EXPERIMENT I

NaCL PURIFICATION
19 Mei 2015

A. OBJECTIVES
1. Study the recrystaliization method with the addition of impurity binder material
2. Understand the methods of NaCl iodisation
3. Calculate the purity levels of NaCl
B. THEORETICAL BACKGROUND
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 with recrystallization method widely applied in industrial laboratories
and aimed to improve the quality of a substance/material. In principle, the substance
which was purified is dissolved in a solvent then it was heated and evaporated again.
Impurities meterials that can not be dissolved, can be separated from the solution by
filtration. The impurities will be soluble in the solution.
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:
1. Dissolving the impurity substances in certain solvent at near the melting point
2. Filtering the particles of insoluble materials in hot solution condition
3. Cooling the hot solution of the solute into the crystal
4. Separating the crystal from the solution of supernatant
Another thing to note on 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.
1. Providing sufficient difference in solubility between the purified substance and
impurities
2. Not leaving impurities in the crystal
3. It easily to be separated from the crystals
4. It is inert (does not react easily with the crystal)
Impurity binder is the ingredient that makes something to be tied / bounded. While
impurities are foreign substances whose presence is not desired in a pure substance. So the
impurity binder is a material or substance that can be used bind foreign substances whose
presence is not desired in a pure substance. In theory salt in the common community is a
salt with consumption levels, it must have a minimum of 94,7% NaCl for salt with no
iodine. According to SNI number 01-3556-2000, iodized salt is a salt containing a major
component of NaCl (sodium Chloride/mineral) 94,7%, water maximum of 5%, potassium
iodate (KIO3) 30 ppm, and other compounds in accordance with specified requirements,
but in fact the levels of NaCl in salt is far below this standard.
For that reason, it needs an effort to improve the purity of the salt. On way to do is
with the addition of a impurities binder material. This binder is an ingredient deliberately
added to a solution of salt in order to bind the impurities that are already there in the salt
through the formation of sediment/precipitate (Inorganic Chemistry Lecture Team, 2015).

Salt (NaCl) is in the form of a white solid material, has the shape of a cube crystal
transparent, non-flammable and has a melting point of 801 oC. Salt is a compound
composed of a strong acid HCl and a strong base NaOH. If this element is treated, it will
form NaCl and H2O. Results of earlier material when put together will form a solution
called saline. The solution formed a homogeneous mixture, the particles are very small but
spread evenly though left in a long time. NaCl or salt will not settle if allowed and can not
be separated from the water by filtration. Partikelpartikel NaCl, ions in the water can not
be seen with a microscope. Solute and solvent completely homogeneously mixed.
Sodium chloride is one material that is widely used by people in food processing
and raw material in various chemical industries. The chemical industry is the most widely
used sodium chloride as raw material is Chlor Alkali industry. The main products of this
industry are chlorine (Cl2) and sodium hydroxide (NaOH), which is required by many
other industries, such as pulp and paper, textiles, detergents, soap and waste water
treatment.
Sodium is a soft silver-white metal, which melt at 97.5 oC.Natrium oxidizes rapidly
in moist air, it should be kept submerged in a solvent naphtha or xylene. The metal reacts
violently with water, forming sodium hydroxide and hydrogen. In the salts of sodium are
as monovalent cations Na+. These salts to form a colorless solution, almost all of the
sodium salt dissolved in water (Vogel, 1979).
In chemical engineering often solid materials to be separated from the solution or
melt, without binding impurities contained in the liquid phase. Often also solid crystalline
material containing impurities must be cleaned or to be produced certain crystalline forms,
for such purposes crystallization process can be used. Crystals are solid materials with the
arrangement of atoms or molecules regularly. The definition of crystallization is the
separation of a crystalline solid material from a solution or melt. Results crystallization
from the melt often must be cooled again or reduced in size (Bernaseoni, 1995).
Purification of saline solution is strongly influenced by the ratio of Ca / Mg, when
the ratio is too small or too large can result in the deposition of impurities are not going
well. The ratio of Ca/Mg is best obtained at 2. From the research found that the addition of
flocculant enough to affect the decreased levels of Ca +2, and relatively little influence
decreased levels of Mg+2 and TSS. The ratio Ca/Mg by 2, Mg +2 levels were already below
the upper limit of the quality standard saline solution, without the addition of flocculants.
While the levels of Ca+2 and TSS is still more than twice the upper limit when no
flocculant, but still slightly above the upper limit for the Ca +2 and two times above the
upper limit for TSS when using flocculants (Bahruddin, 2003).
Influence is the power that exist or arise from something (people, objects, and so
on) are in power or strength. The influence of this research is the relationship that affects
the use of salt (NaCl) in the cooling medium in varying levels of violence in the process of
hardening steel V-155. Cooling material used in this study is the water added salt (NaCl)
to the NaCl content of each are: 9%, 16% and 23% (Rizal, 2005).
Crystallization from solution is categorized as one of the efficient separation
process. In general, the purpose of the crystallization process is to produce a crystalline
product with quality as expected. The resulting crystal quality can be determined from the
parameters of the crystal size distribution of the product that is), the purity of crystal and
crystal form. One of the requirements is the occurrence kiristalisasi supersaturated
condition. Supersaturated condition is a condition where concentration is above the

