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Exp 3-Recrystallization

1) The document describes an experiment on recrystallization to purify acetanilide. Recrystallization uses differences in solubility to separate compounds from impurities as solutions are cooled. 2) Key steps include dissolving the sample in a minimum amount of hot solvent, hot filtering, cooling to induce crystallization, vacuum filtering and washing crystals, then drying the purified product. 3) An appropriate solvent is chosen based on solubility properties - the compound dissolves in hot solvent but crystallizes as it cools. Successful recrystallization recovers the pure compound and removes insoluble and soluble impurities.

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75 views

Exp 3-Recrystallization

1) The document describes an experiment on recrystallization to purify acetanilide. Recrystallization uses differences in solubility to separate compounds from impurities as solutions are cooled. 2) Key steps include dissolving the sample in a minimum amount of hot solvent, hot filtering, cooling to induce crystallization, vacuum filtering and washing crystals, then drying the purified product. 3) An appropriate solvent is chosen based on solubility properties - the compound dissolves in hot solvent but crystallizes as it cools. Successful recrystallization recovers the pure compound and removes insoluble and soluble impurities.

Uploaded by

sisi slay
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PPTX, PDF, TXT or read online on Scribd
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CHEM 331-Lab

Organic Chemistry

Experiment 3

Recrystallization

Department of Chemistry - Faculty of Science


Beirut Arab University
Fall 2020-2021
Aim of the Experiment

Select an appropriate recrystallizing


solvent to separate and purify acetanilide
from a mixture by recrystallization
technique.

Recrystallization | Fall 2020-2021 2


Introduction

 Pure homogeneous compounds consist of the same

molecules and have similar structures. These compounds

may not be totally pure due to possible amounts of

contaminants. The process of Recrystallization can be

used to purify a solid and remove the impurities.

Recrystallization | Fall 2020-2021 3


Separation technique

 Recrystallization is a purification process used to remove impurities from

organic compounds that are solid at room temperature.

 This process is based on the premise that the solubility of a compound in a

solvent increases with temperature, which means that, as solubility increases

temperature increases (you can dissolve more sugar in hot water than in cold

water). And as hot saturated solution cools, it becomes supersaturated and the

solute precipitates (crystallizes) out. So, the solubility of the compound

decreases as the solution cools and crystals form.

Recrystallization | Fall 2020-2021 4


Isolation of Impurities

 The desired product is isolated from its impurities by


differences in solubility.

Two types of impurities: (both removed by recrystallization)


1. 2.

Insoluble impurities and colored impurities: Soluble impurities:


Can be removed from hot solvent through Remain in the cold solvent after
the use of small amount of activated carbon recrystallization which can be
(Charcoal) before filtration. removed by rinsing the crystals with
Small amount is used because it adsorbs also ice cold solvent during Büchner
a certain amount of the desired product if filtration.
large quantity is used

Recrystallization | Fall 2020-2021 5


Recrystallization steps
1. Choose a good recrystallization 1. Cold filtration to separate the solid
solvent. from the solution (mother liquor).
2. Dissolve the sample in the minimum 2. Wash the solid with a small
amount of boiling solvent. amount of cold solvent to remove
3. Hot filtration to remove insoluble the soluble impurities.
impurities. 3. Dry the solid to remove traces of
4. Cool the solution to induce solvent.
crystallization.

Recrystallization | Fall 2020-2021 6


Choice of Solvent
 What solvent and how much will dissolve the desired product?

This operation depends upon solute-solvent To obtain a good recovery of purified material,
interaction involving a number of it is best to avoid using unnecessarily large
parameters including concentration, volumes of solvent. Dissolving the substance
polarity of solute and solvent. in the smallest possible amount of hot

(like dissolves like) solvent minimizes the amount of material

Which means that, the forces that hold the lost by retention in the mother liquors. This

solute molecular forces together are similar helps to prevent separation of the crystals and

to the forces holding the molecules of the clogging of the filter paper during filtration of

solvent together. the hot solution.

Recrystallization | Fall 2020-2021 7


Properties of a good solvent

1. The crude crystals should have low solubility or not at all in the chosen

solvent at room temperature.

2. The crude crystals should have high solubility in the chosen solvent when

heated to boiling.

3. The crude crystals should not react with the solvent.

4. The solvent should boil at temperature below the solid melting point, to

avoid oiling out.

5. The solvent should moderately be volatile so crystals dried readily.

6. The solvent should be non-toxic, non-flammable, and cheap.

Recrystallization | Fall 2020-2021 8


Safety Precautions

As in all laboratory exercises:


• Safety glasses, mask, and gloves must be worn at all
times.
• Avoid skin and eye contact with any chemical reagent.
• In case of skin contact, rinse the area with water for
several minutes.
• For eye contact, flush eyes with water and seek
immediate medical advice.

Recrystallization | Fall 2020-2021 9


Procedure (Attach reflux apparatus)
First of all add a glass funnel and 100 mL funnel in oven to have the pre-heated system.

2) Filtration

1) Bring to while hot


boiling - All
product will
be dissolved

Recrystallization | Fall 2020-2021 10


Procedure (Pre-heated system)

Pre-heated system, should be


removed directly from oven
once the acetanilide is totally
dissolved in the hot solvent.

Erlenmeyer flask is used and not a beaker


because:
Fluted filter paper is used in order: 1. E.F has a narrow neck that allows some
1. To increase the surface area of the refluxing of the solvent and thus slow rate
filter paper of solvent evaporation.
2. Creation of gaps between filter paper 2. Narrow neck allows to swirl the liquid.
and funnel, these gaps provide Thereby aiding in dissolving the solid.
channels for the solvent to flow 3. A flask can be stoppered to prevent
through the filter paper, thus evaporation during cooling down.
increasing the speed of the solvent
through the paper. 4. But, its slightly more difficult the crystals
from an E.F than from a beaker.

Recrystallization | Fall 2020-2021 11


Procedure (Collection of crystals)

3) Cooling at
4) Chilling in ice
room temperature

In order to maximize
White crystals the amount of
began to appear. crystals formed.

5) Collection of crystals
by vacuum filtration 7) Dry your pure
product,
weigh it, and calculate
6) Wash the crystals the percent purity.
with 2 mL cold water.

Recrystallization | Fall 2020-2021 12


Calculation
% Recovery
   of   pure  acetanilide

•   x 100

Recrystallization | Fall 2020-2021 13


Recrystallization | Fall 2020-2021 14

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