Chem 31.1 Experiment 4: Distillation
Transcript of Chem 31.1 Experiment 4: Distillation
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DISTILLATIONDISTILLATION
A laboratory technique used in separation and/or purification of components in a
mixture
The process is mainly based upon the boiling point of liquid substances
Experiment IV: Distillation
heating vaporizing condensing
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DISTILLATIONDISTILLATION
liquid
Experiment IV: Distillation
homogeneous heterogeneous
liquid
mixtures
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RAOULT’S LAWRAOULT’S LAW
It relates the vapor pressure of components to the composition of the solution
Experiment IV: Distillation
for ideal mixtures
It assumes ideal behavior, that is, the physical properties of the components
are identical
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RAOULT’S LAWRAOULT’S LAW
Experiment IV: Distillation
If the two components are very similar, or in the limiting case, differ only in isotopic content,
then the vapor pressure of each component will be equal to the vapor pressure of the pure
substance Po times the mole fraction in the solution
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RAOULT’S LAWRAOULT’S LAW
The total vapor pressure Ptot above the solution is equal to the sum of the vapor pressures of
the two [liquid] components, PA and PB
Experiment IV: Distillation
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RAOULT’S LAWRAOULT’S LAW
Experiment IV: Distillation
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RAOULT’S LAWRAOULT’S LAW
Experiment IV: Distillation
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RAOULT’S LAWRAOULT’S LAW
Experiment IV: Distillation
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RAOULT’S LAWRAOULT’S LAW
Vapor Pressure
Experiment IV: Distillation
It is the pressure exerted by a vapor in equilibrium with its non-vapor phases
Boiling Point
The temperature at which the vapor pressure equals the atmospheric pressure
Boiling PointVapor Pressure 1/1/αα
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AZEOTROPE MIXTUREAZEOTROPE MIXTURE
A mixture of liquids that has a constant boiling point because the vapour has the same
composition as the liquid mixture
Experiment IV: Distillation
The components of the solution cannot be separated by simple distillation
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AZEOTROPE MIXTUREAZEOTROPE MIXTURE
POSITIVE AZEOTROPEMinimum Temperature
Maximum Pressure
Experiment IV: Distillation
NEGATIVE AZEOTROPEMaximum Temperature
Minimum Pressure
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POSITIVE AZEOTROPE MIXTUREPOSITIVE AZEOTROPE MIXTURE
Experiment IV: Distillation
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NEGATIVE AZEOTROPE MIXTURENEGATIVE AZEOTROPE MIXTURE
Experiment IV: Distillation
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KINDS OF DISTILLATIONKINDS OF DISTILLATION
Simple Distillation
Experiment IV: Distillation
Fractional Distillation
Steam Distillation
for homogeneous mixtures
for heterogeneous mixtures
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AZEOTROPE MIXTUREAZEOTROPE MIXTURE
Ethanol
Experiment IV: Distillation
Water
95.5% 4.5%
78.1°C100°C78.3°C
positive azeotrope mixture
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SIMPLE DISTILLATIONSIMPLE DISTILLATION
It is usually used only to separate liquids whose boiling points differ greatly (>70°C) or to separate liquids from involatile solids or oils. In
the process, all the hot vapors produced are immediately channelled into a condenser
which cools and condenses the vapors
Experiment IV: Distillation
Therefore, the distillate will not be as pure
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SIMPLE DISTILLATIONSIMPLE DISTILLATION
A simple distillation set-up consists of a boiling flask (round-bottom flask) attached to an
adapter holding a thermometer (to determine the boiling temperature of the liquid). The
adapter connects to a condenser into which cold water is constantly passed through. The condenser leads into a collection flask for the
purified liquid.
