Mei, 19th 2015

EXPERIMENT I
NaCl PURIFICATION
A. Objectives
1. Study the recrystallization method with the addition of impurity binder material
2. Understand the methods of NaCl Iodization
3. Calculate the purify levels of NaCl
B. Theoritical Basic
In chemistry technics solid must separate from solution or melted and dirty substance. It
can do by crystallization process. Crystall is solid with arrangement structure. Crystallization is
separation solid from solution. Sometimes need recrystallization too (Bernaseoni, 1995).
Precipitate is substance separate as solid phase, out from the solution. It form if solution
become saturated much. Solubility (S) like as molarity from saturated solution. Solubility
influence by temperature, pressure, consentration, and composition (Dina and Istikomah,
20009).
Sodium is soft white logam, melted T 97.5 0C. Sodium can oxidate fastly in humid air, it
must submerged in naphta or silene solvent. This metals reactive in water forming sodium
hydroxide and hydrogen gass. In the salt, sodium as monovalent cation Na +. This salt is
colorless (Vogel, 1979).
Recrystallization is a method used to purify sollids. Andrew and Rispoli (1991) states that
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 substane and impurities in
a particular solvent. Purification with recrystallization method widely applied in industrial
laboratories and aimed to improve the quality of a substance / material.
Supersaturated condition when solution consentration in upper of solubility. It can do with
evaporation, cooling, or mixture of them. There was two phenomena in crystallization procces
there are nucleation forming and crystals growth (Puguh, et al., 2003).
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 substance in certain solvents 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 crystals from the solution of supernatant (Anwar, 1994).
(Inorganic Chemistry Lecturer Team, 2015)
C. Equipment and Material
Equipment :
1. Digital balance
2. Gas stove
3. Burrete 25 ml
4. Erlenmeyer 25 ml
5. Dropping pipette
6. Watch glasses
7. Beaker
Materials :
1. Dirty salt
2. NaCl Pro analys

3. CaO powder
4. Solution of Ba(OH)2 1M

5. Solution of (NH4)2CO3 0.1M

6. Concentrated HCl
7. Aquabides

8. 1000 ppm of KIO3 solution

9. 0.1N AgNO3 solution
10. Universal pH indicator paper

11.
12.
D. Work Instruction
1. Purification of NaCl
13.
Heat 25 mL of
distilled water in
bekerglass up to boil

Allow the solution for

5 minutes, so we can
observe the
formation of
precipitate clearly.

Filter the solution

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

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

Evaporate the
solution up to dry.
Weigh the crystals
obtained.

Add 0.05 g of CaO

into solution, filter
the precipitate
happened

Add Ba(OH)2 1.0M

dropwise until the
last drop does not
form a precipitate.
Filter the precipitate
again.

14.
2. Determination of Purity Levels of NaCl
15.
250 mg samples of dirty salt
dissolved in 100 mL of distilled
water (100 ml volumetric flask),
then move into the erlenmeyer.

Do the deternination of
purity levels of NaCl
before and after
recrystallization process

Check the pH, if too much acid,

add a solution of NaHCO3 and
add HNO3 if too alkaline to be
neutral pH. For the argentometri
titration, take 10 ml of solution
& enter to erlenmeyer

Repeat the titration

two times

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- ion
produces a white precipitate

16.
E. Result of Observation
a. Color of the salt before purified
b. Structure of salt crystals before purified

: turbid white
: rought

c.
d.
e.
f.
g.
h.
i.

Color of the salt after purified

: white
Structure of salt crystals after purified
: smooth
Volume of Ba(OH)2 required is
: 3 mL
Volume of (NH4)2CO3 required is
: 4 mL
The weigh of impurities from salt recrystallizing : 2.5 gram
The weigh of salt crystal from salt recrystallizing : 1.4967 gram
The percentage of pure salt from recrystallization process
weigh of pure NaCl
17.
= weigh of dirty NaCl x 100%
18.

1.4967 gram
2.5000 gram

19.
= 58.78 %
j. Titration data
20. Standardization process
21.
V NaCl (mL) 22.
(mL)
23.
10
24.
25.
10
26.

