NAME; Maitumelo Setlhatshane

ID NO; 202005762
GROUP A; Tuesday and Thursday
WEEK; 6
DATE; 08/Sept/2022
EXPERIMENT 8: GAS CHROMATOGRAPHY
ANALYSIS OF MULTICOMPONENT MIXTURE
ABSTRACT
The sample and alkanes of known concentration were analyzed by gas chromatography. The
retention times of the solutions were used to identify the alkanes present in the unknown mixture.
The retention times of the peaks in the unknown sample were found to be 19.653 which
corresponded to the retention times of decane taken from the chromatography. The component
concentration of each alkane was calculated. Decane were found to be present in the sample with
concentration of 0.19M.
INTRODUCTION:
Chromatography is a popular and an effective method most scientists use to separate the
components within a mixture. Chromatography was first introduced by a Russian botanist,
Mikhail Tswett in 1903. It was first introduced when he separated pigments from a plant to
create beautiful colors through a column of calcium carbonate (Robison and Chymia, 1960). The
separation of components in a solution occurs with a stationary phase and a mobile phase. In the
mobile phase, there can be gas, usually helium or nitrogen. Meanwhile, in the stationary phase, it
can be made up of porous or granular solids, thin film absorbed on a solid or even paper. In gas
chromatography, the stationary phase is a polymer that is coated on the wall of the capillary tube.
One benefit from using the capillary tube is that it speeds up the process of analyzing and
separating the components much faster rather than using packed columns (Jwaili, 2019). A
sample will go through an injection port where helium will mix with said sample. The sample
will then move back and forth from the stationary phase to a mobile phase. To speed up the
process, solvent will be added to force the mobile phase to travel through the columns until the
sample passes through all of the columns (25 meters long) until the sample is eluted. Eluted
compounds are characterized by their retention times, tR, and quantitative analysis is
accomplished by comparing the areas of analyte peaks with those of standard. Chromatography
requires the usage of a thermal conductivity detector to help identify the retention time and peak
area. Peak area will help determine the concentration and the retention time which will help to
figure out the component(s) in the mixture.
The purpose of this experiment is to separate and determine the composition of a mixture of n-
alkanes and identify unknown members of a homologous series by Gas-Liquid Chromatography
(GLC)
LIST OF REAGENTS
 C5-C8 and C9-C12 mixture of alkanes
 Individuals solutions of the above mentioned alkanes
 0.20µl liquid of hydrocarbons mixture containing 0.10% n-hexane and 88.99% n-decane
for FID
EQUIPMENT / APPARATUS
 10.0µl capacity micro-syringes
 Gas Chromatography (with FID)
EXPERIMENTAL PROCEDURE
The GC was turned on according to the instrument manual of the instrument. The temperature of
the column was adjusted to 70ºC using FID while the temperature of the injector to 35 and 40
degrees higher.2µL of acetone was injected and record the chromatogram. The mixtures of C5-C8
and C9-C12 was injected separately which were prepared by pipetting 500µl of each in different
25ml volumetric flasks which were filled to the mark with acetone., and the optimal conditions
was set in each conditions in each case for the best peak resolution. Standard solution(of known
concentration in diethyl ether) was prepared of the individual identified alkanes and 2µL was
injected. The mixture of unknown alkane was also injected and the best peak resolution was
obtained.
RESULTS AND DATA ANALYSIS
TABLE 1;RETENTION TIME FOR ALKANES
Alkanes Retention Width[min] Area[PA*S] Theoretical Concentration(M)
time [min] plate

Pentane 12.312 0.0660 52.55 556787 0.009

Hexane 12.464 0.0753 2.34 438374 0.008
Heptane 13.849 0.0561 1.16×104 975059 0.0068
Octane 15.728 0.0858 2.91×104 537642 0.006
Nonane 17.674 0.0615 6.6×103 1321416 0.005
Decade 19.715 0.0595 5.0×103 1756627 0.0052
Undecane 21.530 0.0731 1.29×104 1387948 0.0047
Dodecade 23.139 0.0433 1.12×103 4569128 0.0044
unknown 19.653 0.0434 4.23×102 3280940 0.19

