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ADAMSON UNIVERSITY

College of Engineering
Chemical Engineering Department
M a n il a

Experiment no. 2

STEAM DISTILLATION

Submitted by:
Lavilles, Francis Dominic
Lee Gee Hyun
Lojica, Kathlyn Joyce M.

Date performed: July 18, 2015


Date submitted: July 27, 2015

ABSTRACT:
Steam distillation is an important method of separating immiscible liquids. This
experiment aims to observe a steam distillation process. In order to observe the steam
distillation process, toluene-water system was used in the study. A simple steam
distillation set up was used in the experiment. The distillation was made and the
temperature was recorded when the total volume of the distillate in the receiver has
reached certain corresponding amounts. The results showed that as the temperature
increases, the pressure also increases for toluene, water and mixture. The value of the
pressure for the mixture was between the values of the pressure of toluene and water. The
pressure versus temperature or toluene water and the mixture was plotted. Near accurate
results of the temperature at each volume of the distillate was obtained. The steam
distillation process was observed comprehensively in this experiment.

INTRODUCTION:
Immiscible liquids are liquids that do not mix to give a single phase. When two
immiscible liquids are boiled, they will boil at temperature lower than the boiling point of
either of the pure liquids. Steam distillation is a useful process of separating immiscible
liquids. In this process, a liquid which is immiscible with water is distilled using steam.
Steam distillation works on the principle that in a mixture, there is a point where
two liquids become immiscible. In this mixture system, the total vapor pressure deviates
from Raoult's Law prediction. Adding the vapor pressure of two liquids comprising the
binary mixture system will result to vapor pressure of the system. The mole fraction of
each liquid in the binary system will not affect the vapor pressure. Also at the boiling
point of the mixture, dividing the partial pressures of the compound in the vapor will
result to the ratio of the vapor pressures of the pure liquids. In this experiment, steam
distillation of the toluene - water system was done. The study aims to examine the steam
distillation process of the toluene - water system.

pA
pB

pA
pB

NAP
= NBP

NA
NB

nA
nB

wAMB
wBMA

>>

wA
wB

MApA
MBpB
REVIEW OF RELATED LITERATURE:
Substances with different volatilities can be separated by distillation. The process
of distillation was first developed by Jabir ibn Hayyan. In modern times, distillations are
widely applied in labortory scale, industial distillaton, distillation of herbs for perfumery
and medicinals, and food processing. Steam distillation is used for compounds that are
heat sensitive. Steam is bubbled through a heated mixture of the raw material. The
vaporization of the target substance can be described by using Raoult's Law.
Steam distillation has many applications. In a recent study, steam distillation is
used to obtain laurel extract (Zekovic, et. al.). In another study, the steam distillation of
essential oils from Lemon Grass was examined (Amenaghawon, 2014). Steam distillation
of essential oils was also investigated in other studies (Mulvaney, et. al.). Another study
probe the extraction of essential oil from Cinnamon (Cinnamomum zeylanicum). The
influence on the quality of essential lemon oil by distillation process is determined by a
recent study (Gamarra, et. al.)
There are also advance ways of performing the distillation of mixtures like
benzene and toluene.(Phiyanalinmat, 2015). Some advance methods use algorithms to
determine the optimum reflux ratio (Abolpour and Mohebbi, 2014)
In mixtures that involve more than two components, more complicated processes
are needed in detection and separation of substances. A complex sample of benzene,
toluene, ethylbenzene and xylene requires a hybrid separation and detection device for
analysis as examined in recent researches (Iglesias et. al. , 2009). When benzene and
toulene mix with other comopund like xylene, the concentrations are dtermined using
advance process such as High Performance Liquid Chromatography-UV detection
(HPLC-UV) (Bahrami, et. al.)

