EXPERIMENT 1

NaCl PURIFICATION AND IODIZATION

18th March 2016

A. OBJECTIVES
1. Study the recrystallization method with the addition of impurity binder material
2. Understand the methods of NaCl iodisation
3. Calculate the purity levels of NaCl

B. BASIC THEORY
Indonesia is the one of the nations who has many natural resource like mineral, salt and
oil. But all of those resource is haven’t yet used optimally because Indonesia still need the
product of import from abroad. For example is salt, salt is the one of the needs that include in
complementer substance in food production and the source of electrolyte for the body.
Production of salt is the national problem for Indonesia, Indonesia as an archipelago country
should has high potential for results the salt from sea. But in fact, for fulfill the national needs
Indonesia must importing the salt. Salt production is low is caused by high intetity of the rain
so that can influence yhe process of production. And the quality of the salt is not good
enough because the content of minerale is low. (Rukmana dan Jumaeri, 2015).

Salt that we know commonly is a chemical compound that the biggest part is NaCl with
the impurities consist of CaSO4, MgSO4, etc. (Sutrisnanto, 2001).
If the sea water is evaporated then will become the salt crystalls and called salt of krosok.
Then the salt that resulted from evaporation of sea water that not yet be purified is contained
impurities substances like Ca2+ , Mg2+, Al3+, Fe3+ , SO42- , I-, Br- (Anonim, 1989).
To increase the quality of salt can through the way of crystallization, recrystallization and
laundering the salt. The other way to increase the quality of salt is by purification by adding
impurities binder substance. Without purification process, then the salt that resulted from the
evaporation sea water is still containing another compound such as MgCl2, MgSO4, CaSO4,
CaCO3 dan KBr , KCl dalam jumlah kecil (Jumaeri, 2003).

Common salt (NaCl) is a material in the form of a white crystalline solid, having the
form of a cube crystalline transparent and is a compound that which is constituted of a strong
acid HCl and strong bases NaOH. If this element direaksikan , it will be formed NaCl dan H2O
which if combined it will be forming a solution of salt. Nevertheless, a saline solution is that it
represents a solution of salt that there are still pengetor. Although the nature of the solution is
that it represents a solution homogeneous, to remove salt from pollutter it can be done with
the process of a recrystallization .
A recrystallization is a method used to purify the solids. This method with the
principle of the difference between substances of soluble resources are purified by a
particular solvent pollutter in a heated back and then evaporated . Pollutter material which
cannot be dissolved , can be separated from a solution by means of filtering, while the
material which dissolves easily pengotor will stay in solution. Purification by a method of a
recrystallization much done in a laboratory or industry to improve the quality of a substance or
material.
Events associated with the reaction of the deposition of a recrystallization. The
sediment is a substance splitting from one phase of the solution get out into a solid and. The
sediment formed if a solution is too saturated with a substance concerned. The solubility of a
precipitate molal saturated is the concentration of solution. The solubility of depends on
temperature, pressure , the concentration of other material contained in solution and
composition solvent.
 Declaring that a recrystallization is one way of purification solid substance used in
the plural which any substance is dissolved in some solvent and crytalline back. (Syabatini:
2008 ).
Crystallization is a method for purification of a substance by the deposition of
solvents and continued. Influenced by crystallization of a compound in organic solvents.
Diluent crystallization is the solvent carried by a solute forming a solid and it depends on the
structure of crystals solutes. ( Oxtoby, 2001 )
In doing a method of a recrystallization, required the terms of a solvent that can be
extrapolated to the process of a recrystallization are:
1. Give power differences soluble large enough between substances that are purified with a
substance pollutter.
2. Leaving no substance pollutter in crystals.
3. Readily separated of crystal.
4. Is inert ( not readily reacting with crystal ) by the presence of a solvent a fastener pollutter
was intended can be used to bind foreign substances whose existence undesired in
substances pure.