solubility price. This supersaturated condition can be achieved by means of evaporation,

cooling or a combination of both. There are two important phenomena in the process of
crystallization is crystal nucleation (nucleation) and crystal growth (crystal growth)
(Puguh, et al., 2003).
To reduce the salt impuristis can be done with a combination of leaching and rapid
dissolution at the time of manufacture garam.Sedangkan removal of impurities from salt
product can be done with a chemical process, ie reacting with Na 2CO3 and NaOH to form
a precipitate CaCO3 and Mg(OH)2. The addition of Na2CO3 and NaOH is a very important
part of the process in the refining process salt solution. To avoid breaking the sediment
caused by nature fragile metal hydroxide, then added Na 2CO3 first of NaOH. The best
results will be obtained if Na2CO3 and NaOH are added simultaneously so that it will
produce the same reaction. Precipitation along CaCO 3 and Mg(OH)2 will take place faster
than the hydroxide sludge that settles itself. Good results are also obtained if Na 2CO3 is
added first before adding NaOH (Bahruddin, et al., 2003).
The decline in the influence of temperature on the Process of Crystals
a. When the temperature drop runs faster then the speed of the crystal nucleus grows faste
than the speed of crystal growth so that the crystal obtained by small, fragile, and more.
b. When the temperature is done slowly decline, the crystal growth rate is faster than the
speed of crystal growth so that the crystal nucleus is freed big, tough, and elastic
(Austin, 1986)

C. EQUIPMENT AND MATERIALS

Equipment :
Digital balance
Bunsen
Burrete 25 mL
Erlenmeyer 25 mL
Dropping pipette
Watch glasses
Beaker
Materials:
Dirty salt
CaO powder
Solution of Ba(OH)2
Solution of (NH4)2CO3
Concentrated HCl
Aquades
Solution KIO3
Solution of HNO3
Solution of AgNO3
Universal pH indicator paper
D. WORK INSTRUCTION

Purification of NaCl
Heat 25 mL of distilled water in beakerglass up to boil

enter 2,5 g of dirty salt to hot water, stir and heat again until all salt
dissolved in boiling water and then filter it

Add 0,05 g of CaO into solution, filter the precipitate happened

Add Ba(OH) 1.0 M dropwise until the last drop does not form a
precipitate

Add about 5 mL (NH4)2CO3 0.10 M dropwise until the last drop does
not form a precipitate

Allow the solution for 5 minutes, so we can observe the formation of

the precipitate clearly

Filter the solution and neutralize the filtrate with dilute HCl (tested
with universal indicator paper)

Evaporate the solution up to dry. Weigh the crystals obtained

Dry and weigh the impurities precipitate obtained from filtration

Determination of Purity of
NaCl

250 mg samples of dirty salt dissolved in 100 mL of

distilled water (100 ml volumetric flask), then move
into the erlenmeyer

Check the pH, if too much acid, add a solution of

NaHCO3 and add HNO3 if too alkalinr to be neutral pH.
for the argentometri titration, take 10 ml of solution
and enter to erlenmeyer

Add 1 ml indicator K2CrO4 5%

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

solution color is red brick. Silver ions from AgNO3 will
react with Cl- ions produces a white precipitate