Process simulation has been applied in a recent study to design the benzene-toluene
distillation (Phiyanalinmat, 2015). Another study presented modeling and simulation of a
benzene recovery process by extractive distillation (Brondani, et. al., 2015)

METHODOLOGY:
A steam distillation set-up was prepared. Eighty milliliters of toluene was placed
in the round bottom flask and water was filled in the distilling flask up to half of the
flask. The distilling flask was heated until the water boiled. When it started to boil, the
flame has been lowered just enough to continue the boiling. The first distillate (2-3mL)
was disposed. The temperature was recorded and the receiver was placed back under the
adapter. The distillation and recording of temperature was continued until the distillate in
the receiver was 2.5ml, 5ml, 7.5ml, 10ml, 12.5ml, 15ml, 17.5ml, 20ml, 22.5ml, 25ml.
Distillation was stopped when the collected distillate had reached 25ml. The distillates
were cooled and were left to separate fully. Each of the distillate were transferred in the
graduated cylinder to measure the volume of water and toluene. The data for vapor
pressure of toluene and water in different temperatures (40c,50c,60c,70c,80c,90c) was
obtained from the handbook. The vapor pressures of the mixture at those temperatures are
computed. The vapor pressures of toluene-water and the mixture was plotted. The
theoretical boiling point of the mixture was determined from the plot. The theoretical
composition of the distillate was also obtained from the plot.

RESULTS AND DISCUSSION:


The pressure v.s temperature graph of toluene and water mixture was made after
applying Raoult's Law to the mixture. As the temperature increases, the pressure also
increases for toluene, water and mixture. The values of the pressure for the mixture were
between the values of the pressure of toluene and water.
The use of steam distillation in extracting inorganic liquids has many advantages.
In the steam distillation process, the water vapor transfer small amounts of the vaporized

substance to the condensation flask where the separation of condensed liquids occurs.
This allows easy collection. Normal distillation of inorganic liquids will require high
temperature. Some of these molecules will be broken up by heating at high temperature.
Using steam distillation avoids this because the required temperature is low.
It is not possible to carry out steam distillation at 100 c because the boiling point
of the water is 100 degree celcius so the water will boil if the temperature exceeds 100
degree celcius. In steam distillation, the pressure of the two components must add up to
1atm.

Table 1: Temperature and vapour pressure of water, toluene, and the mixture.
Temperature ( )

Vapor

40
50
60
70
80
90

Toluene
59.16
92.11
138.96
203.75
291.22
406.74

Pressure

of Vapor

Pressure

Pressure
55.33
92.58
149.44
233.89
355.78
527.42

of Vapor

Pressure

Mixture
55.89
92.51
147.92
229.51
346.40
509.89

Table 2: Volume and boiling point of Distillate


Volume (ml)
Temperature
( )

2.5
36

5
36

7.5
34

10
34

12.5
34

15
34

17.5
34

20
33

22.5
34

25
-

of

Table 3: Volume, mole fraction and volume percent of the mixture


Volume

of Volume

Mixture
2.5
5
7.5
10
12.5
15
17.5
20
22.5
25
Volume

water
0.2
0.8
1.5
1.8
3.8
5.6
10
17.4
22.5
of Mole

Mixture

of

2.5
5
7.5
10
12.5
15
17.5
20
22.5
25

0.85
0.85
0.85
0.85
0.85
0.85
0.85
0.85
0.85
-

of Volume

of Mole of H2O

Toluene
2.8
4.2
6
8.2
11.2
9.4
7.5
2.6
0
fraction Mole fraction

Mole

0.011
0.044
0.083
0.1
0.21
0.31
0.56
0.97
1.25
Volume %

of toluene
0.0019
0.0076
0.014
0.017
0.036
0.053
0.094
0.16
0.2
Volume %

of Toluene

Of

Of

0.15
0.15
0.15
0.15
0.15
0.15
0.15
0.15
0.15
-

H2O
8
16
20
18
25.33
37.33
57.14
87
100
-

Toluene
92
84
80
82
74.67
62.67
42.86
13
0
-

H2O

P vs T graph
600
500
400

toluene
water

pressure 300
200

mixture

100
0
30

40

50

60

70

80

90

100

Temperature

Fig.1 Pressure v.s. Temperature of Toluene, Water and Mixture

CONCLUSIONS AND RECOMMENDATION:


In the conduct of experiment, the process of steam distillation was observed. The
steam distillation of the binary system of toluene and water was examined. A plot of
pressure versus temperature for toluene, water and the mixture was made and was
studied.
The researchers recommended that careful measures must be taken so that there will
be no leakage during the distillation process. This must be done in order to get better
results.

