Purification of NaCl and Iodization

A. OBJECTIVES

1. Study the recrystallization method with the addition of impurity binder material.
2. Calculate the purity levels of NaCl.

B. BASIC THEORY

Sodium is a soft silver white metal, which melts at 97.5°C. Sodium oxidizes
rapidly in moist air, so it must be completely submerged in naphtha or xylene solvents.
This metal reacts violently with water, forming sodium hydroxide and hydrogen. In its
salts, sodium chloride as a monovalent cation of Na+. These salts form a colorless
solution, almost all sodium salt dissolves in water. Most chlorides are soluble in water,
mercurium (I) chloride, HgCl2, silver chloride, AgCl, lead chloride, PbCl2 (which is
very little in cold water, but dissolves easily in boiling water), copper (I) chloride, CuCl,
bismuth oxychloride, BiOCl, stibium oxychloride, SbOCl, and mercurium (II)
oxychloride, HgOCl2 is insoluble in water (Vogel, 1985).

Sodium chloride is an ionic salt of Na metal. This compound is mostly

contained in seawater and salt rocks such as carnalite (NaCl.MgCl.6H2O) which is the
result of evaporation of sea water in geological periods. Salt lakes in Utah and dead
seas in Israel are examples of ongoing evaporation.

The chemical industry which uses the most NaCl as its raw material is the
alkali chlorine industry. The main products of this industry are chlorine (Cl2) and
sodium hydroxide (NaOH), which are needed by many other industries, such as the pulp
and paper industry, textiles, detergents, soaps and wastewater treatment (Bahruddin,
dkk., 2003).

NaCl can be said to have a tightly packed building of the cube so the smaller
Cl- and Na+ ions occupy the okatahedral cavity. In addition, this structure will also
show the shape of a face center cube built by Na+ ions as well as the Cl- ions.
Therefore, the crystal NaCl lattice is two central cube lattices that are embedded in one
another (interpenetration) (Sugiyarto, 2003).

Recrystallization can be used to separate the mixture of liquid and solids which
dissolve. Through recrystallization, a purer solid substance is obtained because the
composition of other solutions which are smaller in size do not participate in
crystallization. Separation of sugar from sugar cane and purification of various
substances is done by crystallization. Purification of salt can be done by
recrystallization. In this case the salt is dissolved in clean water then filtered and then
the filtrate crystallized. A substance that appears as a solid, but does not have a
reproductive structure called amorphous (without form) (Keenan, 1991).

The process of crystal formation is carried out in three stages, namely (1)
achieving supersaturation, (2) formation of a crystal core (nucleation), and 93) growth
of a crystal core into a crystal (crystal growth). Super-saturated conditions can be
achieved by cooling. Evaporation, addition of precipitant or as a result of chemical
reactions between two homogeneous phases. While the formation of the crystal core
occurs after the supersaturated condition is reached (Paryanto, 2007).
 Recrystallization is a separation technique based on differences in the freezing
point of components. The difference must be quite large and the components to be
separated are solid and the others are liquid at room temperature (Syukri, 1991).

There are two ways to get pure NaCl from coarse salt, the recrystallization
method through evaporation and precipitation. The precipitation method is based on the
difference in solubility between the substance to be purified and impurities in certain
solvents. In purification by evaporation it is generally carried out based on the solubility
of the ions in a salt in a particular solvent or solvent mixture in its simple form
(Underwood and Day, 1996).

One of the conditions for ciristalization is the occurrence of supersaturation

conditions. Supersaturation conditions are conditions where the concentration of the
solution is above the value of its solubility. This supersaturation condition can be
achieved by evaporation, cooling or a combination of both. There are two important
phenomena in the process of crystallization, namely the formation of the crystal core
(nucleation) and crystal growth (crystal growth) (Puguh, dkk., 2003).

