CHE 3323

Lab 4: Observing composition in batch distillation

Instructors: Dr. El Awad Osman and Raza Ali

Member of the group:

- Raim Amer H00391461
- Reem Almuhairi H00391609
- Amna Jumaa H00395626

Objective:
- Observing how composition of a water and methanol mixture changes in a batch
distillation.

Introduction:
Distillation is a physical separation that is done between two or more liquids, the
driving force for this separation is the difference in boiling points. The two types of
distillation are continuous and batch, they are selected based of the composition variation. In
batch distillation the composition changes regularly as for continuous there is only a slight
change in composition. Some general applications that batch distillation are used for are
solvent recovery and pharmaceutical. The objective of this lab is to observe the composition
of methanol and water mixture. The main parts of a batch distillation set up are distillation
flask, condenser and receiving flask. The condenser has a water inlet and outlet, the inlet is at
bottom and the outlet is at the top, the reason for that is to make sure that the condenser will
be full of cooling water. The distillation flask holds the mixture and the receiving flask will
hold the methanol since it has a lower boiling point. We will be finding the experimentally
mole fraction of methanol in the distillate then compare it to the calculated one. Then get the
mass fraction of methanol and water by finding the number of moles then convert them into
mass using molecular weight and lastly dividing the given compound with total mass to get
the mass fraction.

1
 Figure 1: schematic of set up

Procedure:

1. Prepare the distillation apparatus for batch distillation.

2. Measure 200 g of CH3OH and 225 g of water and stir them.
3. Put the mixture in a pot and toss in some boiling chips, then calculate X1, L1(R1), L2(R1).
4. Make sure the condenser is full of water and that there are no air bubbles between the fluid layers.
5. For energy supply, turn on the heat.
6. Allow it to run for 30 to 40 minutes to establish a steady condition.
7. After reaching a steady state collect the distillate sample in liquid form.
8. Turn off the heat source and the water supply and cool the sample.
9. Find (L1-L2) and L2 in grams
10. To determine the distillate composition, use a refractometer to analyze the sample.
11. Find the average distillate mole fraction of methanol experimentally.
12. Determine the equivalent mole fraction of methanol X2 by analyzing a sample from the remaining
solution in the still for refractive index.

Reading and Experiment data:

2
L1 = Initial number of moles.

L2 = Final Number of moles remaining.

X1 = Initial Mole fraction of methanol.

X2 = Final Mole fraction of methanol.

Yav = Average mole fraction of metanol in the composited distillate.

L1 in g= 425g

L1 in moles =18.75mole

L1 in (RI)=1.344

L2 in (RI)=1.339

X1= moles of methanol/ total moles

X1=6.25mole/18.75mole=0.33

126mlx0.719g/ml= 90.6g

(L1-L2)g=90.6g

=425-90.6=334.4g

L2=334.4g

3
Data table:

Since, RI for distillate L 2=1.339

Yav from the given graph =0.156

4
L1 X1 = L2 X2 +(L1-L2) Yav
(425) (0.33) = (334.4) (X2) + (90.6) (0.156)
X2 = 0.377 moles

Sample calculations:

Mass fraction= mass of sample /Total mass

Mass fraction of CH3OH = mass CH3OH / Total mass =12.064/ 23.278= 0.52

Mass fraction of H2O = mass H2O / Total mass =11.214/ 23.278= 0.0.48

Component Number of moles Mass Mass Fraction

CH 3 OH X2 * =0.377 = X2 ×MMmethanol =12.064g 0.52

H2O 1-X2 = 0.623 = (1-X2 ) × MMwater= 11.214g 0.48

Total 1 23.278g 1

Sample calculations:

Compare the calculated to the experimental found value of

Mass fraction of methanol in the residue = 0.156
L2 = 334.4 g

Methanol:
Mass fraction of methanol in the residue = mass fraction of methanol (L 2)g
Mass fraction of methanol in the residue = (0.52) (334.4g) =173.888g
Moles of Methanol in Residue = Mass of Methanol in Residue / 32
Moles of Methanol in Residue = 173.888 / 32 = 5.434mol

Water:
Mass fraction of water in the residue = mass fraction of water (L2)g
5
Mass fraction of water in the residue = (0.48) (334.4g) =160.512g
Moles of Water in Residue = Mass of Water in Residue / 18
Moles of Water in Residue = 160.512 / 16 = 8.9173mol

Total moles of residue = L2 = 5.434 + 8.9173 = 14.3513 moles

Find Yav using the formula:

L1X1 = L2X2 + (L1 – L2) Yav
(18.75)(0.33)=(14.3513)(0.377)+(18.75-14.3513)Yav
Yav =0.1767

Discussion:
The purpose of our experiment is to Observe how composition of a water and methanol mixture
changes in a batch distillation in addition, to compare between experimentally mole fraction of
methanol in the distillate and the calculated mole fraction. Doing the experiment result in having
1.339 of distillate composition using the refractive index. Using the value of distillate requires to find
the Y average from the graph of mole fraction verses refractive index which equals 0.156, the Y
average helps us to find out X2 mole fraction of methanol using the equation “L1 X1 = L2 X2 +(L1-
L2) Yav “ which result in 0.377moles. Then by using mass fraction of methanol and water residue we
will find the mole fraction of both residues using the formula of “mole of sample / Total mole” then
apply the values on the formula of “L1 X1 = L2 X2 +(L1-L2) Yav” to get the calculated Y average which
equals 0.1767. Based on the two values of Y average we conclude that the calculated Y average is more
accurate than the value of experiment Y average even that there is small different between them,
maybe because in the experiment Y average not get the actual reading of refractive index which will
effect the value of Experiment Y average.

Conclusion:
In conclusion, this experiment aims to identify the composition of residue and collected distillate in batch
distillation usin methanol-water mixture, it was successfully achieved by following the right procedures, we
were able to find the average distillation mole fraction experimentally and compare it to the theoretical value
we obtained the errors that affected the reading and that the theoritcal one is more accurate, in addition ensure
the apparatus setting is perfectly done to avoid unwanted values and make sure to wipe off the refractometer
from any dust or remaining solution before putting the desired sample, when performing the experiment make
sure to be careful when you’re near the apparatus as its fragile and expensive.

6
References
- Lab instructor
- Class notes