A recrystallization steps were:

1. Dissolving a substance in a solvent.

2. Filtration gravity do.
3. Take crystalline substance dissolved.
4. Collecting crystals with vacum filtration.
5. Crystalline dry ( Fessenden , 1983 )

C. EQUIPMENT AND MATERIALS

 Equipment:
1. Erlenmeyer 25ml
2. Dropping pipette
3. Ball pipette and pipette volume
4. Dropping plate
5. Beaker glass
6. Watch glass
7. Measuring glass
8. Evaporating dish and Spiritus
9. Burette, stative and clamp
10. Spatula
11. Digital balance

 Materials:
1. HCl 1,5M
2. HNO3 p.a
3. AgNO3 0,1 N
4. CaO powder
5. Dirty salt and NaCl p.a
6. Ba(OH)2 1M
7. (NH4)2CO3 0.1 M
8. K2CrO4
9. NaHCO3
10. Aquadest
D. WORK STEPS

1. Purification Of NaCl

Put 2,5 g of dirty salt in stired and heated again Added 0,05 g CaO to the
the beaker glass contained until dissolved, filtered it filtrate and filtered the
25 mL of hot distilled precipitate
water

Allowed the solution for Added 5 mL of Added Ba(OH)2 solution

5 minutes and filtered (NH4)2CO3 0,1M 0,1, then filtered the
the solution dropwise to the filtrate precipitate again

Checked pH and Evaporated the solution Weighed the crystal

Neutralized with dilute up to dry n we got the Dried and weighed the
HCl NaCl crystal impurities precipitate
obtained from the filtration

2. Determination of Purity Levels of NaCl

0,2518 g of NaCl p.a

- Dissolved in 100 ml of distilles water (100 ml

of volumetric flask)
- Moved into the erlenmayer
- Checked the pH
10 ml of solution

Added 3 drops of indicator

K2CrO4 5%

Titrated the solution with 0,1 N

AgNO3 solution until the solution
color is red brick. Repeat twice

Doing the determination of

purity levels og NaCl before
anf after recrystallization
process
E. OBSERVATION
Result of Observation
a. Color of the salt before purified : white muddy
b. Structure of salt crystals before purified : coarse grain
c. Color of the salt after purified : pure white
d. Structure of salt crystals after purified : powder
e. Volume of Ba(OH)2 required is : 3 mL
f. Volume of (NH4)2CO3 required is : 5 mL
g. The weigh of impurities from salt recrystallizing : 0,0862 grams
h. The weigh of salt crystal from salt recrystallizing ; 1,6292 grams
i. The percentage of pure salt from recrystallizing process : 64,88%
j. The purity levels of NaCl before recrystallizing process : 83,90%
k. The purity levels of NaCl after recrystallizing process : 87,31%

F. ANALYSIS DATA

The percentage of pure salt from recrystallizing process:

weigh of pure salt crystal
% 𝑅𝑒𝑛𝑑𝑒𝑚𝑒𝑛 = × 100%
weigh of impurities from salt
1,6269
= × 100%
2,5073
= 64,88%

Titration data:

 M NaCL pa = 0,2518 grams

V solvent = 100 ml
0,2518 𝑥 1000 𝑥 1
N =
58,5𝑥 100

= 0,0430 N

 Standarisation
V1 x N1 = V2 x N2
10 x 0,0430 = 4,48 x N2
N2 = 0,0960 N

The purity levels of NaCl before recrystallizing process:

(𝑉.𝑁)𝐴𝑔𝑁𝑂3 𝑥 58,5
%NaCl = x 100%
𝑊 𝑁𝑎𝐶𝑙 𝑡𝑖𝑡𝑟𝑎𝑡𝑒𝑑 𝑥 1000

(3,79 𝑥 0,0960) 𝑥 58,5

= x 100%
0,02537 𝑔 𝑥 1000

= 83,90 %
 The purity levels of NaCl after recrystallizing process:

(𝑉.𝑁)𝐴𝑔𝑁𝑂3 𝑥 58,46
%NaCl = x 100%
𝑊𝑁𝑎𝐶𝑙 𝑡𝑖𝑡𝑟𝑎𝑡𝑒𝑑 𝑥 1000

(3,89 𝑥 0,0960) 𝑥 58,5

= x 100%
0,02502 𝑔 𝑥 1000

= 87,31 %

The reaction occurs in the purification NaCl and iodisation :

1. Reaction NaCl with CaO
CaO (s) Ca2+ + O2-
2+ 2-
Ca (aq) + CO3 (aq) CaCO3(s)
2+ 2-
Ca (aq) + SO4 (aq) CaSO4(s)

2. Reaction the addition of Ba(OH)2

Ba(OH)2 (aq) Ba2+(aq) + 2OH-(aq)
Fe2+(aq) + 2OH-(aq) Fe(OH)2(s)
Mg2+(aq) + 2OH-(aq) Mg(OH)2(s)