Sediment is a substance that separates as a solid phase out of the solution. A

precipitate is formed if the solution becomes too saturated with the substance in
question. The solubility (S) of a precipitate by definition is the same as the molar
concentration of a saturated solution. Solubility depends on various conditions such as
temperature, pressure, concentration of other ingredients in the solution, and on the
composition of the solvent (Dina and Istikomah, 2009).

C. TOOLS AND MATERIALS

Tools :

In this experiments, several tools were used to support the practical implementation
including burette 50 mL, Erlenmeyer flask 7, digital balance, dropping pipette 6, beaker
glass 4, volumetric pipette 1, bol pipette 1, 2 petri dishes, spirtus+ gauze, Lucifer,
measuring glass 1, graduated pipette 1, volumetric flask 3, funnel 2.

Materials :

In this experiments several materials were used. Some of the materials that used are
chemical compounds that have different functions as a reagent. These compounds are,
CaO powder, dirty salt, Ba(OH)2 1 M solution, (NH4)2CO3 1 M solution, concentrated
HCl, Aquades, HNO3 0,1 M solution, AgNO3 0,1 N. Also used are supporting materials,
universal pH indicator paper, filter paper 4, plastic 5 and vaseline, .

D. WORK STEPS

Purification of NaCl

In this experiment, the first step is heated aquades 25 mL to boiling. After that, put 2.5 g
of dirty kitchen salt into hot water while stirring, then boil and filter. The filtrate from the
previous filter was added with CaO as much as 0.05 g, then the precipitate was filtered.
The next step is filtrate from the filtering plus Ba(OH) 2 1 M dropwise until the precipitate
is not formed again and filtered. Filtered filtrate added (NH 4)2CO3 0.1 M solution drop by
drop until the precipitate has not formed again. After that the solution is left for 5 minutes
so that the precipitate is formed clearly. The filtrate is then filtered and neutralized with
dilute HCl (tested with universal indicator paper). The final step, the solution is
evaporated to dry then weighed the obtained crystals and also impurities deposition.

Determination of purity levels of NaCl

Standardization AgNO3

The AgNO3 standardization process is carried out using NaCl pro anlyze. The first step
weighed 0.0625 grams of NaCl p.a. After that NaCl is dissolved using 25 mL of water.
NaCl solution was added with 5% K 2CrO4 as an indicator of titration. Then the solution is
titrated using AgNO3 solution twice (duplo). The AgNO3 volume obtained was used to
calculate the normality of AgNO3.

Determining the content of dirty salt

The first step weighed 0.6253 grams of dirty salt (before recrystallization) . After that
dirty salt is dissolved using 25 mL of water. NaCl solution was added with 5% K 2CrO4 as
an indicator of titration. Then the solution is titrated using AgNO 3 solution twice (duplo).
The AgNO3 volume obtained was used to calculate the content of dirty salt.

Determining the purity levels of NaCl after recrystallization

The first step weighed 0.0625 grams of purity salt (after recrystallization) . After that
purity salt is dissolved using 25 mL of water. NaCl solution was added with 5% K 2CrO4
as an indicator of titration. Then the solution is titrated using AgNO 3 solution twice
(duplo). The AgNO3 volume obtained was used to calculate the content of salt.

E. OBSERVATION DATA

a. Color of the salt before purified : turbid white

b. Structure of salt crystals before purified : large particle crystals
c. Color of the salt after purified : clean white
d. Structure of salt crystals after purified : small powder solids
e. Volume of Ba(OH)2 required is : 14 drops
f. Volume of (NH4)2CO3 required is : 17 drops
g. The weight of salt crystal from salt recrystallizing : 1,6234 grams
h. The percentage of pure salt from recrystallizing process :
weigh of pure NaCl
The percentage of pure salt = x 100%
weigh of dirty NaCl

1,6234
= x 100 %=64,936 %
2,5
i. Titration data :
1. Standardization AgNO3
Mass of concentated NaCl (p.a) : 0,5843 grams
Volume of distilled water : 10 mL

Volume AgNO3 that needed :