REFERENCES:
1. Zekovic Z.P., Lepojevic Z.D., Mujic I.O., 2009, Laurel Extracts Obtained by Steam
Distillation, Supercritical Fluid and Solvent Extraction. Journal of Natural Products. Vol.
2, pp 104-109
2. Amenaghawon N.A., Okhueleigbe K.E., Ogbeide S.E., and Okieimen C.O. 2014.
Modelling the Kinetics of Steam Distillation of Essential Oils from Lemon Grass
(Cymbopogon Spp.)International Journal of Applied Science and Engineering 2014. 12,2:
pp 107-115
3. Iglesias R.A., TsowF ., Wang R., Forzani E.S., Tao N,. 2009 Hybrid Separation and
Detection Device for Analysis of Benzene, Toluene, Ethylbenzene, and Xylenes in
Complex Samples. Journal of Analytical Chemistry, 2009, 81 (21), pp 89308935
4. Abolpour B., Mohebbi A,. 2014. Optimization of the reflux ratio of benzene-toluene
stage distillation columns by the Cuckoo algorithm. Petroleum Science, 2014, Vol. 11,
Issue 3, pp 446-453
5. Mulvaney J., 2012. Essential Oils and Steam Distillation. Journal of the New Zealand
Association of Medical Herbalists 2012
6. Wong Y.C., Ahmad-Mudzaqqir M.Y., and Wan-nurdiyana W.A., 2014. Extraction of
Essential Oil from Cinnamon (Cinnamon zeylanicum). Oriental Journal of Chemistry,
2014, Vol. 30, No. 1
7. Gamarra F.M.C, Sakanaka L.S., Tambourgi E.B., Cabral F.A., 2006. Influence on the
Quality of Essential Lemon (Citrus aurantifolia) oil by Distillation Process. Brazilian
Journal of Chemical Engineering, 2006, Vol 32, No. 01, pp 283-291
8. Bahrami A., Mahjub H., Sadeghian M., Golbabaei F., 2011. Determination of Benzene,
Toluene and Xylene (BTX) Concentrations in Air Using HPLC Developed Method
Compared to Gas Chromatography.International Journal of Occupational Hygiene 2011
9. Phiyanalinmat S., 2015. Design of Benzene-Toluene Distillation for the Minimum
Energy Consumption by Chemical Process Simulation. Department of Inustrial

Chemistry, Faculty of Science, Thailand. 17th Regional Symposium on chemical


Engieering.
10. Brondani L.B., Flores G.B., Soares R.P., 2015. Modeling and Simulation of a
Benzene Recovery Process by Extractive Distillation. Brazilian Journal of Chemical
Engineering, 2015, Vol. 32, No. 01, pp. 283 - 291

APPENDIX:

Vapor Pressure for Toluene


log 10 ( P mmHg )=6.95464

1344.8
40 +219.482

PmmHg =59.16 mmHg


Vapor Pressure for Water
log 10 ( P mmHg )=6.95464

1750.286
40 +235

PmmHg =59.16 mmHg


Vapor Pressure for Mixture
0.8547 ( 55.33 mmHg )+ 0.1453 ( 59.16 mmHg ) =55.89mmHg
Mole of Water
0.2ml (1

g
)
ml

g
18
mol

=0.011 mole

Mole of Toluene
0.2ml (0.87

g
)
ml

g
92.14
mol

=0.0019mole

Mole fraction of water


0.011 mole
=0.85
0.011 mole+0.0019 mole

Mole fraction of Toluene


0.0019 mole
=0.15
0.011 mole+0.0019 mole
Volume Percentage of Water

0.2
x 100 =8.00
0.2+ 2.3
Volume Percentage of Toluene
2.3
x 100 =92.0
0.2+ 2.3

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