NaCl PURIFICATION

A. Objectives
1. Study the recrystallization method with the addition of impurity binder material.
2. Understand the methods of NaCl iodisation.
3. Calculate the purity levels of NaCl.
B. Theory
Salt is essential and common elements, in processed foods. The use of salt in
processed foods require special standards, so the standard known salt consumption. Salts of
the people known as the krosok salt. These folk salt, still contains impurities such as heavy
metals, and the content of NaCl and iodine is below standard. To separate the impurities in the
salt, often washing by society naturally in salt ponds. The quality of the national salt, less
qualified as NaCl salt consumption because the content is still considerably less than required.
In addition, the low quality of the cleanliness of the salt for consumption. (Nur, M. 2013)
To reduce impuristis in salt can be done with a combination of the washing process and
rapid dissolution during salt production. While the removal of impurities from salt product can be
made by a chemical process, which is reacting with Na2CO3 and NaOH to form a precipitate
CaCO3 and Mg(OH)2. The addition of Na2CO3 and NaOH is part of a very important process in
the refining process salt solution. To avoid a breakdown of sediment caused by nature fragile
metal hydroxide, then Na2CO3 was added in advance of NaOH. Best results will be obtained if
Na2CO3 and NaOH is added simultaneously so that it will produce the same reaction. The
deposition along CaCO3 and Mg(OH)2 will take place faster than the hydroxide precipitate that
settles itself. Good results are also obtained if Na2CO3 is added first before the addition of
NaOH (Bahruddin, et al., 2003).
The precipitate is a substance that separates itself as a solid phase out of solution. The
precipitate formed when the solution becomes too saturated with substance concerned.
Solubility (S) a precipitate is by definition equal to the molar concentration of the saturated
solution. Solubility depends on various conditions such as temperature, pressure, concentration
of other ingredients in the solution, and the composition of the solvent. (Lesdantina, 2009).
Crystals can be classified based on the nature of the bonding between atoms, ions or
molecules that constitute it. This classification would be more fundamental to use the number
and type of elements properly. When the results of the rotation, reflection, or the inverse of an
object can be properly suspended in his native objects, the structure was said to contain certain
elements such as the symmetry axis of rotation, the field of reflection (mirror), or the center
point. This symmetry operations can be applied to geometric forms, on a physical object or
structure of the molecule. Recrystallization stage is:
1. Solvents: dissolve impurities in the crystal.
2. Filtering: separating impurities from a solution of pure crystal.
3. Heating: vaporize and removal of solvent from the crystals.
4. Cooling: crystallizing back purer crystals. (Underwood,1990).

C. Equipment and Materials

Equipment :
1. Digital balance
2. Gas stove
3. Oven
4. Burette 25 mL
Materials :
1. Dirty salt;
2. CaO powder;
3. Ba(OH)2 1 M solution;
4. (NH4)2CO3 0.1 M solution;
5. Concentrated HCl;
6. Aquabides;

5. Erlenmeyer 25 mL 3 pieces
6. Dropping pipette 2 pieces
7. Watch glasses
8. Beaker glasses

7. 1000 ppm of KIO3 solution;

8. HNO3 0.1 M solution;
9. AgNO3 0.1 N solution;
10. Universal pH indicator paper.
11. Distilled water.

D. Procedures
1. Purification of NaCl
2,5 grams of dirty salt

Put in a beaker containing 25 mL of

aquades was heated until dissolved
filtered

filtrate
jjkkkkk

residue

add 0,05 gr of CaO and filter the

precipitate happened
add Ba(OH)2 1 M until the last drop
doesnt form precipitate
filtered the precipitate

filtrate

residue

add 5 mL (NH4)2CO3 0,01 M until the last

drop doesnt form a precipitate.
allowed for 5 minutes until formed
precipitate clearly.
filtered the solution.

filtrate

residue

test pH with universal indicator paper.

neutralized with dilute HCl.
evaporated up to dry.