3. Reaction the addition of (NH4)2CO3

(NH4)2CO3(aq) 2NH4+(aq) + CO32-(aq)
Ba2+(aq) + CO32-(aq) BaCO3(s)
Ca2+(aq) + CO32-(aq) CaCO3(s)

4. Reaction the addition HCl

NH4+(aq) + HCl (aq) NH4Cl (neutral)

A reaction which occurs on the determination of NaCl ( levels titration AgNO3 ) namely:
1. AgNO3+ NaCl AgCl(s)+ NaNO3 (white)
2. AgNO3 + K2CrO4 Ag2Cr2O4 + KNO3 (red brick)

G. DISCUSSION
The first experiment we did is purification of NaCl and iodization. The main material we
used to be purified is salt krosok. In the purification of krosok salt experiment, we applied the
recrystallization proses to get the pure NaCl, recrystallization is the purification of a substance
from the mixture or the impurities by recrystalling its substance after its solved in the correct
solvent. The principle of recrystallization is the difference of the solubility between the
substance that will be purified and the solubility of the impurities substance. The solution that
will be crystalled is should be in saturated condition. The one of the real differences of the
NaCl in crystall form and the ions that arrange it, is the radius of NaCl crystall is bigger than
radius of Na+ and CL- ion. The salt krosok we used was still many pollutter. NaCl separation
of pollutter started by dissolving of salt krosok in aquades in heat condition. It because the
heat of aquadest can make krosok salt solved perfectly. Then the solution is filtered and we
used the filtrate to the next steps.
Therefore, the main goal of this experiment is to separate the salt of krosok from its pollutter.
The pollutter in the salt of krosok is can be like CO32- , SO42- , Fe2+ and Mg2+ ions. In the
steps of purification, we added the CaO powder and Ba(OH)2 solutions, the purpose of
adding CaO powder and Ba(OH)2 solutions is to carried away the pollutter in the salt krosok
by form the precipitation. Then ions of Ba2+ and Ca2+ will bond the pullutter ions like CO32- and
SO42- ions and reacted become CaCO3(s) and CaSO4(s) as the reaction;
 Ca2+ (aq) + CO32-(aq) CaCO3(s)
Ca2+(aq) + SO42-(aq) CaSO4(s)

Ba2+ (aq) + CO32-(aq) BaCO3(s)

Ba2+(aq) + SO42-(aq) BaSO4(s)

Ion Ca2+ reacted with substances of Ca2+ pollutter because the nature of carbonate ions
capable of binding or sulphate . Calcium carbonate can settles for smaller than the ksp of its
concentration [Ca2+] [SO42-] times. Ksp CaSO4 can also settles for smaller than the results of
times the concentration of [Ca2+][SO42-]. Ksp of CaCO3 is 4.8 x 10-9 and Ksp from CaSO4 is
2.3 x 10-4.
Solution is then filtered by paper strain. Then added drops filtrat produced for the drops
with solution Ba(OH)2 dilute not to precipitate formed again. Ba(OH)2 will be decomposized
of being Ba2+ and OH- , OH- it serves bind polutter Fe2+ and Mg2+ of the remaining.
The reaction was:
Ba(OH)2  Ba2+ + 2OH-
Fe2+ + 2OH-  Fe(OH)2(s)
Mg2+ + 2OH-  Mg(OH)2(s )

The next step is we added the (NH4)2CO3(aq) solution, the purpose of added this solution into
NaCl solution is to make NaCl become saturated and (NH4)2CO3(aq) solution can carried the
Ba2+ and Ca2+ ions [ammonium carbonate bond the ions that carried away the impurities
substance] and bound with both ions as the reaction;
(NH4)2CO3(aq) 2NH4+(aq) + CO32-(aq)
Ba2+(aq) + CO32-(aq) BaCO3(s)
2+ 2-
Ca (aq) + CO3 (aq) CaCO3(s)

