EXPERIMENT I

NaCl PURIFICATION
Date of labwork : April 28th 2015

A OBJECTIVE
1 Study the recrystallization method with the addition of impurity binder material.
2 Understand the methode of NaCl iodisation.
3 Calculate the purity levels of NaCl
B THEORETICAL BASIS
Salt or sodium chloride (NaCl) is a white solid substance which can be obtained by
evaporating and purifying sea water. it also can be obtained from the neutralization HCl
with NaOH solution. NaOH almost insoluble in alcohol, but soluble in water by absorb
heat, the change of solubility is very small with temperature. Normal salt is a salt which
does not contain hydrogen or hydroxide group which can be evicted. The aqueous
solution from normal salt is not always neutral to indicator, such as litmus. Double salt
is a salt which id formed from crytallization from an equivalen of two or more certain
salt, for example FeSO4(NH4)2SO4.6H2O and K2SO4Al4(SO4)3.24H2O.In the solution, this
salt is a mixed of any simple ions that will be ionizing when its dissolve again. So,
clearly different with complex salt that produce complex ions in the solution. (Syabatino,
2009)

Figure. 1. The structure of salt (Saito.1996).

Sodium chloride (NaCl) is a typical compound in its structure Cl - anion arranged in
ccpand Na+ cation occupy the octahedral hole (Oh) (Figure.1.). Each Na+ cation is
surrounded by six Cl- anion (Saito.1996). The characteristic of NaCl crystal is cube
formation because NaCl crystallized with lattice cube. NaCl crystal have great energy,
and relatively hard, tends to fall apart when exposed to blows, because the areas of ion
always shifting, moving from a state of attraction into repulsion. (Brady, 1994)
Sodium is a soft silver-white metal, which melt at 97,5 C. Sodium is oxidized
quickly in moist air, so it should be kept submerged in a naphta or xylena solvent. This
metal is reacted very easily with water, forming sodium hydroxide and hydrogen. In the
satl, sodium is as monovalent cation Na+. This salts in forming colorless solution, almost
of all sodium salt are soluble in water. (Shevla, G., 1979)

Sodium chloride is one of material that widely used by people in food processing
and raw material in many chemical industries. The chemical industry that use sodium
chloride as the raw material is chlor alkaly industry. The main product of this industry is
chlorine (Cl2) and sodium chloride (NaOH), which needed by another industry, like pulp
and paper industry, textile, detergen, soap and water processing. (Lesdantina, et al., 2009)
In technical engineering solid materials are often separated from the solution or
melt, without binding the obtained impurities in its liquid phase. Also often the solid
crystalline material which contain the impurity must be cleaned or must be produced in
certain crystal form, so the crystallization process can be used. The crystal are the solid
material with the arrangement of atom or molecule regularly. The definition of
crystallization in the separation of crystal solid material from its solution or melt. The
result of crystallization from its melt often must be cooled again or reduced in size.
(Bernaseoni, 1995)
The crystallization from its solution is categorized as one of the efficient separaton
process. In general, the purpose of crystallization is to produce crystal product with the
quality as expected. The quality of produced crystal can be determined fom the product
parameters, there are crystal size distribution, the purity of crystal and the size of crystal.
One of the crystallization process requirementts is the occurence of supersaturation
condition. The supersaturation condition is the condition when the concentration of the
solution up to its solubility. This condition can be reached by evaporating, colling or the
combination of both. There are two important phenomena in crystallization process is the
formation of crystal nucleous (nucleation) and crystal growth. (Shevla, G., 1989)
The crystallization is a methode for purifying a substance with a solvent followed
by the precipitation process. In organic compound crystallization is affected by the
solvent. The crystallize solvent is a solvent that carried by the solute that forming the
precipitate and depending on its solute crystal structure. (Oxtoby, 2001)
Recrystallization is one of the purifying solid methode that plural used, in which
these substances dissolved in a solvent then recrystalled. This methode is depend on the
solubility of substance in the solvent when the temperature increase. Because of the total
impurities concentration commonly smaller than the concentration of the purified, if
cold, so the impurities concentration low but in the solution the product that has hight
concentration will form precipitate. (Arsyad, 2001)
Reccrystallization events accociated with the precipitation reaction. The precipitate
is a substance that separate as a solid phase and comes out from the solution. the
precipitate formed if the solution become too saturated with the concerned substance.
The solubility (S) of a precipitate according to the definition is equal with the molar
concentration of its saturated solution. the solubility depends on various condition such
as temperature, pressure, the other concentration of substance in the solution, and the
solvent composition. (Keenan, 2009)
The influence of the decreasing temperature in the crystal formation process :
a. If the decreasing temperature run faster, so the nucleous will formed faster than the
formation of crystal so the crystal obtained is small, fragile, and much.

