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Beverages
Maria Salvacion A. Esmalla, M.Sc.
Department of Biochemistry
Faculty of Pharmacy, UST
Objectives
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
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
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
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
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
mL
0.5
1.0
1.5
sample
2.0
2.5
3.0
3.5
4.0
4.5
10
5.0
11
5.5
12
6.0
13
7.0
Mr. A. R. M. Salcedo
Temp
Confirmatory test
Volume of ethanol
% ethanol =
Volume of sample
TEMPERATURE
VOLUME OF DISTILLATE
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
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
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
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
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.