V = 8.1 mL
 gram 1000
NNaCl = x
Mr V

0.5843 1000
= x
58,5 10

= 0,1 N

VNaCl . NNaCl = VAgNO3 . N AgNO3

10 ml . 0,1 N = 8.1 ml . N AgNO3

N AgNO3 = 0,12 N

2. Determining the content of dirty salt

Mass of dirty salt : 0,25 grams

Volume AgNO3 that needed :

V = 2.8 mL

The purity levels of NaCl before recrystallization process :

(V . N ) AgNO 3 . 58,46
¿ ×100 %
w . 1000
2.8. 0,12 .58,5
¿ ×100 %
0,25 . 1000
¿ 7.86 %

3. Determining the purity levels of NaCl after recrystallization

Mass of NaCl after recrystallization : 0,25 grams

Volume AgNO3 that needed :

V = 7.4 ml

The purity levels of NaCl after recrystallization process :

(V . N ) AgNO 3 . 58,46
¿ ×100 %
w . 1000
7.4 . 0,12. 58,46
¿ × 100 %
0,25. 1000
¿ 20.76 %

F. DISCUSSION

NaCl is Sodium Chloride is the chemical name of table salt. Kitchen salt is a
chemical compound composed of 2 elements, metal sodium (Na) and chlorine gas (Cl).
When separated, the two substances have different properties. Sodium is a very reactive
metal. When reacting with water, will cause an explosion. So, Sodium must be stored in
special media, namely kerosene. While Chlorine gas is a green gas that is poisonous and
if inhaled can cause lung disorders. Both of these substances can indeed be detrimental if
it stands alone. However, if reacted to extreme temperatures and pressures, they make a
useful salt. This is caused by the influence of anions bound by Na in NaCl, causing the
nature of Na to disappear. In ionic solids such as crystals composed of ions there will be
attraction between cations and anions namely the Coulomb electrostatic force and the
repulsion of similar ions. The balance between these two things that is, attraction and
repulsion produces the crystal lattice energy. NaCl is one of the halide compounds which
shows that the distance between ions is the sum of the radius of positive ions and the
radius of negative ions, so this number is used to explain the structure of the ionic crystal
(Underwood and Day, 1996).

Recrystallization is the purification of a solid from its mixture / impurity by

recrystallizing the substance after it has been dissolved in a suitable solvent. The
principle of recrystallization is the difference in solubility between the substance to be
purified and the solubility of the mixing agent. The solutions that occur are separated
from each other, then the desired solution of the substance is crystallized by saturating it.
A crystal is a collection of small units called unit cells and ions are expressed as points.
One more significant difference from the crystalline NaCl compound with the ions that
make it up, namely the crystal NaCl radius < Na+ or Cl- ion radius. This is because in
the crystal, there is an interesting occurrence between the cation and the anion which
reduces the distance of the radius between the ions. So, the octahedral structure of NaCl
will overlap with the increasing number of Na and Cl atoms that combine to produce
NaCl crystals (Puguh, dkk., 2003).

In this experiment a way to purify sodium chloride from table salt by using
water as a solvent. NaCi is the main component to be purified because it contains
impurities derived from ions Ca2+, Mg2+, Al3+, SO42-, and Br-. So that the solubility
between NaCl and impurities is large enough, it is necessary to do certain substances.
These additives will form compounds, especially salts that are difficult to dissolve in
water, besides recrystallization can be done by adding a similar ion into the solution of
the substance to be separated.

The first treatment is to dissolve the kitchen salt in the form of a crystal solid
which is quite large and turbid white by using boiling water, the salt is put in boiling
water then stirred and awaited until the dissolved salt boils again. It is intended that the
salt decomposes completely.

Kitchen salt dissolved in hot distilled water will break down into its ions
namely, sodium ions (Na+) and chloride ions (Cl-). The decomposed salt is filtered and
the filtration is taken which will be used for the next process, which is the crystallization
process.