b. If the decreasing temperature run slower, so the formation of crystal will run faster
than the formation of the nucleous so the crystal will be freed big, tough and elastic.
(Austin, 1986)
The precipitate is a substance that separate as a solid phase, out from the solution.
The precipitate is formed if the solution become too saturated with the concernned
substance. The solubility (S) of a precipitate according to the definition is equal with the
molar concentration from its saturated solution. The solubility is deppend on various
condition, such as temperature, pressure, concentration of another substance in its
solution, and the compotion of the solvent.
The solid organic compounds from the isolated organic reaction rarely in pure
form. Its compound are ussually contamined with a little another compound (impurities)
which formed during the reaction occured. The impurities in salt include hygroscopic
compound, there are MgCl2, CaCl2, MgSO4, and some reductor substance, there are Fe,
Cu, Zn and organic compounds. Its impurities can be reacted with hydroxil ion (OH -) so
it form white precipitate Ca(OH)2 and Mg(OH)2. The purification of impure compound id
ussually done by recrystallization with various solvent or mixture solvent. (Bahruddin,
et, al, 2003)
The purification of solid with the recrystallization based upon the differences in the
solubility in current solvent or mixed solvent. There are some definition about the
recrystallization, there are : 1. A process where the metal grains which is deformed is
replaced by the new grains that are not deformed which its nucleous grow until the
original grains included therein. 2. The change of crystal structure due to the heating at
critical temperature. 3. The formation of new structure of the grains through the grow of
nucleous by heating. (Anwar, 1994)
To reduce the salt impurities can be done with the combination froom the leaching
process and dissolving quickly at the process of making salt. While the removal of
impurities from the salt product can be done by chemical process, there is by reacting
with Na2CO3 and NaOH to form CaCO3 ang Mg(OH)2 precipitate. The addition of
Na2CO3 and NaOH is an important process in purifying salt process. To avoid the
occured of precipitate breaking which caused by the flagile metal hydroxide
characteristic, so Na2CO3 and NaOH added simultaneously and react together. The both
precipitation of CaCO3 and Mg(OH)2 will occured faster than the precipitation of
hydroxide. The good result also can be obtained if the Na 2CO3is added first before the
addition of NaOH. (Berseoni, 1995)

C METHODE
Equipment
Analytical balance
Bunsen burner
Burette 50 mL

Material
Dirty salt
CaO powder
Ba(OH)2 solution 1 M

Erlenmeyer 25 mL
Volumetric flask 100 mL
Volume pipette
Evaporating basin
Dropping pipette
Watch glass
Beaker glass
Spatula
Stirrer
Filter paper
Universal pH indicator paper

(NH4)2CO3 solution 0.1 M

Concentrated HCl 0.1 M
AgNO30.1 N solution
Aquades
K2CrO45%
HNO3 solution 0.1 M

Methode
1. Purification of NaCl
Weight 2.5 gram
dirty salt with
analytical balance

Heat 25 mL aquades
in beaker glass up to
boil

Weight 0.05 gram

CaO and then added
into salt solution

Filter the
precipitate formed

Add Ba(OH)2 solution 1

M dropwise until does not
form precipitate

Evaporate the
solution up to dry in
evaporating basin

Weight the dry

crystal obtained

Filter the
precipitate

Neutralize the filtrate with

HCl 0.1 M (tested with
universal indicator paper)

Add 2.5 gram dirty

salt into boiled water
stir and heat again

After all salt

dissolved, filter it
using filter paper

Add Ba(OH)2 solution 1 M

dropwise until does not
form precipitate ( 3 mL)

Allow the solution for 5

minute then filter the
precipitate

Dry and weight the

impurities precipitate
from the filtration

2. Determination of Purity Levels of NaCl

Weight 0.25 mgram
dirty salt using
analytical balance

Dissolve it into 100 mL

aduades in volumetric
flask 100 mL

Move it into
erlenmeyer

Add 1 mL
indicator K2CrO4
5%

Take 10 mL of
solution put into
erlenmeyer

Reperat the
titration two times
and record the
volume of AgNO3

Titrate the solution with

AgNO3 solution until it
become red brick

Check the pH until neutral

with universal indicator paper,
if too acid add NaHCO3 and if
too base add HNO3

Replace the dirty salt

with pure NaCl for
titration and NaCl p.a.
for standaisation

D OBSERVATION DATA
a Color of the salt before purified : dirty white.
b Structur of salt crystals before purified : big, rought.
c Color of the salt after purified : clear white.
d Structure of salt crystals after purified : smooth.
e Volume of Ba(OH) required is : 3 mL
2