NaCl crystal

weigh the crystals obtained

2. Determination of purity levels of NaCl

a) Standardization AgNO3
0,25 gr NaCl pa (pro analys) dissolved in 100 mL of
distilled water, move into the erlenmeyer

10 mL of solution taken

1 mL indicator K2CrO4 5% added

Titrate with 0,1 N AgNO3 solution until the solution color

is red brick

Repeat the titration 3 times

b) Determining the content of dirty salt

250mg dirty salt dissolved in 100 mL distilled water, moved in erlenmeyer.
Check pH, added NaHCO3 if too acid and added HNO3 if too alkaline until
neutral.
Added 1 mL indicator K2CrO4 5%. Titrated it with 0.1 N AgNO3 solution until red
black coloured and produced white precipitate.
We repeated the titration 3 times.

c) Determining the purity levels of NaCl after recrystallization

0,25 grams of NaCl after
recrystallization
-Dissolved in 100 mL of distilled water
then move into the erlenmeyer
.
10 mL of solution

1 mL indicator K2CrO4 5%
added

Titrate with 0,1 N AgNO3 solution

until the solution color is red brick

Repeat the titration

3 times
E. Observation Data
a.
b.
c.
d.
e.
f.
g.
h.
i.

Color of the salt before purified : turbid white and dirty

Structure of salt crystals before purified : rough crystals, big particle, clot salt
Color of the salt after purified
: clean white
Structure of salt crystals after purified
: soft powder salt
Volume of Ba(OH)2 required is
: 33 drops
Volume of (NH4)2CO3 required is
: 5 mL
The weigh of impurities from salt recrystallizing
: 1,1767 grams
The weight of salt crystal from salt recrystallizing
: 1,3234 grams
The percentage of pure salt from recrystallizing process :
The percentage of pure salt

weigh of pure NaCl

weigh of initial NaCl(dirty salt )

1,3234

= 2,5001 x 100

52,93
j.

Titration data :
1. Standardization AgNO3
Mass of concentated NaCl : 0,2502 grams
Volume of distilled water : 100 mL
Volume AgNO3 that needed :
V1 = 4.3 ml
V2 = 4.38 ml V3 = 4.29 ml
Average volume of AgNO3 = 4.295 ml
N NaCl

gram 1000
x
Mr
V

0.2502 1000
x
58.46 100

= 0.0434 N
V NaCl . N NaCl

= VAgNO3 . N AgNO3

x 100%

V NaCl

10 ml .

gra m 1000
x
Mr
V

0.2502 1000
x
58.46
100

= VAgNO3 . N AgNO3

. 99,99%

N AgNO3

= 4.295 ml . N AgNO3

= 0.09963 N

2. Determining the content of dirty salt

Mass of dirty salt: 0,2510 grams
Volume AgNO3 that needed :
V1 = 3.89 ml V2 = 3.91 ml V3 = 3.81 ml
Average volume of AgNO3 = 3.9 ml
The purity levels of NaCl before recrystallization process

( V . N ) AgNO3 . 58.46
100
w . 1000

3.9 0.09963 58.46

100
0,2510 .1000

9.0498 ( 10 ml )
in 100 ml

9.0498 X 10=90,498

3. Determining the purity levels of NaCl after recrystallization

Mass of NaCl after recrystallization : 0,2502 grams
Volume AgNO3 that needed :
V1 = 4.11 ml V2 = 4.10 ml V3 = 4.10 ml
Average volume of AgNO3 = 4.1033 ml
The purity levels of NaCl after recrystallization process :

( V . N ) AgNO 3 .58,46
100
w .1000

4.1033 0.09963 58,46

100
0.2502 1000

9. 552 ( 10 ml )
in 100 ml

F. Discussion

9. 552 10=95.52

NaCl salt purification experiment aims to Study the recrystallization method with the
addition of impurity binder material, Understand the methods of NaCl iodisation, and finally able
to Calculate the purity levels of NaCl. In this experiment, there are four main steps, which is
purification NaCl, AgNO3 standardization, the determination of the initial NaCl concentration,
and determination of the final NaCl.
a) NaCl Purification
Sodium chloride is the main component, which is expected to exist in the salt. Therefore the
purification process is carried out to increase the levels of NaCl on salt. Recrystallization is
one way of purifying solids are often used, in which these substances are dissolved in a
solvent and then crystallized back in. This method relies on the solubility in certain solvents.
At the time of NaCl diluted with hot distilled water, the addition of some substances to
precipitate impurities ions.
Dirty salt is converted from solid state into solution. Salt dissolved in hot distilled water, it
aims to accelerate the dissolution process itself. At the time of the dissolution process
occurs ionization component - component of the salt. In this dirty salt contains not only Na +
and Cl- ions, but also contains ionic impurities such as Ca 2+, Mg2+, Fe2+, SO42-, and CO32-.
NaCl solution is filtered, it aims to remove solid impurities such as sand that may still be
present in the salt.
The resulting filtrate is then added 0:05 grams of calcium oxide (CaO). The function of the
addition of calcium oxide is to precipitate impurities such as impurities roomates contains
SO42-, and CO32- that contained in dirty salt. The reaction that happened:
CaO
Ca2++ CO32Ca2++ SO42-