Repeat the titration two times

Do the determine of purity levels of NaCl before and

after recrystallized process

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

f. Volume of (NH4)2CO3 required is : 4 mL

g. The weight of impurities from salt recrystallization : 2,5 gram
h. The weight of salt crystal from salt recrystallizatiom : 1,4697 grm
F. ANALYSIS DATA
a. The percentage of pure salt from recrystallization process :
Weight of pure NaCl : 1,467 gram
Weight of dirty NaCl : 2,5 gram
weight of pure salt
The percentage of pure salt=
x 100
weight of dirty salt

1,4697
x 100
2,5

= 58,78%
b. Titration data
Standardisasi AgNO3 :
Volume NaCl
10 mL
10 mL
Titration dirty salt
Volume NaCl
10 mL
10 mL

Volume AgNO3
4,4 mL
4,1 mL
4,25 mL

Volume AgNO3
3,5 mL
3,6 mL
3,55 mL

Titration pure salt

Volume NaCl
10 mL
10 mL

Volume AgNO3
3,6 mL
3,7 mL
3,65 mL

c. The purity levels of NaCl before recrystallization process :

V
N
.58,46 100
Purity of NaCl= AgNO 3 . AgNO 3
x 100
W . 1000
10

3,55 . 0,1006 .58,46 100

x
x 100
0,25 . 1000
10

83,51
d. The purity levels of NaCl after recrystallization process :
V
N
.58,46 100
Purity of NaCl= AgNO 3 . AgNO 3
x 100
W . 1000
10

3,65 . 0,1006 .58,46 100

x
x 100
0,25 . 1000
10

 85,86

G. DISCUSSION
a. Purification of NaCl
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. NaCl is the main component to be purified of
impurities derived from the ions Ca2+, Mg2+, Al3+, SO42-. So that the solubility between
NaCl with impurities is large enough, it is necessary to specific substances. Additional
substances that will form compounds mainly poorly soluble salts in the water, in
addition to the recrystallization can be done by adding a type ions into a solution of
the substance to be separated. For this NaCl recrystallization using deposition methods
because the results are better and faster procedure. Recrystallization is refining a solid
substance from a mixture / impurities by way of crystallizing back these substances
after dissolved in a suitable solvent. Recrystallization principle is the difference
between the solubility of the substance to be purified with solubility mixer /
pencemarnya. The solution is happening separated from one another, then a solution of
the desired substance crystallized by menjenuhkannya.
The first step is dissolving 2.5 grams of salt were dirty white with hot water.
Use hot water soluble salt that perfectly. Once dissolved, and then filtered which aims
to filter out impurities in the salt as sand. After the filtrate was added 0.05 grams of
CaO. Addition of CaO is intended to bind impurities such as Ca 2+, Fe3+, and Mg2+,
CO32-, SO42- contained in the salt. Reactions that occur.
CaO(s) CaO(aq)
CaO(aq) Ca2+(aq) + O2-(aq)
Ca2+(aq) + CO32-(aq) CaCO3(s)
Ca2+(aq) + SO42-(aq) CaSO4(s)
Mg2+(aq) + O2-(aq) MgO(s)
2 Fe3+(aq) + 3 O2-(aq) Fe2O3(s)
After the addition of CaO white precipitate is formed which is then filtered.
The filtrate was then added a solution of Ba(OH) 2. Addition of Ba(OH)2 will bind
impurities in the form of Mg2+, Al3+, Fe2+, and SO42-, and prevent the formation of
deposits that may occur due to the addition of CaO in the previous process. Reactions
that occur.
Ba(OH)2(aq) Ba2+(aq) + 2 OH-(aq)
Ba2+(aq) + SO42-(aq) BaSO4(s)
Mg2+(aq) + 2 OH-(aq) Mg(OH)2(s)
Al3+(aq) + 3 OH-(aq) Al(OH)3(s)
Fe2+(aq) + 2 OH-(aq) Fe(OH)2(s)
After that, the precipitate is filtered and set aside. At the filtrate was then added
a solution of (NH4)2CO3 until no more precipitate formed. The addition of a solution of
(NH4)2CO3 to bind more impurities remaining in the form of SO 42-, and excess Ca2+
and Ba2+ from the previous process. His reaction
(NH4)2CO3(aq) 2 NH4+(aq) + CO32-(aq)