Volume of (NH4)2CO3 required is : 5 mL

g
h
i

The weight of impurities from salt recrystallizing :

The weight of salt crystal from salt recrystallizing : 1.295 gram
The precentage of pure salt from recrystallizing process :
mass of pure salt
% pure salt = mass of dirty salt x 100%
=

1.295 gram
2.50 gram

x 100%

= 51.8 %
j

Titration data :
Standarisation of NaCl p.a.
Volume of NaCl p.a.
Volume of AgNO3
10 mL
4.50 mL
10 mL
4.40 mL
Average volume
4.45 mL
Determination of N AgNO3
VNaCl . N NaCl = V AgNO3 . N AgNO3
0.25 gram
1000
10 . 58.46 gram/mol x 100 mL x 1 ekivalen = 4.45 mL . N AgNO3

0.4276 molek/mL
= 4.45 mL . N AgNO3
N AgNO3 = 0.0961 molek/mL
Titration of dirty NaCl

Volume of dirty NaCl

10 mL
10 mL
Average volume

Titration of pure NaCl

Volume of pure NaCl
10 mL
10 mL
Average volume

Volume of AgNO3
3.52 mL
3.50 mL
3.51 mL

Volume of AgNO3
4.18 mL
4.26 mL
4.22 mL

The purity levels of NaCl before recrystallization process :

( V . N ) AgN O3 x 58.46
100
The purity level of NaCl =
x
10
w x 1000
=

3.51 x 0.0961 x 58.46

0.25 x 1000

x 100%

x 10 x 100%

= 78.87 %
l

The purity levels of NaCl after recrystallization process :

( V . N ) AgN O3 x 58.46
100
The purity level of NaCl =
x
10
w x 1000
=

4.22 x 0.0961 x 58.46

0.25 x 1000

x 100%

x 10 x 100%

= 94.83 %
m Reactions :
The reaction between NaCl and CaO
CaO(aq)
Ca2+ (aq) + O2-(aq)
2+
2Ca (aq)+ CO3 (aq) CaCO3(s)
Ca2+(aq)+ SO42-(aq) CaSO4(s)

Ksp = 4.8 x 10-9

Ksp = 2.3 x 10-4

The reaction of Ba(OH)2 addition

Ba(OH)2(aq)
Ba2+(aq) + 2OH-(aq)
2+
Fe (aq) + 2OH (aq) Fe(OH)2(s)
Ksp = 4.8 x 10-16
Mg2+(aq) + 2OH-(aq) Mg(OH)2(s)
Ksp = 3.4 x 10-21
The reaction of (NH4)2CO3addition
(NH4)2CO3(aq)
2NH4+(aq) + CO32-(aq)
Ba2+(aq)+ CO32-(aq)BaCO3(s)
Ksp = 8.1 x 10-9
2+
2Ca (aq)+ CO3 (aq)CaCO3(s)
Ksp = 4.8 x 10-9
The reaction of HCl addition
NH4+(aq) + HCl(aq) NH4Cl(aq)
The reaaction in the determination of the purity levels of NaCl
AgNO3(aq) + NaCl(aq)
AgCl(s) + NaNO3(aq) (white)
2AgNO3(aq) + K2CrO4(aq) Ag2CrO4 (s) + 2KNO3(aq)
(red brick)

