SCHOOL OF BIOPROCESS ENGINEERING

ERT 318 UNIT OPERATION

LAB REPORT: EXPERIMENT 1
Conduct Continuous Distillation of Isopropanol-Water Mixture at
Minimum Reflux Ratio and Feed Flowrate of 2L/hr. The distillate
contains 0.96 mole fraction of isopropanol.

GROUP MEMBER MATRIX NUMBER

LIEW ONN LI 141141170
NUR SZAZWANI BINTI AZMAN 141141192
MUHAMMAD RIDZWAN BIN RAHMAT 141141180

EVALUATED BY: EN MAHFUZ

CONTENT

1.0 Objective

2.0 Results

3.0 Discussion

4.0 Conclusion

5.0 Reference

6.0 Appendix
1.0 OBJECTIVE

1.1 Determine the experimental purity of isopropanol at the top product.

1.2 Determine the number of theoretical trays using Ponchon-Savarit Method.

2.0 RESULTS

Table 1: Constant volume of distilled water with continue adding with 10ml of isopropanol
Volume of Volume of Mole Fraction Mole Fraction Refractive
isopropanol (mL) water (mL) of isopropanol of Water Index
0 100 0.00 1.00 1.3333

10 100 0.02 0.98 1.3358

20 100 0.04 0.96 1.3412

30 100 0.07 0.93 1.3459

40 100 0.09 0.91 1.3504

50 100 0.11 0.89 1.3533

60 100 0.12 0.88 1.3545

70 100 0.14 0.86 1.3591

80 100 0.16 0.84 1.3608

90 100 0.18 0.82 1.3619

100 100 0.19 0.81 1.3642

Table 2: Constant volume of isopropanol with continue adding 10ml of water
Volume of Volume of Mole Fraction Mole Fraction Refractive
isopropanol water (mL) of isopropanol of Water Index
(mL)
100 0 1.00 0.00 1.3753

100 10 0.70 0.30 1.3756

100 20 0.54 0.46 1.3747

100 30 0.44 0.56 1.3737

100 40 0.37 0.63 1.3733

100 50 0.32 0.68 1.3717

100 60 0.28 0.72 1.3704

100 70 0.25 0.75 1.3691

100 80 0.23 0.77 1.3677

100 90 0.21 0.79 1.3667

Mole fraction calculation

Density x Volume
Mole =
Molar Mass

Mole of component Mole of isopropanol

Mole Fraction = =
Total of mole of mixture (Mole of isopropanol + Mole of water)

Example: To calculate mole fraction of 10ml of isopropanol and 100ml of water

kg 10−6 m3 1000g
(786 3 ) x (10ml x )x( )
m 1ml 1kg
Mole of isopropanol = g = 0.131
60
mol
 kg 10−6 m3 1000g
(1000 3 ) x (100ml x )x( )
m 1ml 1kg
Mole of water = g = 5.556
18
mol

0.131
Mole fraction of isopropanol = = 0.02
0.131 + 5.556

5.556
Mole Fraction of water = = 0.98
0.131 + 5.556

GRAPH OF REFRACTIVE INDEX VS MOLE

FRACTION OF ISOPROPANOL
1.38

1.375
1.3749
1.37

1.365
REFRACTIVE INDEX

1.36
1.3558
1.355

1.35

1.345

1.34

1.335

1.33
0.128 0.52
0 0.2 0.4 0.6 0.8 1 1.2
MOLE FRACTION OF ISOPROPANOL

Figure 1: Standard Curve of Refractive Index versus Mole Fraction of Isopropanol

Table 3: Refractive Index and Mole Fraction of Ethanol
Reflux ratio Sample Refractive Index
Top Bottom
71% 1 1.3748 1.3518
2 1.3749 1.3573
3 1.3750 1.3568
4 1.3747 1.3566
5 1.3751 1.3566
Average 1.3749 1.3558

Calculation of mole fraction of feed

kg 10−6 m3 1000g
(786 3 ) x (4800ml x )x( )
m 1ml 1kg
Mole of isopropanol = g = 62.88
60
mol

kg 10−6 m3 1000g
(1000 3 ) x (7200ml x )x( )
m 1ml 1kg
Mole of water = g = 400
18
mol

