EXPERIMENT I

NaCl PURIFICATION
April, 8th 2016
A. Objectives
1. Student can study the recrystallization method with the addion of impurity binder material
2. Student can understand the methods of NaCl ionisation
3. Student can calculate the purity levels of NaCl
B. Literature Review
Sodium is a soft silver-white metal, which melt at 97.5 oC. Natrium oxidizes rapidly in moist
air, it should be kept immersed in the solvent naphtha or xylene. The metal reacts violently with
water, forming sodium hydroxide and hydrogen. In the salts of sodium is present as monovalent
cations Na+. These salts to form a colorless solution, almost all of the sodium salt is soluble in
water. Most chloride dissolves in water, mercury (I) chloride, HgCl2, silver chloride, AgCl, timbale
chloride, PbCl2 (which it dissolves very slightly in cold water, but soluble in boiling water), copper
(I) chloride, CuCl, bismuth oxychloride, BiOCl, antimony oxychloride, SbOCl, and mercury (II)
oxychloride, HgOCl2, insoluble in water (Vogel, 1979).
Crystallization is a method for purifying a substance with a solvent followed by precipitation.
In the crystallization of organic compounds is affected by the solvent. Solvent-solvent
crystallization is carried by solute form a solid and hung in the crystal structure - crystal solutes
(Oxtoby, 2001).
Recrystallization is one way of purifying solids plural is used, in which these substances are
dissolved in a solvent and then crystallized back in. This method relies on the solubility of
substances in certain solvents at temperatures when enlarged. Because of the concentration of
total impuriti usually smaller than the concentration of the purified, if cold, then impuriti low
concentrations but in the solution while the product of high concentration will precipitate
(Arsyad, 2001).
Recrystallization events associated with the precipitation reaction. The precipitate is a
substance that separates from the solid phase and out into the solution. The precipitate formed
when the solution is overly saturated with substance concerned. The solubility of a precipitate is
the molar concentration of the saturated solution. Solubility depends on temperature, pressure,
concentration of other substances contained in the solution and the composition of the solvent
(Svehla, 1985).
Effect of Temperature Decrease in Process of Crystals:
a. When decrease the temperature goes fast growing speed of crystal nucleus faster
than the speed of crystal growth so that crystals obtained by a small, fragile, and
more.
b. When the temperature is done slowly decline, the speed of crystal growth is faster
than the growth rate of crystal nucleus so that the crystals are freed big, tough, and
elastic (Austin, 1986).
The solution crystallized is a compound mixture of solvent and solute. Once heated, the
solvent evaporated and left behind only a crystal. This method is used when the temperature
reduction is not so affect the solubility of the solvent. Evaporation aims to eliminate or
minimalize solvent or residual solvent contained in the filtrate. Crystals are solids that have flat
surfaces. Because many solid substances such as salt, quartz, and snow there in forms that
clearly symmetrical, scientists have long suspected that atoms, ions or molecules of solid
substance is also arranged symmetrically (Keenan, 1999). The crystal structure determined by
the size of the force between atoms and atoms contained in the crystal. To simplify matters, we
can assume ion or atom as a solid sphere of radius r. No structure is hexagonal close packing.

How the preparation in the crystal ball can not be as simple as the metal crystal, because the
ionic crystal consisting of charged ions and have a different kind (Bird, 1987).
To reduce impuristis in salt can be done with a combination of the washing process and
rapid dissolution during the making garam.Sedangkan removal of impurities from salt product
can be made by 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 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).
C. Equipment and material
Equipment:
1. Digital balance
2. Gas Stove
3. Oven
4. Burette 25 ml
5. 3 pieces erlenmeyer 25 ml
6. 2 pieces dropping pipette
7. Watch glasses
8. Beaker
Materials:
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.

Dirty Salt
CaO powder
Solution of Ba(OH)2 1M
Solution of (NH4)2CO3 of 0,1 M
Concentrated HCl
Aquabides
1000 ppm of KIO3 solution
A solution of 0,1 M HNO3
0,1 N AgNO3 solution
Universal pH indicator paper

D. Method
1. Purification of NaCl

Heat 25 mL of
distilled water in
bekerglass up to boil

Add 2,5gr dirty salt to

hot water, stir and
continu heated until
all salt dissolve and
then filter it.