E DISCUSSION AND REVIEW

This experiment is about the NaCl purification and iodisation. The purpose of the
experiment are to learn the NaCl crytallization methode by the addition of the impurities
binder and to determine the purity level of NaCl obtained. To determine the purity level
of NaCl, we done the titration as much as three. The first is the titration to standarisation
AgNO3, then the titration to determine the precentage of dirty salt, and the last is the
titration to determine the purity level of the salt from recrystallization.
1 Purification of NaCl
The first experiment is the purification of NaCl. The principal of this
experiment are crystalization and recrystallization by the evaporation and
precipitation process. This method is based on the differences among the purified
substance with the impurities in a solvent. For the recrystallization process, we need
a solvent with the differences in solubility between the substance and the impurities.
Because in the salt there are some impurities, there are Ca2+, CO32-, and SO42-ions.
In this experiment, we use dirty salt so in this experiment we done the
purification process to remove the impurities from the dirty salt. The first step on
this experiment is we dissolve as much as 2.5 gram dirty salt into 25 mL of boiling
aquades in order to the salt can be dissolved perfectly. In this process the salt will
had the ionization process and it will be decomposed into their ions, there are
sodium ion (Na+) and chloride ion (Cl-). After all the salt was dissolved, then it was
filtered using filter paper and it filtrat will be used to recrystallization process in the
next step.
After we get the filtrat from the first filtration, then add with 0.05 gram of CaO
powder. The fuction of this addition is to precipitate the impurities that contained in
the dirty salt. The principal work of CaO same with the alum, as a coagulants. After
the addition of CaO, Ca2+ ion will separate and it will bind with CO 32-and SO42- ions
and form white precipitate (CaCO3(s)and CaSO4(s)).CaCO3 and CaSO4 can be
precipitated because the Qc of both is smaller than its Ksp. Eventualy, we get the
solution which more pure than before. The occured reactions are :
CaO(aq) Ca2+ (aq) + O2-(aq)
Ca2+(aq)+ CO32-(aq)
CaCO3(s)
Ksp = 4.8 x 10-9
Ca2+(aq)+ SO42-(aq)
CaSO4(s)
Ksp = 2.3 x 10-4
After the precipitate are formed, we filter it using filter paper and then we get
the filtrate and the residue. The residue is Ca 2+ ion and the filtrate is the salt without
Ca2+ ions. Then the filtrate added with Ba(OH) 2 1.0 M dropwise until the last drop
does not form a precipitate, its about 3 mL. The function of Ba(OH) is same as
2

CaO, but Ba(OH)2 is used to remove the Mg2+ and Fe3+ ion as an impurities and form
white precipitate. The white precipitate are Fe(OH)2(s)and Mg(OH)2(s) . Fe(OH)2(s)and
Mg(OH)2(s) can be precipitated because the Qc of both is smaller than its Ksp. The
occured reactions in this process are:
Ba(OH)2(aq)
Ba2+(aq) + 2OH-(aq)
Fe2+(aq) + 2OH-(aq) Fe(OH)2(s)
Ksp = 4.8 x 10-16

Mg2+(aq) + 2OH-(aq) Mg(OH)2(s)

Ksp = 3.4 x 10-21
Then to separate the precipitate with the solution, we filter it using filter paper.
From the filtration we get the residue and the filtrate. The residue is the impurities
precipitate and the filtrate is the more pure salt. After that, we add the filtrate with
0.1 M (NH4)2CO3 solution dropwise until the last drop does not form a precipitate.
Its about 5 mL. This addition is to bind the renmants of impurities that may still
exist, there are Ba2+ and Ca2+ ions. After the addition it will form white precipitate.Its
BaCO3(s) and CaCO3(s) precipitate. BaCO3(s) and CaCO3(s) can be precipitated because
the Qc of both is smaller than its Ksp. The occured reactions in this process are :
(NH4)2CO3(aq)
2NH4+(aq) + CO32-(aq)
Ba2+(aq)+ CO32-(aq)BaCO3(s)
Ksp = 8.1 x 10-9
2+
2Ca (aq)+ CO3 (aq)CaCO3(s)
Ksp = 4.8 x 10-9
Then we separate the precipitate as a residue with the solution as a filtrate by
the filtration process using filtrat paper. With the addition of three solvent, it can be
assumed that the salt have alredy pure and does not contain impurities. But because
of these process makes the solution does not neutralanymore. Eventhough the good
salt is in neutral condition. So, it need neutralization process to make it neutral again
and it can be done by the addition of dillute HCl into the filtrate until it neutral
checked using universal indicator pH paper. The reaction is :
NH4+(aq) + HCl(aq)NH4Cl(aq)
After the solution is neutral, then the solution is evaporate until all solution
formed salt crystal again (recrystallization process). This evaporating process is done
using evaporating basin. The formation of salt after recrystallization is the structure
become smooth and the color become clear white. Then weight the crystal analytical
balance and we get the crystal as much as 1.295 gram, its smaller from initial mass
of salt because its impurities has gone. Based on the calculation we get the
precentage of rendemen 51.8 %.
2

