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ABSTRACT:
boiling points; it was deemed that retention time is proportional to boiling point.
Secondly, the effect of flow rate of the carrier gas on isothermal separation of the
BTEX mixture was observed; 40 cm/s (24 m/min.) was deemed to be the ideal carrier
gas flow rate. By the variation of temperatures, it was determined that higher
temperatures increased resolution but not significantly, and that it must be kept
constant. With the aid of internal standards, the concentrations of the constituents of
BTEX were calculated to be benzene: 536.8 ppm, toluene: 682.4 ppm (inaccurate),
ethylene + m,p-xylenes: 566.8 ppm (b.p.’s are to close) and o-xylene: 48.1 ppm. The
benzene, 6880 ppm of toluene, 3820 ppm of ethylbenzene, 3420 ppm of m/p-xylene,
INTRODUCTION:
phase. Each constituent of the mixture has a characteristic affinity for the immobile
rate, thus is carried out by the solvent system and/or carrier gas at a characteristic rate.
The analyte present in the solvent or eluent is known as the mobile phase and the
opposite as stationary phase. These rates are dependant on physical factors, which this
carry through the analyte, dissolved in hexane and or bromobenzene, through the
column (passageway). The different constituents of the analyte separate and are
The first section of the experiment measures the effect of the speed of the
carrier gas’ flow rate on the retention times (rate of ad/desorption) of the analyte’s
constituents. The second section measures the effects of the column’s temperature on
the retention times, the selectivity (affinity for the stationary to the mobile phase of
the constituents in comparison with one another) of the analyte’s constituents and
resolution. The third seeks to quantify the concentrations of the analyte’s constituents.
xylenes) standard and gasoline, dissolved in hexanes with 1,000 ppm bromobenzene.
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EXPERIMENTAL:
collecting the chromatogram data. The oven temperature was set at 55 oC and the
carrier gas (He) flow rate at 30 cm/s (18 m/min.). Subsequently, 1000 ppm standards
of benzene, toluene, ethylbenzene, xylenes (ortho, meta and para) and bromobenzene
were run singly through the column. Upon collecting the chromatogram data of these
xylenes) was run. Next, the carrier gas flow rate was varied to values of 15 cm/s (9
m/min.), 20 cm/s (12 m/min.), 25 cm/s (15 m/min.), 40 cm/s (24 m/min.) and 50 cm/s
(30 m/min.) and the respective chromatogram data(s) measured. The analyte was,
The second section of the experiment was commenced with resetting the
carrier gas flow rate to 30 cm/s. The 1000 ppm BTEX standard was run at varying
temperatures of 35 oC, 55 oC and 75 oC. Next, the BTEX standard was run under a
Under identical temperature ramp settings, BTEX standards of 100, 500, 1000
and 2000 ppm concentrations were run through the column. The experiment was
boiling point
(oC)
hexanes 69
benzene 80
toluene 110
ethylbenzene 136
p-xylene 138
m-xylene 138
o-xylene 143
bromobenzene 155
! graph depicting retention times (min.) for the compounds analysed under
typical conditions
! &!
! GC 1: Q3
! 0.003004926 13.858
!/avg. (%) 1.170092396 2.590
! t $2
where N = # R &
"W %
L
H= ; where L = 30 m
N
tr ' tm
k'=
tm
area of toluene
!1000 ppm
area of bromobenzene
! GC 1: Q4
He flow rate
u (m/min.) H (=L/N)
(m/min.)
9 7.594 0.0004369
12 10.390 0.0004945
15 12.590 0.0001412
18 14.903 0.0005184
24 20.547 0.0002012
30 25.231 0.0003383
As can be seen from the graph and the table previously, the optimum solvent
The first three values cannot be considered since the general trend of Van
! GC 2: Q1, Q3
difficult to separate them; hence the rise in resolution as the temperature is raised to
that of the boiling point of hexanes and close to that of benzene, two components in
! *$!
the BTEX mixture (though hexane is the solvent). Temperature programming allows
are more accurately separated at lower temperatures and vice versa. However, this
trend is not seen clearly in the data. As the temperature rises and the lower b.p.
components are more accurately separated, the resolution is high but when it is kept
constant at 75 oC, it is reduced (this temperature is far from the b.p.’s of the heavier
! GC 3: Q2
The 1000 ppm sample of BTEX was deemed to provide the best resolution and was
the known concentration of the bromobezene internal standard of 1000 ppm, as shown
previously).
" Ethylbenzene + m/p xylenes: 566.8 ppm (due to their approximate b.p.’s, they
! GC 3: Q3
conc.
abundance component
(ppm)
DISCUSSION:
! GC 1: Q2
Generally, the greater the molecular weight of the molecule, the higher its
boiling point (b.p.) and the longer its retention time, since the molecule is not so much
! GC 1: Q5
o-xylene was relatively easier to separate from the the meta and para forms;
but the meta and para forms of xylene were more difficult to separate from
ethylbenzene since there is a lesser difference amongst the boiling points of these than
with o-xylene.
! GC 3: Q1
unknowns are measured against those of the standard, the concentration of which e.g.
CONCLUSION:
It was observed that the ret. times were proportional to the boiling points of
the compounds tested. The variation of carrier gas flow rate saw 40 cm/s to be the
most viable rate, providing the lowest H-value. By varying the temperatures, it was
determined that resolution was raised slightly as lower boiling fractions e.g. hexanes
and bezene were prevented from contributing to the chromatogram. Lastly, the
resolved) and o-xylene: 48.1 ppm. The concentrations of these components in the
gasoline sample were 9274 ppm of benzene, 6880 ppm of toluene, 3820 ppm of