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Ebt 105 Organic Chemistry Laboratory: Experiment 1: Crystallization

This document describes an experiment on the crystallization of benzoic acid. The objectives are to study the crystallization process and purify an organic compound through recrystallization. Benzoic acid crystals are dissolved in hot water and allowed to crystallize by cooling in an ice bath. The crystals are filtered and dried, yielding a 82.78% recovery of purified benzoic acid. Recrystallization removes impurities from the compound by favoring crystallization of the pure compound. Water is a slightly inappropriate solvent due to the low solubility of benzoic acid, but it dissolves the compound when heated due to increased energy overcoming hydrogen bonding.

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0% found this document useful (0 votes)
157 views7 pages

Ebt 105 Organic Chemistry Laboratory: Experiment 1: Crystallization

This document describes an experiment on the crystallization of benzoic acid. The objectives are to study the crystallization process and purify an organic compound through recrystallization. Benzoic acid crystals are dissolved in hot water and allowed to crystallize by cooling in an ice bath. The crystals are filtered and dried, yielding a 82.78% recovery of purified benzoic acid. Recrystallization removes impurities from the compound by favoring crystallization of the pure compound. Water is a slightly inappropriate solvent due to the low solubility of benzoic acid, but it dissolves the compound when heated due to increased energy overcoming hydrogen bonding.

Uploaded by

Harmol Singh
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© © All Rights Reserved
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EBT 105 ORGANIC CHEMISTRY LABORATORY

EXPERIMENT 1: CRYSTALLIZATION

NAME MATRIC NO.


1. NUR SYAZWANI BINTI MANAF 191172390
2. HAZWANI BINTI ZAIDOL 191172378
3. AMEIRUL QAYYUM EIMAN BIN RAMLI 191171290
4. MAHESWARAN A/L GUNALAN 191172380

LECTURER: DR. MOHD FAIRUL SHARIN ABD RAZAK

DATE OF SUBMISSION: 16 OCTOBER 2019


1.1 INTRODUCTION

Crystallization is a process of formation of solid crystals precipitating from a


solution, melt, or more rarely deposited directly from a gas. Crystallization can also
refer to the solid-liquid separation and purification technique in which mass transfer
occurs from the liquid solution to a pure solid crystalline phase, occurs in 2 stages
which are nucleation and crystal grow.

Crystallization is based on principles of solubility: compunds (solutes) tend to


be more soluble in hot liquid (solvent) then they are in cold liquids. If a saturated hot
solution is allowed to cool, the solid is no longer soluble in the solvent and forms
crystal of pure compound. Impurities are excluded from the growing crystals and the
pure solid crystals can be separated from the dissolved impurities by filtration.
Usually crystallization spontaneously occurs upon cooling the solution. If it does not,
crystallization maybe induced by cooling the solution in an ice bath, scratching the
vessel wall with a glass stirring rod or by adding a single crystal of pure material (a
seed crystal). The collected crystals are then washed with ice cold solvent to further
remove impurities.

1.2 OBJECTIVES
To study the crystallization process of an organic compound.

1
2.0 LAB EXPERIMENTAL

2.1 CHEMICAL AND APPARATUS

- Benzoic Acid
- 50 ml Erlenmeyer Flask
- Distilled Water
- Ice Bath
- Glass Funnel
- Watch Glass
- Hot Plate
- Glass Rod
- Graduated Cylinder
- Filter Paper
- Thermometer

2.2 PROCEDURE
1. 1.8 gram of benzoic acid placed in 50 ml of Erlenmeyer flask.
2. 10 ml of water added to the solid in the flask, heating began.
3. Water drop added continuosly from graduated cylinder as water begins to boil until
the solid completely dissolves.
4. The total volume of water required to dissolve the benzoic acid crystals recorded.
5. The solution allowed to be cooled undisturbed at room temperature. During thos
slow cooling, crystals of the solid formed.
6. The flask was placed when it has reached room temperature in an ice bath for
atleast 10 minutes. Crystals observed.
7. Crystal was collected by filtration, followed by transferring the crystal from the
funnel to watch glass. Another piece of filter paper was placed on top of the crystal
and press firmly to remove some of water and allowed to dry.
8. After the crystal was completely dried, the weight of benzoic acid recovered by
recrystallization obtained.

2
Figure 1: Benzoic acid weighted Figure 2: 10 ml of water added Figure 3: Heating mixture

Figure 4: Measure temperature (100C) Figure 5: Add water drop Figure 6: Swirl mixture

3
Figure 7: Cooling (Room temp.) Figure 8: Ice bath Figure 9: Filtration

Figure 10: Drying crystals Figure 11: Crystal formed Figure 12: Crystal weighted

4
3.0 RESULT AND DISCUSSION

3.1 RESULT

W1 of benzoic acid 1.8 g


Volume of water added 6 ml
Wt of benzoic acid recovered 2.54 g - 1.05 g = 1.49 g

3.2 DISCUSSION
1. Calculate the percentage recovery of solid.
Percent recovery= amount of substance actually collected
100 %
amount of original substance
= 1.49g
100 %
1.80g
= 82.78%

2. Impure benzoic acid was dissolved in hot water. The container of solution was
placed in an ice bath instead of being allowed cooling slowly at room
temperature. What will be the result of cooling the solution in this manner?
-The result of cooling in this manner is that impurities will be removed from the
impure benzoic acid resulting in a more purified benzoic acid. The method
described above is known as recrystallization and it is often used to remove
impurities from substance by choosing conditions that will favour the
recrystallization of the substance only, thus leaving the impurities behind.

3. Was the solvent appropriate for crystallization of the compound? Use your
understanding of polarity and solubility to explain.
-The compound is considered slightly polar, benzoic acid is only slightly soluble in
water when heated because as the temperature increase, more energy is present to
overcome the hydrogen bonding between water molecules to form weaker Van der
Waals forces of attraction between benzoic acid and water. So it is slightly
unappropriate.

5
4.0 CONCLUSION
The crystallization process of an organic compound can be studied, which is
the percentage recovery of solid is 82.78%.

5.0 REFERENCES

Dr Mohamad Kahar Bin AB Wahab, Dr Jalilah Jalil, Dr Mohd Fairul Sharin


Abd Razak (2019). Experiment 1 Crystallization. EBT105 Organic
Chemistry.

Pn Zurain Bt Zawawi (2018). Drying Of Process Materials. Unit Operation


Politeknik Kuching, Sarawak.

Calculation of percent recovery during recrystallization,


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