Pollutter in crystal consisting of two categories is pollutter who are on the surface of crystals
and pollutter in the crystals. Pollutter who are on the surface of crystalline derived from
solution of the parent being carried away on the surface of crystals at the time the process of
separation of solids from solution of its parent. Pollutter crystalline on the surface this can be
separated only by laundering. A liquid used for washing should be having the nature that can
dissolve pollutter but could not crystal solids dissolve. One of a liquid that meet the nature of
this is a saturated solution of crystalline substance to be washed, but can also used a solvent
generally meet these criteria. The pollutter located in crystal which cannot be eliminated by
means of laundering. One way not to eliminate pollutter existing in a way, is a
recrystallization namely by dissolving the crystalline back later or recrystallizing. Any excess
the process of separating a recrystallization this compared with others that pollutter only be
borne in crystals in a fine if it is orientated by a crystal lattice.
To salt filtrate krosok already strained, it allegedly contains pollutter substance that can
dissolve in aquadest. Pollutter is needed to separate a certain substances that would
establish a particularly tricky salt that is soluble in water.

After we did the experiment, the next step is we should determine the levels of dirty salt
and pure salt or salt that had been separated from the polllutter substances that done by a
recrystallization. On experiments we used AgNO3 solution to be standaritated by NaCl p.a
solution and got the result 0,0960 N. In the process of titrating argentometry there will formed
AgCl precipitate that has white color, and AgNO3 would react with the indicator solution of
K2CrO4 to form the mixture of Ag2CrO4 in red brick color. After the process of titrating, we got
the results of the dirty salt content for krosok is 83,90 %. And for pure salt content of the
results by recrystallization process, is 87,31 %.
Based the theory of purification of NaCl, the results of the concentration of NaCl after
recrystallized must bigger than the concentration of NaCl before recrystallized. And in our
experiment, all the steps that we’re doing got the result of that the concentration of NaCl
 after recrystallized is bigger than the concentration of NaCl before recrystallized, it means
our result of this experiment is proper with the theory.

H. CONCLUSION
 Dirty salt pollutter is still in the salt krosok solution. Pollutter that included in the solution
are Ca2+, Mg2+, Al3+, Fe3+, SO42-. To purify this solution, the impurities should be carried by
some substances. They are carrried away by the CaO powder and Ba(OH)2 solution and
the existance of (NH4)2CO3(aq) makes salt solution is saturated so we can get the pure salt.
 Recrystallization is the purification of a substance from the mixture or the impurities by
recrystalling its substance after its solved in the correct solvent. The principle of
recrystallization is the difference of the solubility between the substance that will be
purified and the solubility of the impurities substance.
 The purity levels of NaCl before recrystallization is 83,90 % and the purity levels of NaCl
after recrystallization is 87,31 %

I. SUGGESTION
 Practician need to know who will practiced elementary lab work.
 Practician in a group should work same time and each other.
 Every practician should ensure that materials in accordance with a substance needed
especially normality.

J. REFERENCE
Fessenden. 1983. “Kimia Organik”. Jakarta : Erlangga
Jumaeri, dkk., 2003. Pengaruh Penambahan Bahan Pengikat Impurities terhadap Kemurnian
Natrium Klorida Pada Proses Pemurnian Garam Dapur Melalui Proses Kristalisasi. Laporan
Penelitian. Semarang: Lembaga Penelitian UNNES.
Jumaeri, R.d., 2015. PEMURNIAN GARAM DAPUR DENGAN METODE REKRISALISASI
DENGAN ZEOLIT ALAM SEBAGAI BAHAN PENGIKAT IMPURITIES. Indonesian
Journal of Chemical Science, 4. p.145.
Oxtoby, David. 2001. Prinsip-Prinsip Kimia Modern Jilid I Edisi 4. Ditejemahkan oleh
Achmadi, Suminah S. Jakarta : Erlangga.
Setyopratomo, Pungguh dkk. 2003. Studi Eksperimental Pemurnian Garam NaCl dengan
Cara Rekristalisasi.PDF. Surabaya : Jurusan Teknik Kimia Universitas Surabaya.
Sutrisnanto Danny. 2001. Persiapan Lahan dan Sarana Penunjang untuk Garam dan
Tambak. Departemen Perindustrian dan Perdagangan. Jakarta.
Syabatini, Annisa. 2008. Pemurnian Bahan Melalui Rekristalisasi (Purification of Material
Through Recrystallization).
(http://annisanfushie.wordpress.com/2008/12/26/pemurnian-bahan-melalui-
rekristalisasi/) Banjarmasin: Kimia FMIPA Universitas Lambung Mangkurat. Diunduh
pada 28 Maret 2014 Pukul 21.08 WIB.