Add 0,05 gr CaO and

filter the precipitate
happened

Wait 5 minutes and

observe the
formation of
precipitate

Add 5 ml (NH44)22CO33
0,1M dropwise until
not form precipitate

Add Ba(OH)22 1M
dropwise until not
form precipitate and
filter the precipitate
again

Filter and neutralize

the filtrate with dilute
HCl (tested with
universal indicator
paper)

Evaporate until dry

and weigh the
crystals

Dry and weight the

impurities precipitate
obtained from
filtration

2. Detemination of Purity Levels of NaCl

250 mg dirty salt

dissolved in 100ml (mixed in volumetric flask)

move into erlenmeyer
Check the pH, if acid (add NaHCO3 ) if alkaline HNO3)

take 10 ml move into erlenmeyer

Add 1 ml indicator K2CrO4 5%

Titrate the solution with 0,1N AgNO3

until the solution color is red brick and white precipitate
from (silver ion will be react with Cl- (repeat 2 times)
Determine of purity levels of NaCl before
and ater recrystallization process
E. Observation data
1. Color of the salt before purified: white turbid
2. Structure of salt crystals before purified: form large or coarse
3. Color of the salt after purified: pure white, soft and fluffy
4. Structure of salt crystal after purified: soft and more fulffy

5.
6.
7.
8.
9.

Volume of Ba(OH)2 required is: 4 mL

Volume of (NH4)2CO3 required is: 5 mL
The weigh of impurities from salt crystallizing: 0.1958 gram
The weigh of salt crystal from salt crystallizing: 1.4573 gram
The percentage of pure salt from recrystallization process:
%

Weight of pure NaCl

Weight of dirty NaCl

1.4573
2.5062

x 100%

x 100%

= 58.1478 %
10. Titration data
a. Standaritation of AgNO3
Mass of concentrated NaCl = 0.2540 gram
Volume of distilled water = 100 mL
Volume AgNO3 that needed
V1 = 4.3 mL
V2 = 4.3 mL
Vrata-rata = 4.3 mL

N NaCl=

massa 1000
x
Mr
V

0.2540 1000
x
58.48
100

0.0434 N
V NaCl . N NaCl=V Ag NO 3 . NAg NO3
NAg NO 3=10 mL x 0.0434 N : 4.3 mL
NAg NO 3=0.1009 N
11. The purity levels of NaCl before recrystallization process:
V

Ag NO 3

V1 = 3.6 mL
V2 = 3.7 mL
Vrata-rata = 3.65 mL
The purity levels of NaCl =

=
In 100 mL solution

( V . N ) Ag NO3 . Mr NaCl
x 100
w .1000
( 3.65 x 0.1009 ) 58.46
x 100
0.2504 .1000

= 8.59822 % ( in 10 mL solution)
= 8.59822 % x 10

= 85.9822 %
12. The purity levels of NaCl after recrystallization
V

Ag NO 3

V1 = 4.00 mL
V2 = 4.00 mL
Vrata-rata = 4.00 mL
The purity levels of NaCl =

( V . N ) Ag NO3 . Mr NaCl
x 100
w .1000
=

In 100 mL solution

( 4.00 x 0.1009 ) 58.46

x 100
0.2504 . 1000

= 9.4227 %
( in 10 mL solution)
= 9.4227 %x 10
= 94.227 %

Reaction of purification of NaCl

CaO Ca2+ + O2Ca2+ + CO32- CaCO3
Ca2+ + SO42- CaSO4
Added Ba(OH)2
Ba(OH)2 Ba2+ + OHBa2+ + SO42- BaSO4
Reaction between OH- with Fe2+ and Mg2+
Fe2+ + 2OH- Fe(OH)2
Mg2+ + 2OH- Mg(OH)2
Adding (NH4)2CO3
Reaction : (NH4)2CO3 2NH4+ + CO32Ba2+ + CO32- BaCO3
Ca2+ + CO32- CaCO3
The reaction that occur
NH4+ + HCl NH4Cl (neutralization)
AgNO3 + NaCl AgCl + NaNO3 (white precipitate)
AgNO3 + K2CrO4 Ag2CrO4 + KNO3 (red brick)

F. Discussion
This experiments aims to study the recrystallization NaCl with the addition of impurities and
calculate the rate of NaCl. In this experiment doing titration to standarization AgNO 3. The
titration between NaCl pro analys with AgNO 3. After the standarization the normality of AgNO 3 is
0.1009 N. The tiitration well done for dirty NaCl to determine the ratio of the purity levels of NaCl
before recrystallization and after recrystallization. The purity levels of NaCl before
recrystallization is 85.9822%.
In the purification of NaCl required experiment dirty salt which will be in the recrystallization
to obtain pure salt without impurities. Previously, heating water to boil and then put salt dirty.
NaCl is soluble in water because NaCl is polar and ionic, in which ionic compounds will take the
form of ions the ion in solution. The filtrate from filtration was added CaO which aims to increase
the solubility difference between NaCl and impurities, which CaO will attract ions Cl -, causing a
white precipitate CaCl2. the reaction is:
2 NaCl(aq) + CaO(s) + H2O CaCl2 + 2 Na+ + 2 OHCa2+ ions react with substances impurities such as Ca 2+, Fe3+ and Mg 2+, because Ca2 + is
able to bind carbonates or sulfates. Calcium carbonate can precipitate due to its Ksp smaller
than the product of the concentration of [Ca 2+] [SO42-]. CaSO4 can also settle for Ksp is smaller
than the product of the concentration of [Ca2+] [SO42-]. Ksp of CaCO3 is 4.8 x 10-9 and Ksp
CaSO4 was 2.3 x 10-4. the reaction is:
CaO Ca2+ + O2Ca2+ + CO32- CaCO3
Ca2+ + SO42- CaSO4
The filtrate from the filter is then added Ba (OH) 2 dropwise until no more precipitate formed,
addition of Ba (OH)2 until no precipitates is 4 ml. Addition of Ba (OH)2 aims to separate Cl- ions
of CaCl2. Ba (OH)2 will also break down into Ba 2+ and OH-, OH- serves bind impurities such as
Fe2+ and Mg2+ remaining and prove that the Cl - ions contained in the solution has been to bind
all the resulting precipitate Ba2 + BaCl2. the reaction is:
Ba(OH)2 Ba2+ + 2 OHReaction between OH- with Fe2+ and Mg2+ :
Fe2+ + 2 OH- Fe(OH)2

