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Distillation of Alcoholic

Beverages
Maria Salvacion A. Esmalla, M.Sc.
Department of Biochemistry
Faculty of Pharmacy, UST

Objectives

Separate the components of alcoholic beverage using


distillation

Construct a distillation curve

Calculate the percent ethanol in the alcoholic beverage

Compare the efficiency of simple and fractional distillation in


separating liquid mixture

Distillation
process of heating a liquid until its more volatile
constituents pass into the vapor phase, and then cooling
the vapor to recover such constituents in liquid form by
condensation.
the main purpose of distillation is to separate a mixture
of several components by taking advantage of their
different volatilities, or the separation of volatile materials
from nonvolatile materials.

Types of Distillation
Simple Distillation
Used to separate mixtures of liquids with a large difference
in volatility

Fractional Distillation
Used when liquids have close boiling points
Repeated distillation

Steam Distillation
Passing steam through liquid mixture

Vacuum Distillation
Distilling at a low pressure for components to boil at lower
boiling point
Useful for compounds that degrade at high temperatures

Simple Distillation Set-up


4

5
7

1
8
6

1.
2.
3.
4.
5.
6.
7.
8.
9.

Distilling flask
Distilling head
Thermometer packet
Thermometer
Condenser
Cooling water in
Cooling water out
Adapter
Receiving flask

Fractional Distillation Set-up


5

4
8
3

7
6

10

1.
2.
3.
4.
5.
6.
7.
8.
9.
10.

Distilling flask
Fractionating column
Distilling head
Thermometer packet
Thermometer
Condenser
Cooling water in
Cooling water out
Adapter
Receiving flask

Vapor Pressure
is the equilibrium
pressure of a vapor
above its liquid
As temperature
increases vapor pressure
also increases

Boiling Point
Temperature at which
vapor pressure equals
atmospheric pressure
(1 atm)
Varies significantly
with pressure
Characterized as
vigorous bubbling of
liquid as it vaporizes

Daltons Law
Total pressure is equal to the sum of the
partial pressures of all gases
PT = P1 + P2 + P3 + P4 +

Raoults Law
For liquid mixtures, the partial pressure of
liquid A (PA) is equal to the vapor pressure of
the pure liquid A (PA) multiplied by its mole
fraction (XA) in the mixture
PA = XAPA
For mixture of liquid A and B,
PT = PA + PB= XAPA + XBPB

Liquid-Vapor Phase Diagram


Shows the temperature at which a mixture with a
certain composition starts to boil
Boiling point of pure B
Vapor composition line

Liquid composition line


Boiling point of pure A

Liquid-Vapor Phase Diagram


100

T
E
M
P
E
R
A
T
U
R
E

90

80

100 A

80 A
20 B

60 A
40 B

40 A
60 B

COMPOSITION (%)

20 A
80 B

100 B

Liquid-Vapor Phase Diagram

Methodology
15 mL of test sample
+ boiling chips

distill
Stop when:
* the temperature reaches 100C
* the volume of the sample remaining in
the flask is approximately 1-2 mL

DISTILLATE
- Collect 0.5 mL using the calibrated test tubes
- Record the temperature for each fraction
collected
- Perform flammability test
Mr. A. R. M. Salcedo

RESIDUE
- Measure volume remaining in the flask

Boiling Chips
Porous rock that releases bubbles of
entrapped air to the solution being heated
Prevents bumping
Promotes smooth boiling
Porcelain, glass, unglazed clay, alumina
Do not add boiling chips when solution is hot

Data and Results


Test
tube

mL

0.5

test positive with the flammability test

1.0

Compute the percent ethanol in your

1.5

sample

2.0

2.5

3.0

3.5

Measure the volume of sample

4.0

4.5

remaining in the flask, and add it to the


total volume of the distillate (Vaccounted)

10

5.0

11

5.5

12

6.0

13
7.0
Mr. A. R. M. Salcedo

Temp

Confirmatory test

Get the volume of the distillate that will

Volume of ethanol
% ethanol =

Volume of sample

Compute the percent loss


% loss =

Vol of sample - Vaccounted


Volume of sample

Data and Results


DISTILLATION CURVE

TEMPERATURE

VOLUME OF DISTILLATE

Simple Distillation Curve

Fractional Distillation Curve

Comparison of Results
GROUP
1
2
3
4
5
6
7
8
9
10

SAMPLE

% EtOH
(Actual)

TYPE

% EtOH
(Experimental)

Fractional Distillation

Fractional Distillation

Fractional Distillation
EFFICIENCY
- refers to how well a fractionating column can separate
components of a liquid mixture

- depends on:
Length
Packing material
Reflux ratio

- reported in theoretical plates

Theoretical Plates
- is the number of steps needed to bring about a specified
degree of separation of two components in a mixture.

Theoretical Plates
NUMBER OF THEORETICAL PLATES NEEDED TO SEPARATE
A BINARY MIXTURE
Number of TP

Approx. bp difference (oC)

100

35

10

20

50

100

Theoretical Plates
CHARACTERISTICS OF SOME FRACTIONATING COLUMNS
Holdup
(mL)

Theoretical
Plates
(TP)

Height of
Each TP
(cm)

Separable
Bp diffrnce
(oC)

1.5

50

Glass helices

30

Metal sponge

30

Spinning band

0.2

11-61

0.4-2

3-20

Type of column

Vigreux

Azeotropes
Greek for no change in boiling
is a mixture of two or more solvents in such
a ratio that its
composition cannot be
changed by simple distillation
when boiled, the resulting vapor has the
same ratio of constituents as the original
mixture of liquids
also known as constant boiling mixtures

Positive Azeotropes
also called minimum boiling azeotrope
boils at a lower temperature than any
other ratio of its constituents
strong intermolecular attraction with
similar molecules

azeotrope

Example: 95.6% ethanol / 4.4% water


BptetOH = 78.4C
Bptwater = 100C

Mr. A. R. M. Salcedo

Bptazeotrope = 78.1C
Boiling point of liquid
Vapor composition

Negative Azeotropes
also called maximum boiling
azeotrope
boils at a higher temperature than
any other ratio of its constituents

azeotrope

strong intermolecular attraction with


different molecules
Example: 20.2% hydrogen chloride / 79.8% water
BptHCl = -84C
Bptwater = 100C
Boiling point of liquid
Vapor composition

The End
Nothing is as hard as it looks;
everything is more rewarding than
you expect; and if anything can go
right it will and at the best possible
moment.

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