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Naufal Bin Mohd Shukri | 754840 | Group 5

Experiment 15: Gas-Liquid Chromatography Analysis of Organic Compounds


Introduction:
The gas chromatograph works by injecting the sample being studied is injected into a sample
part that heats up and vaporises the sample. Supply of inert N2 gases carry the sample into the
hot separation column that contains a liquid stationary phase covering the inside of the tube.
The sample is separated into its components and is washed into the flame ionization detector.
This detector picks up the data produces a chromatograph. A simplified diagram of the gas
chromatograph is shown in figure 1. Gas chromatograph is suitable for volatile compounds
and hydrocarbons.

Figure 1. retrieved from CHEM20019 Practical Chemistry Laboratory Manual

Aim:
-

To gain experience with the use of Gas-Liquid Chromatography (GLC)


To separate volatile organic molecules from a mixture and determine the relative
amount present in the mixture.

Experimental Method:
Please refer to page 119 of the CHEM20019 Practical Chemistry Laboratory Manual.
Equipment:
Detection
Column (Stationary Phase)
Carrier Gas (Mobile Phase)
Split
Linear Flow
Tinjector
Toven
Tdetector
Injection Volume

Flame Ionization Detector


Alltech EC-wax (30mm x 0.25mm x 0.25 m)
Helium
90:1
30 cm/s
200C
130C
200C
1 L

Naufal Bin Mohd Shukri | 754840 | Group 5

Results and Discussion:


Run No.

Sample
1
2
3

Acetone

Peak No.
1
1
1

Mean
4
5
6

Toluene

1
1
1

Mean
7
8
9

P-xylene

1
1
1

Mean
10

Sample C

11

Sample C

12

Sample C

Mean

Compound

1
2
1
2
1
2
1
2

Retention Time (mins)


1.856
1.861
1.861
1.859333333
2.112
2.107
2.112
2.110333333
2.363
2.357
2.357
2.359
1.856
2.112
1.861
2.112
1.861
2.117
1.859333333
2.113666667

Peak Area
75625920
84266621
85127113
81673218
204734783
197007939
198057593
199933438
227548249
215274962
220372353
221065188
35160858
113827500
33419945
108945737
34846918
113191615
34475907
111988284

Table 1. tabulated results of chromatogram

From the tabulated data above, we can compare the retention times of the peaks in sample C
with the pure compounds and identify the two unknown compounds in the sample. Table 2
below shows that the two compounds in the sample are toluene and acetone.
Acetone
1.86

Mean Retention Time Comparison (mins)


Toluene
Peak 1 in Sample C
Peak 2 in Sample C
1.86
2.11
2.11
Table 2. Comparison of mean retention time

Using the statistical calculations from Table 3, the relative standard deviation (RSD) shows
that the precision of the measurements performed is quite accurate. An RSD of 2.8% and
2.3% means that the sample measurements do not deviate too much from the calculated
means. Potential sources of any errors or inaccuracy comes down human errors when timing
the insertion of the sample and running the GC. Since it is a fairly sensitive equipment, any
slight changes in the timing can result in lower or higher peak areas.

Naufal Bin Mohd Shukri | 754840 | Group 5

Acetone
Toluene

Percentage Composition in Sample C


Sample 10
Sample 11
Sample 12 Mean
43.1%
40.9%
42.7% 42.2%
56.9%
54.5%
56.6%
56%

Standard
C.I. (at 95%)
Deviation
1.17%
422%
1.31%
562%

RSD
2.8%
2.3%

Table 3. Statistical calculations of identified compounds in sample C

Conclusion:
The two compounds identified in sample C are toluene and acetone, with peak 1in the sample
identified as acetone and peak 2 as toluene. Acetone was found to have an average of 42.2%
composition while Toluene had an average of 56% composition.