2 NH4+(aq) + SO42-(aq) (NH4)2SO4(s)

Ca2+(aq) + CO32-(aq) CaCO3(s)
Ba2+ + CO32- BaCO3(s)
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, and (NH4)2CO3 so filtrate needs to
be neutralized by the addition of HCl solution, until the solution becomes neutral as
indicated by the green color on universal pH indicator paper. The reaction :
NH4++ HCl NH4Cl
Filtart then evaporated until all the solvent evaporates and obtained crystals of
pure NaCl. After the NaCl crystals obtained weighed 1.4697 grams total with the
percent pure salt amounted to 58.78%. The color of salt obtained are cleaner than the
salt used for crystallization before.
b. Determine purity NaCl
To determine levels of purity NaCl purification results above do titration using
AgNO3 solution using K2CrO4 solution as an indicator. AgNO3 solution to be used
should be standardized beforehand because AgNO3 is not a primary standard solution.
The solution used for standardization AgNO3 solution is a solution of HCl pa after that
titrated obtained normality AgNO3 solution is 0.1006 N. The reaction when titration :
AgNO3+ NaCl NaNO3 + AgCl(s) (white)
AgNO3 + K2CrO4 KNO3 + Ag2Cr2O4(s) (redbrick)

Then do the titration duplicate for each salt before and after the crystallization
process of the crystallization process. To salt prior to the crystallization process
required 3.55 mL AgNO3 solution, and obtained this level of purity of 83.51% NaCl.
As for the salt that has crystallized titration require as much as 3.65 mL AgNO 3
solution and NaCl purity obtained after recrystallization process by 85.86%. This
shows an increase NaCl purity, it can be stated that this crystallization process can
bind impurities in the salt so that the purity increases. However, the increase in the
level of purity NaCl did not show significant numbers, it can happen for several
reasons, which include the addition of a binder impurities such as CaO, Ba(OH) 2, and
(NH4)2CO3 too much so that in addition to binding impurities also become impurities
itself because it is not bound.
H. CONCLUSSION
1. Purification of NaCl can be done through the process of crystallization with the
addition of materials that can bind impurities, this material can be CaO, Ba(OH) 2, and
(NH4)2CO3 which can bind to ions in NaCl form of Mg2+, Fe2+, Al3+, CO32-, and SO42-.
2. From the obtained salt crystallization process as much as 1.4697 gram of pure NaCl
with the percent 58.78%
3. To determine the degree of purity of NaCl carried out by titration using AgNO 3
standard solution. Titration obtained from NaCl purity before recrystallization process
by 83.51%, and after the process of crystallization increased to 85.86% purity.
I. SUGGESTION
1. Before the practitioner should have a grasp lab practicum process
2. When adding a binder impurities considered when sediment really is no longer formed
3. Thorough in reading the scale on the buret

J. REFERENCE
Bernaseoni,G. 1995. Teknologi Kimia. PT Padya Pranita. Jakarta.
Bahruddin, Zulfansyah, Aman, Ilyas Arin & Nurfatihayati. 2003. Penentuan Rasio
Ca/Mg Optimum pada Proses Pemurnian Garam Dapur. Laboratorium Teknologi
Produk, Laboratorium Proses Pemisahan & Pemurnian, Laboratorium Teknik
Reaksi Kimia, Jurusan Teknik Kimia, FT, Universitas Riau, Pekanbaru.
Inorganic Chemistry Lecture Team. 2015. Manual Work of Inorganic Chemistry
Practicum. Semarang: Laboratorium Kimia Anorganik
Lesdantina, Dina dan Istikomah. 2009. Pemurnian Nacl
Dengan Menggunakan
Natrium Karbonat . Siminar Tugas Akhir S1 Teknik Kimia UNDIP. Jurusan
Teknik Kimia.Fak. Teknik. Universitas Diponegoro.
Rizal Taufan. 2005. Pengaruh Kadar Garam Dapur (Nacl) Dalam Media Pendingin
Terhadap Tingkat Kerasan Pada Proses Pegerasan Baja V-155. Fakultas
Teknik Universitas Negeri Semarang
Setyo,puguh, Wahyudi Siswanto, dan Heru Sugiyanto Ilham.Studi eksperimental
pemurnian garam NaCl dengan Cara Rekristalisasi.Jurusan Tekhnik
Kimia,Universitas Surabaya, Vol.11 No.2