Distillation of Ethanol from Alcoholic Beverage

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.

-it is a physical separation process, and NOT a chemical reaction.

Types of Distillation

Simple distillation - use to separate mixtures of liquids with significant difference in

volatility

Fractional distillation - used when components of a mixture have close boiling points

Steam distillation - the process of separating or purifying a liquid by passing steam

through it

Vacuum distillation - distilling liquid at low pressure so that it boils at a lower boiling point

Simple Distillation Set up

4

1. Distilling flask

2. Distilling head
3

3. Pocket Thermometer 4. Thermometer

2 7 1

5. Condenser

6. Cooling water in
6 8

7. Cooling water out 8. Adapter

9

9. Receiving flask

Fractional Distillation Set up

1. Distilling flask
5

2. Fractionating column 3. Distilling head

8

4. Pocket Thermometer
7 6 9

5. Thermometer 6. Condenser 7. Cooling water in 8. Cooling water out

10

9. Adapter

10. Receiving flask

Boiling Point
- temperature at which the vapor pressure equals the atmospheric pressure

- temperature at which the vapor pressure of a liquid slightly exceeds the pressure of the atmosphere above the liquid
- characterized by vigorous bubbling and churning of the liquid as it vaporizes

- varies significantly with changes in pressure

Effect of Pressure
Daltons Law of Partial Pressure
- the sum of the partial pressures of all the gases equals the total
pressure

PT = P1 + P2 + P3 +

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

Boiling point of pure B Vapor composition line

Liquid composition line

Boiling point of pure A

Liquid-Vapor Phase Diagram

Application
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

20 A 80 B

100 B

COMPOSITION (%)

Application
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

20 A 80 B

100 B

COMPOSITION (%)

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

RESIDUE
- Measure volume remaining in the flask

Precaution:
have the set up check before starting the distillation proper never add boiling chips when the distillation has started the sample will boil over if the heat is not regulated make sure that the calibrated test tubes are clean and dry

Data and Results

Test tube
1 1 2 3 4 5 6 7 8 9 10 11 12 13

mL 0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 7.0

Temp

Confirmatory test

Get the volume of the distillate that will

test positive with the flammability test

Compute the percent ethanol in your

sample Volume of ethanol % ethanol =
x 100

Volume of sample

Measure the volume of sample

remaining in the flask, and add it to the total volume of the distillate (Vaccounted)

Compute the percent loss

% loss = Vol of sample - Vaccounted x 100 Volume of sample

Data and Results

DISTILLATION CURVE

TEMPERATURE

VOLUME OF DISTILLATE

Data and Results

Simple Distillation Curve

Data and Results

Fractional Distillation Curve

Data and Results

Efficiency
GROUP
1 2 3 4 5 6 7 8 9 10

SAMPLE

% EtOH
(Actual)

TYPE

% EtOH
(Experimental)

Fractional Distillation
FRACTIONATING COLUMN

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

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

Fractional Distillation
Theoretical Plates
NUMBER OF THEORETICAL PLATES NEEDED TO SEPARATE A BINARY MIXTURE
Number of TP 1 5 10 50 100 Approx. bp difference (oC) 100 35 20 4 2

Fractional Distillation
Theoretical Plates
CHARACTERISTICS OF SOME FRACTIONATING COLUMN
Type of column Holdup (mL) 1.5 5 9 0.2
Theoretical Plates (TP)

Height of Each TP (cm) 8 4 4 0.4-2

Separable Bp diffrnce (oC) 50 30 30 3-20

Vigreux Glass helices Metal sponge Spinning band

3 6 6 11-61

Azeotropes
- 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

Azeotropes
Types of Azeotropes:
POSITIVE AZEOTROPES - also called minimum boiling mixture - 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 Bptazeotrope = 78.1C
Boiling point of liquid Mr. A. R. M. Salcedo Vapor composition

Azeotropes
Types of Azeotropes:
NEGATIVE AZEOTROPES - also called maximum boiling mixture - 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 Bptazeotrope = 110C
Boiling point of liquid Mr. A. R. M. Salcedo Vapor composition