UNIVERSITY OF DUHOK

COLLEGE OG SCIENCE
CHEMISTRY DEPARTMENT

A LABORATORY REPORT ABOUT:

RECRYSTALLIZATION

Experimenters: Reber Ch. Hussein, Muhammed M. Hussein,

Hashim Y. Jarjees
Academic year: 2023/2024 (1st semester)
Instructors: Mrs. Jihan, Mrs. Banaz, Mr. Sood
Starting Date: November 22, 2023
Submission Date: November 29, 2023
 Aim of the Experiment:

Purification of a solid organic compound,

Glassware/Equipment:

1. Heater
2. Cylinder
3. Funnel
4. Conical flask
5. Stirring rod
6. Filter paper
7. Buchner funnel
8. Beaker
9. Burner.
10. Wire gauze.
11. Tripod stand.
12. Rubber tubing

Chemicals:

1. Water (as solvent)

2. Benzoic Acid (as solute)

Theory:

The most widely used method for the purification of a solid organic compound is
recrystallization (the selective crystallization of one compound from a mixture of
solid compounds).
The recrystallization method operates on the principle that the undesired compounds in the
mixture will have solubility properties that differ from those of the desired compound in a
selected solvent some of the undesired contaminates may be insoluble in the solvent after the
desired compound has dissolved, others may remain dissolved in the solvent after the desired
compound has crystallized.
The operations that must be performed during recrystallization include:
1- Choose of a suitable solvent- - -To recrystallize known organic compound, the chemical
literature may report or recommend the use of certain solvent. However, if the compound is
unknown, no theoretical considerations are used in choosing the solvent except the very
rough
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generalization that (like dissolves like). Therefore, the solvent must be determined
experimentally, putting in consideration that it must be characterized by:
a-It must be chemically inert toward the solute.
b-The solute should dissolve readily in the boiling
solvent. c-The solute should be sparingly soluble in cold
solvent.
d-The solvent should dissolve the impurities either very easily or not at all.
e-The solvent should be highly volatile so that it can readily be evaporated from the
crystals. f-The solvent should be inflammable, inexpensive and nontoxic.
2- Dissolution of the sample in a minimum volume of the selected solvent by heating----The
energy supplied for the dissolution process In consumed to
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overcome the intermolecular attractive forces that hold the molecules together (the
lattice energy) and break it.
3- Decolorizing the solution------The presence of colored impurities in a sample or a solution
of a colorless compound can be removed by adding activated charcoal to the hot solution prior
to filtration.
4- Hot filtration- - - -Hot filtration by gravity is performed to get-rid of insoluble impurities.
5- Cooling the filtrate The rate of cooling determines the size and the shape of the
crystals. Fast cooling tends to form and smaller crystals, slow cooling tends to form fewer and
larger crystals. The very small crystals are undesirable because it is difficult to wash them free
of the solvent and the soluble impurities, and it takes longer time to dry them.
6- Cold filtration by suction When crystallization is complete, the product is collected by
vacuum filtration on a Buchner funnel.
7- Washing the crystals------After the liquid has been drawn off by suction filtration, some
fresh cold solvent should be poured over the crystals in order to wash off the liquid containing
the soluble impurities. If this is not done, the soluble impurities will be deposited on the
crystals when the solvent evaporated.
8- Drying the crystals After the crystals have been collected by suction filtration and
washed, they can be dried by continuing to draw air over them in the funnel until the solvent
has almost stopped dripping, then spread them out on a piece of filter paper.

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Figure:

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 Results:

Data:

Wtimpure Benzoic acid=1g

Wtpure Benzoic acid=

Caculations:
𝑤𝑡 𝑜𝑓 𝑝𝑢𝑟𝑒 𝑏𝑒𝑛𝑧𝑜𝑖𝑐 𝑎𝑐𝑖𝑑
× 100
𝑤𝑡 𝑜𝑓 𝑖𝑚𝑝𝑢𝑟𝑒 𝑏𝑒𝑛𝑧𝑜𝑖𝑐 𝑎𝑐𝑖𝑑
Percentage of pure Benzoic Acid (Wt/Wt)=

= × 100 =
1

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 Discussion:

The process of recrystallization is a fundamental technique used for purifying

solid compounds, as demonstrated in the experiment focusing on the purification
of benzoic acid. The procedure involved several key steps aimed at isolating a
high-purity product. Initially, the crushed sample was dissolved in a selected
solvent, water in this case, forming a saturated solution to dissolve the solute.
The addition of activated charcoal helped remove impurities by adsorption,
followed by filtration to eliminate any remaining contaminants. The crucial
cooling process allowed the formation of pure crystals, which were subsequently
collected using vacuum filtration. This meticulous method resulted in obtaining
purified benzoic acid crystals, characterized by their melting point and yield.
The experiment showcased the significance of recrystallization in isolating
compounds with enhanced purity, enabling the determination of their physical
properties for identification and further analysis. The yield calculation served as
a quantitative measure to assess the success of the purification process,
emphasizing the importance of precise techniques in organic compound
purification.

Asked in the lab

What’s the difference between gravity filtration and Vacuum filtration?

Gravity filtration and vacuum filtration are two distinct techniques used in the laboratory to
separate solids from liquids, primarily during the purification or isolation of substances. The
key differences lie in the method of filtration and the driving force used to facilitate the
separation.

Gravity Filtration:
Process: Gravity filtration relies solely on gravity to pass the liquid mixture through a filter
medium, such as filter paper or other porous material. The mixture is poured into a filter
funnel with filter paper, allowing the liquid to flow through the filter by the force of
gravity. Solid particles are retained on the filter paper while the liquid (filtrate) passes
through and collects in the receiving flask.
Application: Gravity filtration is suitable for filtering smaller volumes of solutions and is
commonly used when a mild separation method is adequate, especially for solutions
containing larger particles that won't clog the filter paper.

Vacuum Filtration:
Process: Vacuum filtration involves the use of a vacuum pump or aspirator to create a
pressure difference, which accelerates the filtration process. A Buchner funnel, often fitted
with a filter paper, is connected to a vacuum source. The reduced pressure generated by
the
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vacuum draws the liquid through the filter paper, speeding up the filtration process
significantly compared to gravity filtration.
Application: Vacuum filtration is preferred when filtering larger volumes of solutions or when
a faster filtration rate is necessary. It is especially useful for fine precipitates or when a higher
level of separation efficiency is required.

Key Differences:
Driving Force: Gravity filtration relies on gravity alone, while vacuum filtration employs a
pressure difference created by a vacuum source.
Filtration Rate: Vacuum filtration is generally faster than gravity filtration due to the applied
pressure difference.
Suitability: Gravity filtration is suitable for smaller volumes and when gentle filtration is
sufficient. Vacuum filtration is more efficient for larger volumes or when a faster and more
thorough separation is needed.