the retention time,tR of the
analyte. This retention time of standard then we will compare the retention time of unknown
sample. Noted that in determining retention time of unknown the temperature and time elapse
must be constant. The process to determining unknown sample firstly, we need to obtain standard
chromatogram. The retention time of 2-propanol is 3.690 minutes while n-butanol is 4.440 minutes.
For the unknown sample the retention time is 3.584 minutes. By comparing all this retention time
we can conclude that the unknown sample is actually 2-propanol. The accuracy of the unknown
sample to the 2-propanol is equal to 97.13%. This percentage can be increase if we reduce time
between injection time and start (running time) of the instrument.

Secondly, when we run the instrument by manipulating the oven (column) temperature on
the standard mixture at the temperature of 70 C, 100 C and 140 C. We observed that the
distribution of the separation is changing from non-overlap (70degree) bands to over-lapping bands
(140 C). This effect can be explained base on temperature of oven. At different temperature it give
read out the different separation even the sample used is same compound. As conclusion, different
compound have their own specific temperature to give out a good separation of chromatogram.
CONCLUSION

As a conclusion we are managed to determine the retention time of n-butanol (4.440mins)

and 2-propanol (3.690mins) and from that we managed to identify the unknown sample is actually
2-propanol besides, we able to explain the effect of temperature on the chromatogram.

REFERENCES

1. http://toxics.usgs.gov/definitions/vocs.html
2. http://www.shsu.edu/chm_tgc/primers/FID.html
3. http://faculty.fiu.edu/~almirall/Lecture21.pdf