Ca2+ + O2CaCO3(s)
CaSO4(s)

The solution which has been added CaO powder was then added again with a solution of
Ba(OH)2 aqueous to bind impurities in the form of Mg2+, CO32-, Fe2+, dan SO42-.
Ba(OH)2
Ba2+ + 2OH2+
2Ba + CO3
CaCO3(s)
Ba2+ + SO42BaSO4(s)
Fe2++ 2OHFe(OH)2(s)
Mg2++ 2OHMg(OH)2(s)
Then the solution was filtered to remove sediment that occurs.
Added (NH4)2CO3, drop by drop until no white precipitate formed to bind Ca 2+ and Ba2+
derived from CaO and Ba(OH)2. The addition is done dropwise with the aim to avoid excess
reagent (CO32-) that would contaminate the salt back. The reactions that occur
(NH4)2CO3

2NH4++ CO32-

Ba2++ CO32Ca2++ CO32-

BaCO3(s)
CaCO3(s)

The solution was allowed to stand 5 minutes, then filtered to obtain a filtrate, expected this
filtrate containing NaCl at higher levels. Good salt should have a neutral pH of the filtrate
was added HCl until the solution became neutral. The reaction that occur:

NH4+ + HCl

NH4Cl (neutralization)

Furthermore, the filtrate evaporated to regain solid NaCl crystals, NaCl results of
observations refining the color whiter and finer-textured. Having weighed and calculating an
increase in levels of NaCl, of 90 498% to 95.52%.

b) Determination of purity levels of NaCl

To determine the levels of NaCl in the salt that has been purified, it is necessary to titration.
Do three kinds of titration with 3 repetitions to obtain the right volume. NaCl is titrated with
AgNO3 and K2CrO4 as an indicator. Titration is done until the color changes to red brick and
white precipitate formed.
The initial stage is done is standardized AgNO 3 with NaCl. From the trial and after the
calculations, the normality of AgNO3 0.09963 N. titration is then performed to determine the
initial NaCl concentration in the same way. Averages volume AgNO 3 gained 3.9 ml and the
obtained data, the NaCl levels of 90 498%. Lastly, to the titration to determine the
concentration of NaCl after purified. Averages volume AgNO 3 used to react with NaCl hasi
purification of 4.1033 ml after calculation known final concentration of NaCl 95.52%. The
reaction that occur is:
AgNO3+ NaCl
AgNO3 + K2CrO4

AgCl(s) +
white precipitation
Ag2Cr2O4 +
red brick

NaNO3
KNO3

G. Conclusion
1. Crystallization is the separation of a crystalline solid material from a solution based on the
differences of solubility between the purified substance and impurities in a particular
solvent.
2. NaCl purification is done by recrystallization method with the addition of impurity binder material
such as CaO, Ba(OH)2, and (NH4)2CO3.
3. The purity levels of NaCl decrease after purification, from 90.498% into 95.52%.
H. Suggestion
1
2
3

I.

We must study the theory before do the experiment

We must do the experiment carefully
When adding acid (HCl) must be done carefully then the pH not changes too acid.

Bibliography
Bahruddin, Zulfansyah, Aman, Ilyas Arin, and Nurfatihayati .2003. Penentuan Rasio Ca/Mg
Optimum pada Proses Pemurnian Garam Dapur. Jurnal Natur Indonesia 6, Vol.1 No.16.

Lesdantina, Dina dan Istikomah, 2009, Pemurnian Nacl Dengan Menggunakan Natrium
Karbonat, Seminar Tugas Akhir S1 Teknik Kimia. Semarang.UNDIP
Nur, M. 2013 . Pengayaan Yodium dan Kadar NaCl pada Garam Krosok menjadi Garam
Konsumsi standar SNI. Jurnal Sains dan Matematika. Vol. 21 (1): 1-6.
Underwood, A. L dan Day A. R. 1990. Analisis Kimia Kuantitatif Edisi Kelima. Jakarta : Penerbit
Erlangga.

J. Attachment