TABLE 2;RETENTION TIMES OF ALKANE CORRESPONDING TO MIXTURE C5-

C8
a)
RETENTION TIME
C5 12.312
C5-C8 12.257

b)
RETENTION TIME
C6 12.464
C5-C 12.449
c)
RETENTION TIME
C7 13.849
C5-C8 13.840

d)
RETENTION TIME
C8 15.728
C5-C8 15.628

TABLE 3;RETENTION TIME OF ALKANE CORRESPONDING TO MIXTURE C9-C12

a)
RETENTION TIME
C9 17.674
C9-C12 17.628

b)
RETENTION TIME
C10 19.715
C9-C12 19.657

c)
RETENTION TIME
C11 21.530
C9-C12 21.448
d)
RETENTION TIME
C12 23.139
C9-C12 23.108

(i)Peak resolution RS of the two peaks

(a) Using C6 and C8 peaks
2(t R 2−t R 1)
R S=
W 1+W 2

=2(15.728-12.464)/(0.0753+0.0858)
=40.42
ii) Average number of theoretical plates

( )
2
tR
N=16 ×
w

average =
∑ theoritical paltes for all peaks
total number of peaks
13849834.71
average= =1538871 plates
9
iii)HEPT for 90cm column
HEPT=L/N
=90cm/ 153887
=0.000058
iv) Calculations of concentrations of alkanes in the sample
(a)Using hexane peak;
concentration= Moles/volume
Mass=Density×volume
= 0.6606g/mL×0.5ml
0.3303g
Moles=0.330g/86.178gmol-1
3.833×10-3
Concentration of hexane=0.08×(422.48085/32.99369)
=0.03M

(b)Calculation of sample in the unknown mixture

Hexane=concentration of standard×(peak area in unknown/peak area of standard)
=0.08×(12.3802÷32.99369)
=0.03M
Decane concentration=0.0052×(422.68085/11.38740)
=0.19M
(c)Calculation for number of theoretical plates (N)

( )
2
tR
N=16 ×
w

N=16 × ( 0.0753 min)

12.464 min 2
=438374

DISCUSSION
The gas chromatography experiment was done to determine the alkanes present in unknown
mixture of alkanes. Retention time was used to analyze the alkanes present in the unknown
mixture thus finding their concentrations. The retention times of the peaks in the unknown
sample were found to be 19.653 which corresponded to the retention times of decane taken from
the chromatography. The literature value of retention time for decane is 22.9 min and this
correspond to the retention time observed. Flame-ionization detection was used as the detector
which has a number of advantages. Flame-ionization detection, or FID, is widely used because it
senses carbon ions, allowing it to detect virtually any organic compound. The detector is
insensitive to inorganic gases, water, carbon dioxide, sulfur dioxide, nitrogen oxides and other
non-combustible gases., The fact that it requires both compressed air and hydrogen, as well as
carrier gas, can be an inconvenience, especially when instrumental portability is an issue, (Skoon
and Leary, 1992). The disadvantages of gas chromatography are due to the reliance on volatile
compounds. It is not a reliable method for non-volatile substances. The reliance on volatility also
means it must be performed at high temperatures. This means compounds that degrade with heat
can't be analyzed through gas chromatography.Some standards showed multiple peaks of alkanes
which were never present in them, this affected the accuracy of the results. The presence of these
multiple peaks might have been due to contamination of the column as it is known that there is
no an easy way to clean it between injections.

CONCLUSION
The mixture of unknown alkanes was separated successfully with gas chromatography. The
sample was found to contain decade and nonane at concentrations of 14.7% and 5.37%
respectively.
REFERENCES
1. Jwaili, M. (2019) Pharmaceutical Applications of Gas Chromatography. Open Journal of
Applied Sciences, 9, 683-690

2. Robinson, T. (1960). Michael Tswett. Chymia, 6, 146–161.

https://doi.org/10.2307/27757196

3. Bower, N. W. (1992). Principles of instrumental analysis. 4th edition (Skoog, D. A.;

Leary, J. J.). Journal of Chemical Education, 69(8).
https://doi.org/10.1021/ed069pa224.1