Experiment IV: Distillation
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SIMPLE DISTILLATIONSIMPLE DISTILLATION
Experiment IV: Distillation
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SIMPLE DISTILLATIONSIMPLE DISTILLATION
Experiment IV: Distillation
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FRACTIONAL DISTILLATIONFRACTIONAL DISTILLATION
It is usually employed with separation of complex mixtures at small boiling points
difference (about 25°C). It can separate the mixture into its component parts or fractions
Experiment IV: Distillation
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FRACTIONAL DISTILLATIONFRACTIONAL DISTILLATION
It is essentially the same as simple distillation except that a fractionating column is placed between the boiling flask and the condenser. The glass beads
found in the fractionating column provide "theoretical plates" on which the refluxing liquid can condense, re-
evaporate, and condense again, essentially distilling the compound over and over. The more volatile
liquids will tend to push towards the top of the fractionating column, while less volatile liquid will stay
towards the bottom, giving a better separation between the liquids
Experiment IV: Distillation
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FRACTIONAL DISTILLATIONFRACTIONAL DISTILLATION
Experiment IV: Distillation
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FRACTIONAL DISTILLATIONFRACTIONAL DISTILLATION
Experiment IV: Distillation
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SIMPLE vs FRACTIONAL DISTILLATION SIMPLE vs FRACTIONAL DISTILLATION
Experiment IV: Distillation
Simple distillation Fractional distillation
Advantages • simpler setup than fractional• faster distillation times• consumes less energy than fractional distillation
•much better separation between liquids than simple distillation•can more readily purify complex mixtures than simple distillation
Disadvantages • requires the liquids to have large boiling point differences (>70oC)• gives poorer separation than fractional distillation• only works well with relatively pure liquids
• more complicated setup than simple distillation• takes longer for liquids to distil• consumes more energy than simple distillation
Best used for: separating relatively pure liquids with large boiling differences or liquids with solid impurities
separating complex mixtures of liquids with smaller boiling point separations.
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SIMPLE vs FRACTIONAL DISTILLATION SIMPLE vs FRACTIONAL DISTILLATION
Experiment IV: Distillation
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STEAM DISTILLATIONSTEAM DISTILLATION
It is the process of purifying a substance through application of steam. It deals with compounds that are
heat sensitive (e.g. natural aromatic compounds). Steam distillation works on the principle that
immiscible substance when mixed together can lower the boiling point of each other.
Experiment IV: Distillation
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STEAM DISTILLATIONSTEAM DISTILLATION
0.864g/mL Xylene
Experiment IV: Distillation
Water 0.988g/mL
60% 40%
94.5°C100°C139.1°C
positive azeotrope mixture
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STEAM DISTILLATIONSTEAM DISTILLATION
Many organic compounds tend to decompose at high sustained temperatures. Separation by normal
distillation would then not be an option, so water or steam is introduced into the distillation apparatus. By
adding water or steam, the boiling points of the compounds are depressed, allowing them to
evaporate at lower temperatures, preferably below the temperatures at which the deterioration of the
material becomes appreciable
Experiment IV: Distillation
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STEAM DISTILLATIONSTEAM DISTILLATION
Experiment IV: Distillation
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STEAM DISTILLATIONSTEAM DISTILLATION
Experiment IV: Distillation
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STEAM DISTILLATIONSTEAM DISTILLATION
Experiment IV: Distillation
Volume Xylene (mL)
Volume Water (mL)
Weight Ratio
First Fraction
0.5 1.3 0.33 : 1
Second Fraction*
-no data- -no data- -no data-
*the experiment was unsuccessful
σ of xylene = 0.87 g/mLσ of water = 1 g/mL
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GUIDE QUESTIONSGUIDE QUESTIONS
Experiment IV: Distillation
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Explain the differences of the distillation curves between simple distillation and fractional
distillation.
Experiment IV: Distillation
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SIMPLE vs FRACTIONAL DISTILLATION SIMPLE vs FRACTIONAL DISTILLATION
Experiment IV: Distillation
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In the separation of the ethanol from water using fractional distillation, the distillate always
contains about 5% water. Explain.
Experiment IV: Distillation
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t vs. % concentration of ethanol-water mixture
Experiment IV: Distillation
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p vs. % concentration of ethanol-water mixture
Experiment IV: Distillation
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t vs. % concentration of liquid mixture, which does not form azeotrope
Experiment IV: Distillation
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Based on the phase diagram of 4(a), what is the approximate composition of the ethanol-
water mixture, which begins to distill at 80°C?
Experiment IV: Distillation
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At 95°C the vapor pressure of n-heptane is 684 mmHg and of n-octane is 303 mmHg.
Calculate the mole ratio and weight ratio of the two components in a mixture of n-heptane and n-octane, which begins to distill at 95°C at 650
mmHg.
Experiment IV: Distillation
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P sol = 650 mmHg684 x + 303 (1-x) = 650
684x + 303 – 303x = 650x= 0.9107
1-x = 0.089Mole ratio: 0.9107/0.089 = 10.23 (10.23 mols
of n-heptane for every 1 mol of n-octane)Weight ratio: 91.25/10.17 = 8.98 (8.98 g of n-
heptane for every 1 g of n-octane)
Experiment IV: Distillation
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Explain the difference in the values of toluene/water weight ratios between the first
and second fractions.
Experiment IV: Distillation
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Cite some important application of steam distillation and vacuum distillation
Experiment IV: Distillation