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Recrystallization: Activity No. 6

1. The experiment aimed to purify a solid compound through recrystallization by dissolving it in a solvent and recrystallizing to obtain pure crystals. 2. Recrystallization involves choosing a solvent, dissolving the impure solid in heated solvent, cooling to form crystals, filtering and drying the crystals. 3. The purity of the recrystallized crystals was determined using melting point analysis and comparing the melting point range to literature values, with a narrow range indicating high purity.

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103 views

Recrystallization: Activity No. 6

1. The experiment aimed to purify a solid compound through recrystallization by dissolving it in a solvent and recrystallizing to obtain pure crystals. 2. Recrystallization involves choosing a solvent, dissolving the impure solid in heated solvent, cooling to form crystals, filtering and drying the crystals. 3. The purity of the recrystallized crystals was determined using melting point analysis and comparing the melting point range to literature values, with a narrow range indicating high purity.

Uploaded by

Mary Jean Steffen
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Activity No.

Recrystallization

Group 4

Montes, Marie Therese Ann J.


Magan, Quinone
Mocorro, Maria Aiza L.
Obsioma, Jade A.
Perez, Jhonna lyn B.

BS Chemistry 2H1

Organic Chemistry Laboratory 1

Anorico, Nova Fe E.

November 11, 2021


INTRODUCTION

1.1 Rationale of the Experiment

The impurities present in solids are either natural occurring or added during a
synthesis in a laboratory. Impurities are the unwanted chemical substances that make a
solid impure. The process of purifying a solid is called recrystallization. Recrystallization
is the process in which a solid is dissolved in a particular solvent and recrystallized to
derive pure crystal solids. Scientists often use this technique to derive a pure compound
rather than just crystallization.

At room temperature, the compound should be a solid. In choosing a solid, the


best characteristics are to be very soluble at high temperature and very insoluble at cold
temperature. As temperature increases, solubility increases, given that the dissolution of
the solid is successful. In addition to this, as the solids recrystallized, the purer the crystal
solids became. The purpose of this experiment is to derive the purity of solid through
recrystallization.

1.2 Objective of the Experiment


The purpose of this experiment is to derive the purity of solid through recrystallization.
The objectives are as follows:
1. To remove the impurity of a substance by recrystallization
2. To test purity of crystal solids
MATERIALS AND METHODOLOGY

2.1 Experimental Set-up and Materials

The materials that were used when conducting the experiment are chosen solvent, ice
bath, and seed crystal, Erlenmeyer flask, beaker, hot plate, stirring rod, filter paper, and
vacuum-ready Buchner funnel.

Figure 2.1 Experimental set-up of recrystallization (taken from Zubrick n.d.)

2.2 Recrystallization

Recrystallization as in purification of solids works by choosing a particular solvent to


dissolve solid. Solvent in the Erlenmeyer flask were heated up to boiling with the use of hot
plate. A necessary amount of the heated solvent were then added to the impure solid placed in
a beaker for dissolution. More solvents were added to the impure solid and these were heated
then stirred with a stirring rod until all of the solid were dissolved. When the dissolution were
finally complete, the cooling process were started. Hot plate were removed from the beaker
and the beaker were then placed in an ice bath to draw heat away from its contents. As the
crystals of pure solid were form, scratching the side of the beaker with a stirring rod and seed
crystal can be used if a crystal formation were difficult to initiate. Crystals were collected by
filtration, placed filter paper on the vacuum-ready Buchner funnel and dumped the contents
of the beaker on it. By utilizing the vacuum, solvent went through the funnel and the crystals
slowly dried on top of the filter paper. The dry and pure crystals were then collected. The
purity of Crystals were tested by performing melting point analysis and the melting point
range were compared to the tabulated values to pure compounds.

Figure 2.2 Procedural summary of single solvent crystallization (taken from Nichols 2021)
RESULTS AND ANALYSIS

This section discusses the result of the experiment.


Recrystallization is a technique for removing a trace of impurity from a compound.
The purity of the recrystallized substance was determined in this experiment. Purity was
determined using the melting point method. A compound's melting point is the temperature at
which the solid becomes equilibrated with its liquid. When the molecules of a solid
compound gain enough energy to overcome the forces that hold them together in an ordered
crystalline lattice, the solid compound becomes a liquid. These intermolecular forces are
relatively weak in the majority of organic compounds. The melting point range is defined as
the temperature range between when the crystals begin to liquefy and when the entire sample
becomes liquid. The majority of pure organic compounds melt at temperatures between 1-2
°C. The presence of a soluble impurity almost always results in a decrease in the expected
melting point for the pure compound and a widening of the melting point range, i.e. greater
than 5°C or more indicates that the compound is impure.
REFERENCES
JoVE, Cambridge, MA, (2021). JoVE Science Education Database. Organic Chemistry.
Purifying Compounds by Recrystallization. Retrieved on November 11, 2021 from
https://www.jove.com/v/10184/purifying-compounds-by-recrystallization
Libretexts, & Nichols, L. (2021, August 4). November 10, 2021, 7.13: Single Solvent
Crystallization. Chemistry LibreTexts.
https://chem.libretexts.org/Bookshelves/Organic_Chemistry/Organic_Chemistry_Lab
_Techniques_(Nichols)/07%3A_Technique_Summaries/
7.13%3A_Single_Solvent_Crystallization
Recrystallization Introduction. Retrieved on Novemeber 11, 2021 from
http://classes.kvcc.edu/chm220/Recrystallization/prelab/introduction.htm
Zubrick, J. W. (n.d.). November 10, 2021, Recrystallization Part 1 (Laboratory Manual).
What-When-How. http://what-when-how.com/organic-chemistry-laboratory-survival-
manual/recrystallization-part-1-laboratory-manual/

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