Ksp = 4,8 x 10 -16

Mg2+ + 2 OH- Mg(OH)2

Ksp = 3,4 x 10 -11

All of reaction :
2NaCl (aq) + CaO (s) + Ba(OH)2 (aq) + H2O BaCl2 + Na+ + 4OH- + Ca2+
The filtrate is then added (NH4)2CO3 dropwise until no more precipitate formed, addition of
(NH4)2CO3 until no precipitates is 5 ml. Addition of (NH 4)2CO3 aims to separate Ba2+ ions and
Ca2+ ions contained in the solution in excess so obtained white precipitate again. the reaction is:

Ba2+ + CO32- BaCO3

Ksp = 8,1 x 10 -9

Ca2+ + CO32- CaCO3

Ksp = 4,8 x 10 -9

All of reaction:
BaCl2 + Na+ + 4OH- + Ca2+ + (NH4)2CO3 BaCO3 + NH3 + Na2CO3 + CaCl2
After settling a few minutes and filtered to separate precipitate the impurites in that solution.
after filtrate obtained the characteristics is base because consist of NH4+ ion from (NH4)2CO3, so
neutralized with acidic solutions is HCl solution. The function was neutralized for the formation of
salt, because salt is neutral. After neutralize then evaporated, which aims to evaporate solvent and
ions are volatile so obtained pure salt. in this experiment result recrystallized salt 1.4573 g with a
yield of 58.1478 %. The weigh salt after purification is smaller than before purification ie 2.5062 g,
because the impurities are gone. The reaction of neutralization:
NH4+ + HCl NH4Cl (neutralization)
After obtained pure salt, titration well done with AgNo 3 solution and used K2CrO4 as indicator .
The purity levels of NaCl after recrystallization is 94.227 %. color salt after recrystallization whiter
and cleaner. It can be seen that the percentage of salt after purification is higher because the
impurities have been removed during the purification process. The reaction in titration:
AgNO3 + NaCl AgCl + NaNO3 (white precipitate)
AgNO3 + K2CrO4 Ag2CrO4 + KNO3 (red brick)
G. Conclusion
The principle of purification and crystallization of NaCl with recrystallization method is to
separate the NaCl from impurity substances based on differences in solubility both in certain
solvents such as CaO, Ba(OH)2 and (NH4)2CO3. Impurity substances which have been tied up in
a suitable solvent and precipitated with NaCl so that it can be separated by filtration. From these
experiments the yield obtained at 58.1478%. The percentage of salt after purification is higher
because the impurities have been removed during the purification process. The purity levels of
NaCl before recrystallization is 85.9822%. The purity levels of NaCl after recrystallization is
94.227%.
H. Suggestion
1. Be carefully when drop some solution.
2. Be carefully doing titration because used AgNO3 solution and other solution.
3. Be carefully when doing recrystallization NaCl
4. References
Arsyad, M. Natsir. 2001. Kamus Kimia Arti dan Penjelasan Istilah. Jakarta: Gramedia
Austin, G.T, 1996, Industri Proses Kimia, Edisi Kelima. Penerbit Erlangga, Jakarta, Hal 308
Keenan, C.W. 1999. Kimia untuk Universitas Jilid 2. Erlangga. Jakarta.
Oxtoby, D.W. 2001. Kimia Modern. Erlangga. Jakarta.
Svehla,G., (1985), Analisis Anorganik Kualitatif Makro dan Semimakro, Edisi kelima, Bagian I.
Kalman Media Pusaka, Jakarta.
Vogel, 1979, Analisis Anorganik Kualitatif Makro dan Semimikro, PT. Kalman Media Pustaka,
Jakarta.