The filtrate we obtained was added 0.2 grams of calcium oxide (CaO).

2 NaCl (aq) + CaO (s) + H 2 O  CaCl 2  + 2 Na + + 2 OH –

The function of the addition of calcium oxide is to whiten the NaCl to be

recrystallized and precipitate impurities such as impurities which contain Ca2+, Fe3+,
and Mg2+ ions contained in table salt. . Calcium Carbonate can precipitate because Ksp
is smaller than the product of [Ca 2+ ] concentration [SO 4 2- ]. Ksp of CaCO 3 is 4.8 x 10 -
9 
and Ksp of CaSO 4 is 2.3 x 10 -4 . The reaction is:

CaO  Ca 2+ + O 2-

Ca 2+ + CO 3 2-  CaCO 3 
 Ca 2+ + SO 4 2-  CaSO 4 

Furthermore, the filtrate was added again with a solution of barium hydroxide
Ba (OH)2, the addition of Ba (OH)2 solution was carried out until the solution did not
form more deposits, in this experiment added a solution of Ba (OH)2 as much as 14
drops. The addition of this solution aims to remove deposits or prevent the formation of
more deposits, due to the addition of calcium oxide before. Sediment is a substance that
separates from one solid phase and comes out into the solution. A precipitate is formed if
the solution is too saturated with the substance in question. The solubility of a precipitate
is the molal concentration of a saturated solution. Solubility depends on the temperature,
pressure, concentration of other ingredients contained in the solution and the composition
of the solvent.

Ba (OH) 2  Ba 2+ + 2 OH -

The reaction between OH - with Fe 2+ and Mg 2+ :

Fe 2+ + 2 OH -  Fe (OH) 2   Ksp = 4.8 x 10 -16              

Mg 2+ + 2 OH -  Mg (OH) 2   Ksp = 3.4 x 10 -11

The overall reaction:

2NaCl (aq) + CaO (s) + Ba (OH) 2 (aq) + H 2 O  bacl 2  + Na + + 4OH - + Ca 2+

To the filtrate was also added with diamonium carbonate (NH4)2 CO3, this
addition was carried out to form a precipitate, in this experiment the addition of a solution
(NH4)2 CO3 as much as 17 drops. This addition aims to make the solution saturated and
bind impurities in the form of Ca2+, Mg2+, Al3+. To bind again the remaining impurities
that are SO42-, and Br-. The next step is to carry out a filter to separate the deposits
which are impurities present in the solution.

BaCl 2  + Na + + 4OH - + Ca 2+   + (NH 4 ) 2 CO 3  Baco 3  + NH 3  + Na 2 CO 3 +

CaCl 2 

Then the filtrate obtained (basic), neutralized with an acidic solution, HCl is dilute.

NaCl + Ba (OH) 2  + NH4Cl + HCl  BaCl2  + NaCl + NH3 + Cl2  + H2 O

The results of the filter filtrate were neutralized with HCl solution. Then it is
evaporated until dry so that NaCl crystals are obtained which are whiter than salt. NaCl
crystals that have been obtained are then weighed, and it is known that the weight of the
salt produced is 1.6234 grams. So that it can be seen the yield level of 64.938%. The salt
after purification is in the form of a small, pure white crystalline powder.

To determine the level of NaCl salt, the first step is to standardize the AgNO3
solution with concentrated NaCl. The resulting standardization is the normality of 0.12
N. AgNO3. Then further determine the level of purity of NaCl before recrystallization
with 0.2536 grams of dirty salt dissolved in 25 ml of distilled water and titrate with
AgNO3 with the K2CrO4 indicator. Titration is stopped until the color of the solution
turns brick red and produces a white precipitate. The average volume of AgNO3 in
titration is 2.8 ml. After the calculation the level of NaCl purity before recrystallization is
7.86%.
 The second is to determine the level of purity of NaCl after recrystallization in
the same way. The result is the average volume of AgNO3 in the titration is 7.4 ml with
the level of purity of NaCl after recrystallization is 20.76%.

