SCCH 159/169/189 : Recrystallization of Aspirin 1

Experimental Report

Recrystallization of Aspirin

Scuijah Aiadrveng 6405660 SCBE

1. Name……………………Surname…………..………..ID……………….Program…………….….
2. Name……………………Surname…………..………..ID……………….Program…………….….
3. Name……………………Surname…………..………..ID……………….Program…………….….
4. Name……………………Surname…………..………..ID……………….Program…………….….

Experiment
Purification of Acetylsalicylic Acid (ASA) by Recrystallization

1. Prepare 5% (v/v) ethanol/water mixture by combining water (95 ml) and ethanol (5 ml) in
a 250 mL beaker. (The volume of hot solvent required in a recrystallization depends on
the amount of crude sample and its solubility in the solvent) In this recrystallization,
approximately 20 mL of the solvent per gram of crude ASA will be needed.
2. Weigh about 2 g of crude ASA and record the exact mass in the report.

2.044
Mass of crude ASA …………………………g
40
Expected volume of solvent…………………mL

3. Heat the required amount of water/ethanol mixture on a hot plate until small bubbles are
forming. Then, add your estimated solvent mixture volume to the ASA sample. Swirl the
flask to mix the contents and warm it on the steam bath/hot plate. (Caution! The flask is
hot) Keep the solvent hot on the steam bath throughout this process. If any solid remains,
add hot solvent in 5-10 mL portions, with warming between each addition, until all the
solid has dissolved. If any solid still remains, filter solution while hot through fluted filter
paper into a heated flask.
4. Once all the solid has dissolved, place the flask on a heat-proof mat on your bench to cool.
Crystal should soon begin to deposit in your flask. When the solution has cooled to about
40 C (i.e. warm, not hot, if held in your hand) place the flask in an ice-bath (use a 500
mL beaker) and allow it to cool for 5-10 minutes to complete crystallization.
5. Set up a vacuum filtration apparatus using a Büchner funnel (see Fig. 8.1), making sure
the filter flask is clean. Dampen the filter paper circle with a little water, apply the vacuum
and check that a good seal is obtained.
6. Collect the crystals by swirling the flask to suspend them and then pouring the suspension
into the filter funnel, trying to leave as few crystals in the conical flask as possible. Any
remaining crystals can be transferred by using fresh cold solvent.
7. Dry the crystals by drawing air through the product for 5 mins. Then, transfer the crystal
to wash glass and dry over the steam bath. Do not directly put the wash glass on the hot
plate! Determine the mass of recrystallized ASA.
SCCH 159/169/189 : Recrystallization of Aspirin 2

Figure 8.1. Büchner funnel set up. (http://what-when-how.com/wp-

content/uploads/2011/06/tmp30127_thumb1.png)

1. 541
Mass of recrystallized ASA …………………….g

Calculate your percentage yield of recrystallizes ASA

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Percentage of recovery mass of crystallized G) ✗ too
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=

Cg mass of crude ,
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1.541
✗
=
100

ts.it percentage of
2. 044

recovery
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=

Conclusion
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from this eperiment purpose for how to calculate
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percen yeild and explain how to Recrystallization has many

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Varibles to
purify substances as as weighing, coding , mixing,heating .fi/Hation
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to
,

washing and
dry
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'

..

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SCCH 159/169/189 : Recrystallization of Aspirin 3

Review Questions
1. If your percentage yield of recrystallizes ASA is greater than 100 %, explain at least one
reason:
large
Create a or amount
precursor
substrate
contaminants
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2. If your percentage yield of recrystallizes ASA is less than 100 %, explain at least two
reasons:
1. Point out that the product has infected little
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All of the product not contaminated

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2 .
.

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3. Why fresh cold solvent is used to transfer crystals, but not fresh solvent at room
temperature?
fresh cold solvent have
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low temperature than not fresh solvent
a .

However the solvent will have time to crystallite Because crystals cannot
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,
. -

be transferred immediately The crystals structure will

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.
change .

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4. What are the important factors in this experiment to obtain pure aspirin?

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Weighing , cooling mixing , heating , filtration washing and dry
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, ,
.

All of these the most important ( pore aspirins

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so .

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5. If you have a chance to design this experiment based on the same principles, briefly suggest
your idea how to improve this experiment.
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Conduct experiments explain the step to step and the most important
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should conduct experiments carefully and carefulness for good results
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