62.88
Mole fraction of isopropanol = = 0.14
62.88 + 400

400
Mole Fraction of water = = 0.86
62.88 + 400

Mole fraction of isopropanol feed = 0.14

Mole fraction of water feed = 0.86
Mole fraction based on standard curve
Refractive index of distillate = 1.3749
Mole fraction of isopropanol in distillate = 0.52

Refractive index of bottom = 1.3558

Mole fraction of isopropanol in bottom = 0.128

Reflux at 71% Average refractive Mole fraction of Purity of isopropanol

index isopropanol
Top 1.3749 0.52 52.0%
bottom 1.3558 0.128 12.8%
3.0 DISCUSSION
In this experiment, the continuous distillation on a binary mixture, isopropanol-water mixture was
performed by using a continuous distillation column with 71% reflux ratio.

In the experiment, the binary mixture with 0.14 mole fraction of isopropanol and 0.86 mole
fraction of water is prepared. Isopropanol has the lower boiling point that is 82.6˚C (Dow, 2012)
which is the more volatile component and is serve as light key components in the distillation
column. While, water has higher boiling point (100˚C) which is the less volatile component and is
serve as the heavy key component. Concentration of isopropanol is increasing when moving up
the distillation column as the isopropanol boils faster than water. Therefore, the temperature of
reboiler is set at 90˚C that is higher than the boiling point of light key component and lower than
boiling point of heavy key component so that isopropanol with lower boiling point than water will
be distilled over first. If the temperature is higher than the boiling point of the mixture, then the
vapour or the light key component will not condensed in the distillation column before it reached
the condenser (Saville, 2011).

A sample of mixture 40% v/v isopropanol and 60% v/v of water was prepared. 8 litres of
mixture solution was put in reboiler and another 4 litres was put in feed tank. The column was then
heated to steady state. Firstly, the reflux percentage set to 71% and the reboiler boiled, the top and
bottom product is taken at the interval of ten minutes for six times to measure it average refractive
index by using the refractometer. Due to our careless mistakes, we did not label one of the samples,
we cannot differentiate which is top or bottom product, so we only have five top and bottom
product. The average refractive index of five top product is 1.3749 while the average refractive
index of five bottom product is 1.3558. The bottom product got from the reboiler is hot, hence it
must be cooled down before analysing the refractive index. The distillation has set up a calibration
curve in order to determine the weight fractions of the top and bottom products at the reflux
percentage of 71% via refractive index. Hence, the standard curve of refractive index versus mole
fraction of isopropanol is plotted.

Based on the graph of standard curve of refractive index versus mole fraction of
isopropanol, increasing the mole fraction of isopropanol in sample will increase the refractive
index and eventually become constant at the mole fraction of 0.6. Based on the standard curve, the
mole fraction of distillate (top product) is 0.52 when the refractive index of isopropanol in distillate
is 1.3749, while the mole fraction of bottom is 0.128 when the refractive index of isopropanol in
bottom is 1.3558. The purity of isopropanol for the top and bottom are 52.0% and 12.8%
respectively.

Before this experiment, the minimum reflux ratio is 2.5 by using Ponchon-Savarit method
by assuming the feed mole fraction is 0.4. For our result, we fail to conduct experiment that the
distillate contains 0.96 mole fraction of isopropanol. We only contains 0.52 mole fraction of
isopropanol. This is due to our mathematical calculation problem, we calculate the mole fraction
of isopropanol wrongly. This causes we use the minimum reflux ratio incorrectly.

