NaCl Purification

By
Riski Ayu Candra
Umar Faruq Muttaqiin
Levina Ayu Arastika
Introduction
Recrystallization is a method used to purify solids. The crystallization
method can be used to separate the solids from other solids. Recrystallization
method is based on the differences of solubility between the purified substance
and impurities in a particularly solvent.

Purification by recrystallization of solids based on the difference in

solubility of the substance to be purified in certain solvents. The general
procedure is often used in the recrystallization is:

Dissolving the impurities substances in certain solvent at near the melting

point
Filtering the particles of insoluble materials in hot solution condition
Cooling the hot solution of the solute into the crystal
Separating the crystal from the solution of supernatant
 Another thing to note in the recrystallization process is the selection
of an appropriate solvent. Some of the requirements of a solvent can be used in
the recrystallization process include:

Providing sufficient difference in solubility between the purified substance

and impurities
Not leaving the impurites in the crystal
It is easily to be separated from the crystal
It is inert (does not react easily with the crystal)
Equipment and Materials
Equipment: Materials:

Digital balance 1. Dirty salt

Bunsen burner 2. CaO powder
Burette and Clamps 3. Ba(OH)2 1 M solution
Erlenmayer 4. (NH4)2CO3 0.1 M solution
Dropping pippete 5. HCl concentrated
Watch glasses 6. Aquabides
Beaker glass 7. KIO3 solution
Tripod and case 8. HNO3 0.1 M solution
Evaporation chamber 9. AgNO3 0.1 N solution
Spatula 10. Universal pH indicator
paper
Observation Data Sheet
Color of the salt before purified: turbid white and dirty
Structure of salt crystals before purified: large/ coarse crystalline
Color of the salt after purified: white clear crystall
Structure of salt crystals after purified: soft powder
Volume of Ba(OH)2 required is: 4.8 mL (96 drops)
Volume of (NH4)2CO3 required is: 4 mL (80 drops)
The weight of salt crystal from salt recrystallization: 1.3659 g
The percentage of pure salt from recrystallization process:

weight of pure salt 1.3659 grams

100% = x 100% = 54.49 %
weight of dirty salt 2.5067 grams

N AgNO3 is 0.0867 N
The Purity level of NaCl before recrystallization process is 82.14%
The purity level of NaCl after recrystallization process is: 94.198 %
Reaction that occured in NaCl
purification
Reaction NaCl with CaO to precipitate
another impurities and to give the white colored of
NaCl purified
CaO Ca2++ O2-
Ca2+ + CO32- CaCO3(s)
Ca2+ + SO42- CaSO4(s)
Mg2+ + O2- MgO (s)
2 Fe3+ + 3 O2- Fe2O3 (s)
 Reaction the addition of Ba(OH)2 to eliminate
or prevent the formation of precipitate again due
to the addition of CaO
Ba(OH)2 Ba2+ + 2OH-
Fe2+ + 2OH- Fe(OH)2(s)
Mg2+ + 2OH- Mg(OH)2(s)
Al3+ + 3OH- Al(OH)3 (s)
Ba2+ + SO42- BaSO4 (s)
 Reaction the addition of (NH4)2CO3 to form the
saturated solution and to bind the remaining impurities
(NH4)2CO3 2NH4++ CO32-
Ba2+ + CO32- BaCO3(s)
Ca2+ + CO32- CaCO3(s)

Reaction the addition HCl to balance pH value of

purified NaCl after addition of Ba(OH)2/ neutralization
NH4+ + HCl NH4Cl (neutralization)
Discussion: NaCl Purification
In this experiment aims to study the crystallization
method with the addition of a binder impurities, can
understand the method of iodized sodium chloride, and can
calculate the degree of purity NaCl. Recrystallization is used
to purify solids. Usually this method works best when there
is only a small amount of impurity in the solid.
The first step was dissolving 2.5grams of dirty salt in
hot water, it made the dirty salt decomposed to their ions,
namely Na+ and Cl-. The hot distilled used to make the dirty
salt dissolved completely. After the filtration, the filtrate
then added with CaO. The function of CaO was intended to
bind impurities such as Ca2+, Mg2+, Fe3+, CO32-, and SO42-
that contained the salt.
 After the addition of CaO, white precipitate
was formed which is then filtered again. The
solution then added with Ba(OH)2 which has the
function to bind impurities in the form of Mg2+,
Al3+, Fe3+, and SO42-, and prevent the formation of
deposits that may occur due to the addition of CaO
in the previous process.
After that the precipitate was filtered and set
aside. At the filtrate was then added a solution of
(NH4)2CO3 which had the function to bind another
impurities remaining in the form of SO42-, and the
excess of Ca2+, and Ba2+ from the previous process.
 After waiting for 5 minutes, then filtered. The
filtrate was likely to be alkaline due to the effect of the
addition of CaO, Ba(OH)2, (NH4)2CO3 so filtrate needed
to be neutralized by the addition of HCl solution, until
the solution became neutral that indicated on universal
pH indicator paper.
Filtrate then evaporated until all the solvent
evaporates and obtained crystals purified NaCl. After
the NaCl crystal was obtained then weighing with the
mass of purified crystal was 1.3659 grams with percent
pure salt amounted to 54.49%. The obtained color salt
was cleaner and more white rather than dirty salt
before.
Discussion: The Purity Level of
NaCl
To determine the purity level of NaCl, we must did the
titration using AgNO3 solution as titrant and K2CrO4 solution as
indicator. The solution used for AgNO3 standardization was NaCl
pa and after that the obtained normality value of AgNO3 was
0.0867 N.
Then did the titration 2 times (duplo) for each salt before
and after the crystallization process. The dirty salt was required
4.05ml of AgNO3 solution and obtained the purity level was
82.14%. As for the purified salt was required 4.65ml of AgNO3
solution and obtained the purity level was 94.198%.