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AnaChem Lab 2 - Purifying Organic Compounds

The document discusses different methods for purifying organic compounds including filtration, centrifugation, crystallization, solvent extraction, distillation, fractional distillation, sublimation, and chromatography. It defines each technique and provides examples of laboratory setups and uses in industry.

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G.9 Saharah Gandarosa
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59 views40 pages

AnaChem Lab 2 - Purifying Organic Compounds

The document discusses different methods for purifying organic compounds including filtration, centrifugation, crystallization, solvent extraction, distillation, fractional distillation, sublimation, and chromatography. It defines each technique and provides examples of laboratory setups and uses in industry.

Uploaded by

G.9 Saharah Gandarosa
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PPTX, PDF, TXT or read online on Scribd
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BIOCHEMISTRY LABORATORY

DIFFERENT METHODS OF
PURIFYING ORGANIC
COMPOUNDS
Analytical Chemistry
Laboratory

AND EQUIPMENT
Objectives
At the end of the session, you should be able to:
1. enumerate the different methods of purifying organic
substances.
2. define and explain the different methods of purifying
organic substances.
3. identify the names of the different laboratory apparatus.
4. know the uses of the different laboratory apparatus.
Discussion
• Organic compounds are isolated either from natural
sources or from reaction mixtures.
• These compounds are seldom pure and are usually
contaminated with small amounts of other similar
compounds, which are found to exist together or
formed during the reaction.
• In order to characterize them, it is important to purify
them.
Discussion
• The various steps involved in the characterization of
organic compounds are Purification, Qualitative
Analysis, determination of molecular mass, calculation
of empirical formula and molecular formula, and
elucidation of the structure by various methods
including chemical methods.
Discussion
• The common techniques used for the purification of a
particular compound are based on its nature and on
the nature of the impurities present in it.
• Extraction is a useful technique for separating
compounds that have different polarities.
Discussion
• The compounds to be separated are treated with a
mixture of a polar and non-polar solvent.
• This technique is also used to extract solutes from a
solid.
Purification of Organic
Compounds
• These techniques include:
1. Filtration
2. Centrifugation
3. Crystallization
4. Solvent extraction
5. Distillation
Purification of Organic
Compounds
• These techniques include:
5. Fractional distillation
6. Sublimation
7. Chromatography
8. Steam distillation
Filtration
• To separate an insoluble solid from a liquid
particularly when the solid is suspended
throughout the liquid
• The solid/liquid mixture is called a
suspension
Filtration

The laboratory set-up of filtration


Filtration

• There are many small holes in the filter paper


 allow very small particles of solvent
and dissolved solutes to pass through as
filtrate
• Larger insoluble particles are retained on the
filter paper as residue
Centrifugation
• When there is only a small amount of
suspension, or when much faster
separation is required
 Centrifugation is often used
instead of filtration
Centrifugation
• The liquid containing
undissolved solids is put
in a centrifuge tube
• The tubes are then put
into the tube holders in a
centrifuge

A centrifuge
Centrifugation
• The holders and tubes are spun around at a
very high rate and are thrown outwards
• The denser solid is collected as a lump at
the bottom of the tube with the clear liquid
above
Crystallization

• Crystals are solids that have


 a definite regular shape
 smooth flat faces and straight edges
• Crystallization is the process of forming
crystals
1. Crystallization by Cooling a Hot
Concentrated Solution
• To obtain crystals from an unsaturated
aqueous solution
 the solution is gently heated to make
it more concentrated
• After, the solution is allowed to cool at
room conditions
1. Crystallization by Cooling a Hot
Concentrated Solution
• The solubilities of most solids increase
with temperature
• When a hot concentrated solution is
cooled
 the solution cannot hold all of the
dissolved solutes
• The “excess” solute separates out as
crystals
1. Crystallization by Cooling a Hot
Concentrated Solution

Crystallization by cooling a hot concentrated solution


2. Crystallization by Evaporating a Cold
Solution at Room Temperature
• As the solvent in a solution evaporates,
 the remaining solution becomes
more and more concentrated
 eventually the solution becomes
saturated
 further evaporation causes
crystallization to occur
2. Crystallization by Evaporating a Cold
Solution at Room Temperature

• If a solution is allowed to stand at room


temperature,
 evaporation will be slow
• It may take days or even weeks for crystals
to form
2. Crystallization by Evaporating a Cold
Solution at Room Temperature

Crystallization by slow evaporation of a solution (preferably saturated)


at room temperature
Solvent Extraction
• Involves extracting a component from a
mixture with a suitable solvent
• Water is the solvent used to extract salts
from a mixture containing salts and sand
• Non-aqueous solvents (e.g. 1,1,1-
trichloroethane and diethyl ether) can be
used to extract organic products
Solvent Extraction
• Often involves the use of a separating
funnel
• When an aqueous solution containing
the organic product is shaken with
diethyl ether in a separating funnel,
 the organic product dissolves
into the ether layer
Solvent Extraction

The organic product in an aqueous solution can be extracted by solvent


extraction using diethyl ether
Distillation
• A method used to separate a solvent
from a solution containing non-volatile
solutes
• When a solution is boiled,
 only the solvent vaporizes
 the hot vapour formed condenses
to liquid again on a cold surface
• The liquid collected is the distillate
Distillation

The laboratory set-up of distillation


Distillation
• Before the solution is heated,
 several pieces of anti-bumping
granules are added into the flask
 prevent vigorous movement of the
liquid called bumping to occur
during heating
 make boiling smooth
Distillation

• If bumping occurs during distillation,


 some solution (not yet
vaporized) may spurt out into
the collecting vessel
Fractional Distillation
• A method used to separate a mixture of
two or more miscible liquids
Fractional Distillation

The laboratory set-up of fractional


distillation
Fractional Distillation
• A fractionating column is attached vertically
between the flask and the condenser
 a column packed with glass beads
 provide a large surface area for the
repeated condensation and vaporization
of the mixture to occur
Fractional Distillation
• The temperature of the escaping vapour
is measured using a thermometer
• When the temperature reading becomes
steady,
 the vapour with the lowest boiling
point firstly comes out from the top
of the column
Fractional Distillation
• When all of that liquid has distilled off,
 the temperature reading rises and
becomes steady later on
 another liquid with a higher boiling
point distils out
• Fractions with different boiling points can
be collected separately
Sublimation
• Sublimation is the direct change of
 a solid to vapour on heating, or
 a vapour to solid on cooling
 without going through the liquid
state
Sublimation
• A mixture of two compounds is heated in an
evaporating dish
• One compound changes from solid to
vapour directly
 The vapour changes back to solid on
a cold surface
• The other compound is not affected by
heating and remains in the evaporating dish
Sublimation

A mixture of two compounds can be separated by


sublimation
SUMMARY

37
CONCLUSION

• Purification process is widely used in industry.


• Distillation is among the most important and widely
used in industrial operations today. About 95% of all
separation process today is carried out in the industry
with more than 40,000 distillation system.
• Sublimation is also used to create freeze-dried
substances. e.g. tea, soup, drug.

38
CONCLUSION

 Steam distillation is employed in the industry


for the recovery of various essential oils from
plants and flowers.
 Better chemical stability, the crystallization
process is used due it helps to increase
physical stability, bioavailability, and
sustained release.

39

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