27. V AgNO3
28.
29.
30.

x 100%

V AgNO3
4.4
4.1
:

4.25

Titration of dirty salt

V NaCl (mL) 31.
V AgNO3
(mL)
34.
10
35.
3.5
38.
10
39.
3.6

42. V AgNO3
: 3.55

32.
V
(mL)
36.
10
40.
10

43. V

Titration of purification
NaCl 33.
V AgNO3
(mL)
37.
3.6
41.
3.7
AgNO3

3.65

44.
k. The purity levels of NaCl before recrystallization process :
( V . N ) AgNO 3 x 58.46
volume of NaCl
45. Purity of NaCl =
x
volumeerlenmeyer x 100%
W x 1000
46.

3.55 x 58.46
0.25 x 1000

100
10

x 100%

47.
= 83.51%
l. The purity levels of NaCl after recrystallization process :
3.65 x 58.46
100
48. Purity of NaCl = 0.25 x 1000 x 10 x 100%
49.
= 85.86%
50.
F. Discusion
51. In this experiment practicant do NaCl purification and determine of purity levels of
NaCl. NaCl purification is to purify the salt from dirty substance, so we can know process of it
clearly. If the salt have purification, so the purity will increase. Practicant do purification,
recrystallization, and titration.
1. Purification of NaCl

52.
Dirty salt dissolve in hot aquadest. Aquadest at high temperature can dissolve
the salt more easily than low temperature. It become solution and we need filter it. Filtrate
used for next process of purification. Aquadest can separate little of dirty substance from
dirty salt. But that still much another substance.
53.
Then CaO solid added into solution, it can forms precipitate. So it filter again
between filtrate and precipitate. CaO bind the dirty substance like as CO 32- and SO42- in salt
solution, and it bind Mg or Fe ion. Binding between Ca2+ and that ions forms precipitate,
because solubility of the binding result is very little. Look at this reaction :
54.
CaO Ca2++ O255.
Ca2+(aq) + CO32-(aq)
CaCO3(s)
56.
Ca2+(aq) + SO42-(aq)
CaSO4(s)
22+
57.
O + Mg MgO
58.
O2- + Fe2+ FeO
59.
The filtrate used for next step, it is adding Ba(OH)2 solution. It can forms
precipitate. So it filter again between filtrate and precipitate. Ba(OH) 2 occurs ionization
become Ba2+ and OH- ion. That ions bind the dirty substance in salt solution. That ions and
the dirty substance forms precipitate, because solubility of the binding result is very little.
So it can separate between filtrate and precipitate to purify NaCl. Look at this reaction :
60.
Ba(OH)2(aq)

Ba2+(aq) + 2OH-(aq)
2+
61. Ba ion with dirty substance :
62.
Ba2+(aq) + CO32-(aq)
BaCO3(s)
Ba2+(aq) + SO42-(aq)
BaSO4(s)
63.
OH
ion
with
dirty
substance
:
64.
65.
Fe2+(aq) + 2OH-(aq)

Fe(OH)2(s)
66.
Mg2+(aq)+ 2OH-(aq)

Mg(OH)2(s)
67.
The filtrate used again for next step, it is adding (NH 4)2CO3 solution. The
(NH4)2CO3 solution dropwise until the last drop does not form a precipitate. After that
waiting for 5 minutes, and the precipitate can look clearly. CO 32- ion from ionization of
(NH4)2CO3 can bind the dirty substance in salt solution. That ions and the dirty substance
forms precipitate, because solubility of the binding result is very little. So it can separate
between filtrate and precipitate to purify NaCl. Look at this reaction :
68.
(NH4)2CO3(aq) 2NH4+(aq) + CO32-(aq)
69.
Ba2+(aq) + CO32-(aq)

BaCO3(s)
70.
Ca2+(aq) + CO32-(aq)

CaCO3(s)
71.
The binding of dirty substance are CaO, Ba(OH)2, and (NH4)2CO3. We can
know that CaO is oxide of calsium, Ba(OH) 2 is strong base, and (NH 4)2CO3 is salt. So
Ba(OH)2 give big influence to pH of solution, the solution of salt become not neutral. Based
on experiment it check used universal indicator, and it suitable with theory the pH is base. It
neutralization used HCl dillute. We drops HCl dillute in solution carefully until the pH of
solution become neutral.
72.
The salt evaporated until the liquids lost to forming crystals. So we get solid
salt in this experiment. Then the crystal weighed and we can know the rendement of salt.
Based on experiment, the crystals of pure salt is 1.4697 gram and the rendement is 58.78%.
2. Determination of Purity Levels of NaCl
73.
This sub-experiment was three activity, there are standardization of AgNO 3
solution, determination of NaCl purity levels in beginning and NaCl purity levels after
purification. Determination thats by titration.
74.
At first time, there are standardization of AgNO3. AgNO3 solution as titrant
and NaCl Pa as titrate in erlenmeyer. The solution of NaCl Pa checked the pH, then

