Introduction

Crystallization is a chemical solid-liquid separation process in which mass transfer of a solute

from the liquid solution to a pure solid crystalline phase [1]. During the crystallization
process, the atom is arranged in a defined and periodic manner to form a structure. This step
is called nucleation. It is the stage where the solute molecules start to merge into small groups
and become stable. The growth of the nucleus is the next step in the evolution of the solid-
liquid system following by supersaturation [2]. Typically, the solution is cooled until the
solute concentration exceeds its solubility at the temperature. The solute then precipitates out
of the solution, generating crystals of approximately pure solute [3].
A solution must be supersaturated for crystallization to occur. Supersaturation was created by
a decrease in temperature. Depending on how the solution was cooled, a different product
was obtained. The relationship between the mole fraction solubility of a solute and the
temperature in a real solution can be determined by using Van’t Hoff equation (Eq.1) where
R is the gas constant and ∆Hd and ∆Sd are the dissolution enthalpy and entropy.

−∆ H d ∆ Sd
ln x 1= + (Eq.1)
RT R

Therefore, the present work aims to determine the dissolution enthalpy and entropy of Epsom
salt (MgSO4) in ethanol, acetone and water through the Van’t Hoff equation. This work also
to study the crystal shape of Epsom salt (MgSO4), sugar and copper sulphate in water and the
recrystallization of MgSO4 by using crash and natural cooling crystallization. The
experiment was done at 30°C, 40°C, and 50°C for the dissolution enthalpy and entropy of
Epsom salt. On the other hand, the experiment for the different types of crystal and crash
cooling vs natural cooling crystallization was done at 55°C
2. Methodology
2.1 Equipment/Apparatus/Material
Crucible, Measuring Cylinder, Measuring Beaker, Glass Rod, Hot Plate, Freezer,
Furnace, Epsom Salt, Sugar, Copper Sulphate, Ethanol, Acetone, and Water.

2.2 Experimental
2.2.1 Dissolution enthalpy and entropy of Epsom salt

Empty crucibles were weighed and labelled as a solvent for 3 different temperatures
of 30°C, 40°C and 50°C. Then, 30 mL of acetone, ethanol and water solvents were
prepared and labelled in beakers respectively. 10mL of acetone was measured using a
measuring cylinder and poured into a beaker on a hot plate. Epsom salt was added
slowly and stirred well until in excess at the temperatures of 30°C, 40°C and 50°C.
Acetone with saturated Epsom salt in the beaker was filtered to remove the excess salt
and the remaining solution was collected in the crucible. The weight of the crucible
before drying was weighed and recorded. Then, the step was repeated for the ethanol
and water solvent. Nine crucibles were placed in the furnace for 24 hours. The dry
solvent under different conditions was weighed and recorded

2.2.2 Different types of crystal

Three empty crucibles were weighed and labelled for sugar, copper sulphate and
Epsom salt solvents. Sugar was poured into 10mL of distilled water at 50°C until it
became a saturated solution. The solution was stirred well until all the solute was well
dissolved and in excess. Next, the saturated solution was filtered to remove the
excess. It was repeated with cooper sulphate and Epsom salt. Then, three beakers with
the filtered saturated solution were poured into a crucible each and the weight of the
crucibles before drying were weighed and recorded. Three crucibles were placed in
the furnace for drying purposes for 24 hours. The weight of the dry solvent was
weighed and recorded. After salt crystal formation, the shapes of crystal formed was
observed
2.2.3 Crash cooling vs natural cooling crystallization

50mL of distilled water was filled in the two sets of beakers. The Epsom salt was
added into each beaker until it became a saturated solution. Both solutions were
stirred thoroughly to ensure it was homogenously mixed. The first beaker was
labelled as natural cooling was put under room temperature for natural cooling. The
second beaker was labelled as crash cooling was kept in a freezer for the crash
cooling process. In 2 minutes time interval, the temperature of each solution in the
beaker were recorded. The formation of crystal in each beaker were also obeserved.

References

[1] Mullin J. W., Crystallisation, Butterworth Heinemann

[2] 12.1: Crystalline and Amorphous Solids - Chemistry LibreTexts. (n.d.). Retrieved November 3, 2021, from
https://chem.libretexts.org/Bookshelves/General_Chemistry/Book%3A_General_Chemistry
%3A_Principles_Patterns_and_Applications_(Averill)/12%3A_Solids/12.01%3A_Crystalline_and_Amor
phous_Solids
[3] Crystallization. (n.d.). Retrieved November 3, 2021, from/http://www.reciprocalnet.org/edumodules/crystall