In this experiment, the results obtained are in accordance with the theory, that
the level of purity of NaCl after recrystallization is greater than before recrystallization.
But also, in this experiment, the results were not good in the process of determining the
level of NaCl, ie the percentage of levels obtained was very small.

NaCl produced is a fine powder with a clean white color.

The reaction that occur is:

AgNO3+ NaCl  AgCl(s) + NaNO3

white precipitation
AgNO3 + K2CrO4  Ag2Cr2O4 + KNO3
red brick

The result of recrystallization is influenced by the solvent used by evaporation

adding impurities and recrystallization at the appropriate temperature. The solubility of
each substance is added and NaCl itself depends on the temperature, pressure,
concentration of other ingredients contained in the solution and the composition of the
solvent (Vogel, 1985). Besides that the pH of the solution can also affect, where the pH
of the solution must be in a neutral or weak base (pH = 6-8). This must be done because
if it takes place in an acidic atmosphere, the concentration of CrO42 ions will decrease.
Then if the titration is carried out in a strong alkaline atmosphere, peroxide deposits will
appear. In addition, the titration must also be done quickly and the shock must be carried
out strongly so that Ag+ is not oxidized to AgO which will make the end point of the
titration difficult to achieve.

During the mohr titration the solution must be stirred well because if not the
excess titrant will occur locally which causes the indicator to settle before the equivalent
point is reached and clogged by AgCl deposits that form so that the point eventually
becomes not sharp (Harjadi, 1993).

G. CONCLUSION AND SUGGESTION

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.NaCl purification is done by recrystallization method.
2. The purity levels of NaCl before recrystallization is 7.86% and the purity levels of
NaCl after recrystallization is 20.76%.

SUGGESTION
1. Should be doing titration duplo or triplo to get valid data.
2. The addition of impurity binder must be considered and adjusted precisely so that
there is no excess of binding agent which will add to the disrupting ions of the
recrystallization process.
3. When the evaporation of NaCl solution must be completely dry and has no water
content.
H. REFERENCES

Bahruddin, Z., dkk. 2003. “Penentuan Rasio Ca/Mg Optimum pada Proses Pemurnian
Garam Dapur”. Jurnal Natur Indonesia, 6(1): 16-19.

Dina, L. dan Istikomah.2009. Pemurnian NaCl dengan Menggunakan Natrium Karbonat.

Semarang: UNDIP.

Harjadi, W. 1993. Ilmu Kimia Analitik Dasar. Jakarta: Universitas Indonesia Press.
Keenan, Charles W. 1991. Kimia Untuk Universitas Jilid 1. Jakarta: Erlangga.
Paryanto, I. 2007. “Pengaruh Penambahan Garam Halus Pada Proses Kristalisasi Garam
Farmasetis”. Jurnal Sains dan Teknologi Indonesia, Vol.2 No.9, hal. 5-9.
Puguh, S., Wahyudi S., dan Heru S. I. 2003. ”Studi Eksperimental Pemurnian Garam
NaCl dengan Cara Rekristalisasi. Jurnal Teknik Kimia Universitas Surabaya, Vol.11
No.2.
Sugiyarto, Kristian H. 2003. Kimia Anorganik II. Yogyakarta: UNJ.
Syukri, S. 1991. Kimia Dasar. Bandung: Institut Teknologi Bandung.
Underwood, A.L dan Day R.A. 1996. Analisis Kimia Kuantitatif. Jakarta: Erlangga.
Vogel. 1985. Analisis Anorganik Kualitatif Makro dan Semimikro. Jakarta: PT. Kalman
Media Pustaka.
I. ATTACHMENT

Salt impurities. Salt yield after Weight of salt

recrystallization. recrystallization

Doing titration. Concentrated NaCl NaCl dirty salt

titration results. titration results.

Titration of NaCl
salts results from
recrystallization
ACC