In the experiment, we are using Ponchon-Savarit method to find the theoretical tray. Two
graph are needed, that are enthalpy of mixture of isopropanol and water in liquid and vapour state
and vapour-liquid equilibrium for isopropanol-water. Firstly, the equilibrium curve and the
enthalpy concentration diagram for the mixture to be separated is drawn. Secondly, after the
compositions of the feed, distillate and bottom products are known, these compositions are located
on the enthalpy concentration diagram. Thirdly, the composition of feed is touched to HL line and
then one line is drawn downward to VLE diagram and then the line is drawn upward until the Hv
line. The point that intersect the Hv line is called HG. Since the point of HF and HG are known, then
one tie line can be drawn. The tie line is extended to the composition of distillate, the point is called
Q’. The tie line is also extended to the composition of bottom product, the point is called Q’’.
Lastly, the number of theoretical plates is then determined by application of the straight line
relationship on the H-x-y diagram and the equilibrium data of the y-x diagram. (Fractional
Distillation using Enthalpy-Concentration Method, 2012). From this experiment, we only can get
three theoretical trays in rectifying section. In stripping section, we have one theoretical tray. In
reboiler section, we cannot get any theoretical tray since the mole fraction of bottom product is
0.128 so near with that of feed which is 0.14. The tray line is exceed the mole fraction of bottom
product so there is no contain theoretical tray. The total theoretical trays is 4.

There are few precaution steps to improve the experiment and prevent the accident
happened. First, the temperature used in the experiment must be different with the boiling point
of azeotrope mixture so that the mixture is able to separate by distillation column. Second, the
temperature of all trays inside the column must be higher than the boiling point of the light key
component (isopropanol) during the experiment. Hence, the vapour produced in the column will
not condensed back to liquid before reaching the condenser. Third, the glove is needed when
collecting the bottom product from the reboiler since the solution is hot. Fourth, make sure that
the isopropanol-water mixture, top products and bottom product are in room temperature before
placing it on the refractometer. This is because of the temperature of liquid droplets may affect
the value of refractive index.

4.0 CONCLUSION

As a conclusion, the binary mixture of isopropanol-water can be separated by using

continuous distillation with ratio percentage of 71%. For the experimental result, the refractive
index for the top and bottom product are 1.3749 and 1.3558 respectively. By referring the standard
curve obtained from experimental result, the mole fraction of isopropanol in top and bottom
product are 0.52 and 0.128 respectively. The purity of isopropanol for the top and bottom are
52.0% and 12.8% respectively. The total number of theoretical trays obtained is 4. In rectifying
section, there has 3 theoretical tray while there has 1 tray in stripping section.
5.0 REFERENCES

Baker E.M.: Equilibria in Isopropanol-Water System at Atmospheric Pressure. Ind.Eng.Chem.

Ind.Ed. 34 (1942) 1501-1504.

Dow (2012). Technical Data Sheet of Isopropanol. Retrieved on 2012 from

http://msdssearch.dow.com/PublishedLiteratureDOWCOM/dh_08ac/0901b803808aca73.pdf?file
path=oxysolvents/pdfs/noreg/327-00031.pdf&fromPage=GetDoc

Encyclopedia of chemical engineering equipment (n. d.). Retrieved on July 23, 2007 from
http://encyclopedia.che.engin.umich.edu/Pages/SeparationsChemical/DistillationColumns/Distill
ationColumns.html

Fouad M Khoury (2005). Multistage Separation Process, Parks Library, United States(US), Boca
Raton, FL : CRC Press, 2005.

Fractional Distillation using Enthalpy-Concentration Method (n.d). Retrieved on July 25,

2012 from http://ihome.ust.hk/~kexhu/ceng3210/221-05.pdf

Gumilir.A. (n. d.). Basic Theory Distillation. Retrieved on September 2, 2009 from
http://chemeng-processing.blogspot.my/2009/02/basic-theory-distillation.html

Housam Binous, Nadhir A. Al-Baghli, and Brian G. Higgins, Wolfram Demonstrations Project,
"Ponchon-Savarit Diagram for an Isopropanol-Water Binary Mixture" . Retrieved on January 17,
2012 from
http://demonstrations.wolfram.com/PonchonSavaritDiagramForAnEthanolWaterBinaryMixture/

Saville. G.. Thermodynamics of Binary systems. Retrieved on February 2011 from

http://www.thermopedia.com/content/582/

Tham M.T. (n. d.). Basic Distillation Equipment and Operation. Retrieved on 1997 from
http://www.istitutofermiverona.it/LEZIONI/distil/distileqp.htm