Determine the Purity Levels of NaCl

The determination of purity levels of NaCl in done two times. The first is to
determine the purity levels of dirty salt and the second in to determine the purity
levels of pure salt from the first experiment. But before the determination of purity
levels, we have to standardization AgNO3 solution at first. After the standardization
process, we can determine the number of N AgNO 3 that we used to titration with
dirty and pure salt. Based on the calculation, the N of AgNO3 is 0.0961 molek/mL.
After that we determine the purity levels of dirty salt by the titration process.
The first we weight as much as 0.25 gram dirty salt and dissolved in 100 mL
aquades. Then take 10 mL of the solution for titration and add with K 2Cr2O4 as
indicator. Titrate the solution with AgNO3 until the color of solution become red
brick. Based on the data, the average volume of AgNO3 neede in the titration process
is 3.51 mL and based on the calculation we get that the purity levels of this salt is
78.87%.
Then, we determine the purity levels of pure salt from the recrystallization
process. Same with before, to determine the purity levels of salt we weight as much

as 0.25 gram of salt and then dissolved in 100 ml aquades. Then take 10 mL of the
solution and add with K2Cr2O4 as indicator. Titrate it with AgNO3 until the color
become red brick. Based on the experiment, the average volume of AgNO 3 is 4.22
mL and based on the calculation the purity levels of this salt is 94.83 %.
This is accordance with the theory that the purity levels after recrystallization
is bigger than the purity levels of dirty salt. The structure of the pure salt become
smooth and the colour become clearl white. The occured reaction is this process are :
AgNO3(aq) + NaCl(aq) NaNO3(aq) + AgCl(s)
(white)
2AgNO3(aq) + K2CrO4(aq) 2KNO3(aq) + Ag2CrO4 (s) (red brick)
F CONCLUSION
The principal method of the NaCl purification is recrystallization with the
evaporation and with the addition of some solutions such as CaO, Ba(OH) 2, and
(NH4)2CO3 to bind the impurities like Ca2+, CO32-, SO42-, Mg2+ and Fe2+ions.
The purity levels of NaCl ditry salt is 78.87% and the purity levels of NaCl pure salt
from recrystallization is 94.83%.
The NaCl salt after the purification process has smooth structure and the color
become clear white because the impurities has gone.
G SUGGESTION
Be carefull with dangerous material such as AgNO3 and use gloves when use it.
Be careful when add some binder material.
Do the titration accurately and carefully.
Observe the experiment result accurately.
H LITERATURE
Anwar, C. 1994. Pengantar Praktikum Kimia Organik I. Yogyakarta :FMIPA UGM..
Arsyad, M. Natsir. 2001. Kamus Kimia dan Penjelasan Istilah. Jakarta : Gramedia.
Austin, G. T. 1996. Industri Proses Kimia, Edisi Kelima. Jakarta : Erlangga.
Bahruddin, Zulfansyah, Aman, Ilyas Arin, Nurfatihayati. 2003. Penentuan Rasio Ca/Mg
Optimum pada Proses Pemurnian Garam Dapur. Jurnal Natur Indonesia 6(1):
16-19.
Bernaseoni,G. 1995. Teknologi Kimia. Jakarta : PT Padya Pranita.
G. Svehla. 1979. Buku Teks Analisis Anorganik Kualitatif Makro dan Semi Mikro Bagian
I. Jakarta : PT Kalman Media Pustaka.
G. Svehla. 1985. Buku Teks Analisis Anorganik Kualitatif Makro dan Semi Mikro Bagian
I. Jakarta : PT Kalman Media Pustaka.
Keenam.1979. Kimia Universitas Jilid 2.Jakarta:Erlangga.
Lesdantina, D., dan Istikomah, 2009. Pemurnian Nacl Dengan Menggunakan Natrium
Karbonat. Seminar Tugas Akhir S1 Teknik Kimia UNDIP.
Oxtoby, D. W. 2001. Kimia Modern. Jakarta : Erlangga.
Saito, Taro. 1996. Muki Kagoku. Tokyo : Iwanami Shoten Publisher
Syabatini, A.,. 2009. Pemurnian Bahan Melalui Rekristalisasi. http://annisanfushie.
wordpress.com. Diakses tanggal 28 April 2015.

APPENDIX
1 Purification of NaCl

Boiling aquades

Dirty salt + boiled aquades

Impurities

Filtrate + CaO

Residue (CaCO3(s)and CaSO4(s))

White precipitate

Residue

Evaporate the salt

Filtrate

Residue

Filtrate

Ba(OH)2

Filtrate

Check pH

Pure salt crystall from recrystallization

Filtrate +Ba(OH)2
dropwise

Filtrate + (NH4)2CO3

Pure salt solution

Weight the crystal

Determination of purity levels of NaCl

Standarisation AgNO3

Check pH

Titration of dirty salt

Titration of the salt

Titration of pure salt