neutralization if more acid use NaHCO3 solution. After standardization we can know that
normalization of AgNO3 used is 0.1006N.
75.
Second, determination of NaCl purity levels of dirty salt at first time. 0,25
gram dirty salt dissolve in 100 mL aquadest. We must check the pH of NaCl solution use
indicator universal. If it more acid, we must add NaHCO 3 solution until the pH neutral.
NaHCO3 is salt from strong base and weak acid, so it can make pH increase. Then 10 mL
from that solution as titrate, AgNO 3 solution as titrant, and indicator for this titration is
K2CrO4. Titration do until the color of solution in erlenmeyer become red brick. From
experiment titration need 3.55 mL AgNO3 in titration end point. The data of that volume use
for calculated the purity levels of dirty salt, it is 83.51%.
76.
Third, determination of NaCl degree in after purification used pure salt. 0.25
gram pure salt dissolve in 100 mL aquadest. We must check the pH of NaCl solution use
indicator universal. If it more acid, we must add NaHCO 3 solution until the pH neutral.
NaHCO3 is salt from strong base and weak acid, so it can make pH increase. Then 10 mL
from that solution as titrate, AgNO 3 solution as titrant, and indicator for this titration is
K2CrO4. Titration do until the color of solution in erlenmeyer become red brick. From
experiment titration need 3.65 mL AgNO3 in titration end point. The data of that volume use
for calculated the purity levels of pure salt, it is 85.86%.
77. Based on experiment, the purity levels of pure NaCl more higher than dirty NaCl. It
is suitable with theory, if we do purification of salt, so it will increase the purity levels. The
structure and color of pure salt more soft and white than the structure and color of dirty salt.
This is reaction occurs when titration :
78. AgNO3(aq) + NaCl(aq)
AgCl(s)+ NaNO3(aq)
79. AgNO3(aq) + K2CrO4(aq)
Ag2Cr2O4(s) + KNO3(aq)
80.
(red brick)
81.
G. Conclusion
1. Dirty salt contain some substance like as Mg, Fe, CO 32-, SO42- and other. That can be lost
used CaO, Ba(OH)2, and (NH4)2CO3 to become pure salt.
2. Based on experiment, rendement of NaCl is 58,78%. We also get result the purity levels of
NaCl before recrystallization process 83.51% and the purity levels of NaCl before
recrystallization process 85.86%. So the purity increase until 2.35%.
3. Pure salt have purity levels more higher than dirty salt. It also has structure and color more
soft and white than dirty salt.
82.
H. Suggestion
1. Before experiment,we must understand objectives, theory, and procedure experiment.
2. Practitioner more elaborate in read scale from apparatus.
3. Practitioner carefully in this experiment, so that not happen accident.
4. We need good team work.
5. All of apparatus must in good condition
6. After use apparatus,it must cleaned. So the chemistry substance is not contaminated.
83.
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90.

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100.
I. Refference
101. Bernaseoni, G. 1995. Teknologi Kimia. Jakarta : PT.Padya Pranita.
102. Inorganic Chemistry Lecturer Team. 2015. Manual Work of Inorganic Chemistry
Practicum. Semarang : UNNES.
103. Lesdantina, Dina & Istikomah. 2009. Pemurnian Nacl Dengan Menggunakan Natrium
Karbonat. Seminar Tugas Akhir S1 Teknik Kimia UNDIP.Semarang : UNDIP.
104. Setyopratomo, Puguh, Wahyudi Siswanto, dan Heru Sugiyanto Ilham. Studi
Eksperimental Pemurnian Garam NaCl dengan Cara Rekristalisasi. Surabaya :
Universitas Surabaya Jurusan Teknik Kimia.
105. Vogel, 1979. Analisis Anorganik Kualitatif Makro dan Semimikro. Jakarta : PT. Kalman
Media Pustaka.
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146.

Documentation

147.

148.

Standardization of AgNO3 Titration of dirty salt

Titration of pure salt

149.

150.

151.Neutralization

Solution of salt evaporated

Crystals of pure salt