NaCl PURIFICATION AND IODISATION

2th June 2015

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 FOR THEORY
Of 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.
According to (Syabatini: 2008 ) 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. According to ( Oxtoby, 2001 ) 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.
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.
1.
2.
3.
4.
5.

According to ( Fessenden , 1983 ) can also a recrystallization steps were:

Dissolving a substance in a solvent.
Filtration gravity do.
Take crystalline substance dissolved.
Collecting crystals with vacum filtration.
Crystalline dry

C. EQUIPMENT AND MATERIALS

Equipment:
1. Spiritus
2. Erlenmeyer 25ml
3. Dropping pipette
4. Ball pipette and pipette volume
5. Droping plate
6. Beakerglass
7. Watch glass
8. Measuring glass
9. Evaporating dish
10. Burette
11. Spatula

Materials:
1. HCl 1,5M
2. HNO3 p.a
3. AgNO3 0,1 N
4. CaO
5. Dirty salt
6. Ba(OH)2 1M
7. (NH4)2CO3 0.1 M
8. K2CrO4
9. NaHCO3
10. Aquadest
D. WORK STEPS
1. Purification Of NaCl
2,5 g of dirty slat
-Including dirty salt in the beaker glass
containing 25 mL of hot distilled
water, stirring and heating again
until dissolved
-Filtering the solution

Filtrate

Residue

-Adding 0,05 g CaO and filtering the

pericipitate
-Adding Ba(OH)2 solution 0,1, then
filtering the precipitate again

Filtrate

Residue

Adding 5 mL of (NH4)2CO3
0,1M dropwise
Allowing the solution for 5
minutes
Filtering the solution

Filtrate

Residue

-Checking pH
-Neutralizing with dilute HCl
-Evaporating the solution up to
dry
NaCl crystal
-Weighing the crystal
-Drying and weighing the
precipitate
2. Determination impurities
of Purity Levels
of NaCl
obtained from the
filtration
0,25 g of dirty
-Dissolving in 100 ml of distilles water
(100 ml of volumetric flask)
-Moving into the erlenmayer
-Checking the pH, if too much acid,
adding a solution of NaHCO3, if too
10 ml of alkaline adding HNO3

Adding 1 ml of
indicator K2CrO4 5%

Titrating the solution with

0,1 N AgNO3 solution until
the solution color is red

Repeating
the

Doing the
determination of purity
levels og NaCl before
anf after

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: 1,503 gram
h. The weigh of salt crystal from salt recrystallizing: 2,50 gram
i. The percentage of pure salt from recrystallizing process: 59,82%
j. The purity levels of NaCl before recrystallizing process: 94,72 %
k. The purity levels of NaCl after recrystallizing process: 96,48 %
F. ANALYSIS DATA
The percentage of pure salt from recrystallizing process:
weigh of impurities
weigh of pure salt crystal
Rendemen=
salt 100

1,503
100
2,50

60,12

Titration data:

M NaCL pa = 0,25 gram

V solvent = 100 ml
0,25 x 1000 x 1
N =
58, 46 x 100

Standarisation
V1 x N1
= V2 x N2
10 x 0,043 = 2,4 x N2
N2 = 0,1791

= 0,043 N

Before a recrystallization titration

V1 = 2,5 ml
V2 = 2 ml

Vtot= 2,25 ml

%NaCl=

( V . N ) AgNO 3 x 58,46
W x 1000

x 100%

( 2,25 x 0,1791 ) x 58,46

x
0,2491 g x 1000

100%

The purity levels of NaCl before

recrystallizing process:

= 94,72 %

After a recrystallization titration

V1 = 2,2 ml
V2 = 2,4 ml

Vtot= 2,3 ml

The purity levels of NaCl after

recrystallizing process:

%NaCl=

( V . N ) AgNO 3 x 58,46
W x 1000

x 100%

( 2,25 x 0,1791 ) x 58,46

x
0,2496 g x 1000
100%

= 96, 48 %

The reaction occurs in the purification NaCl and iodisation namely:

1. Reaction NaCl with CaO
CaO
Ca2++ O2 Ca2++ CO32CaCO3(s)
2+
2 Ca + SO4
CaSO4(s)
2. Reaction the addition of Ba(OH)2
Ba(OH)2
Ba2+ + 2OH Fe2++ 2OHFe(OH)2(s)
Ksp = 4,8 x 10-16
Mg2++ 2OHMg(OH)2(s)
Ksp = 3,4 x 10-21
3. Reaction the addition of (NH4)2CO3
(NH4)2CO3
2NH4++ CO32 Ba2++ CO32BaCO3(s)
Ksp = 8,1 x 10-9
Ca2++ CO32CaCO3(s)
Ksp = 4,8 x 10-9
4. Reaction the addition HCl
NH4++ HCl
NH4Cl (neutral)
A reaction which occurs on the determination of NaCl ( levels titration AgNO3 )
namely:
1. AgNO3+ NaCl
2. AgNO3 + K2CrO4

AgCl(s)+ NaNO3 (white)

Ag2Cr2O4 + KNO3 (red brick)

G. DISCUSSION

At the time we did this experiment is purification NaCl and

iodisation.

Materials used to be purified is salt krosok. A salt of krosok we choose aims to purify salt.
Salt krosok is it still many pollutter. Therefore, it should be done so that the purification is
separated from pollutter krosok salts. Pollutter being carried away by a usually derived
from ions Ca2+, Mg2+, Al3+, Fe3+, SO42-, I- and Br-.

Pollutter in crystal consisting of two categories is pollutter who are on the

surface of crystals and pollutter in in 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 terorientasi a crystal lattice.

In the purification krosok salt is NaCl separation of pollutter started dissolving

of salt krosok aquades in heat. The use of heat is intended to aquadest krosok readily
soluble or requiring relatively short time late to be perfect. On dissolving the salt this
krosok pollutter which are outside the lines the salt will settles. Then filtering done. Of the
results of screening used in the next step is filtrate.

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. Besides recristaltisation be
done by adding similar ions into a solution that will be separated.

The first is the addition of the pollen CaO serves to enlarge the difference
between resources soluble NaCl and pollutter, where CaO will break down into Ca2+ and
O2- and will attract Cl, and CaO ions so that arising precipitate white CaCl2 are white.
Reaction: 2NaCl(aq) + CaO(s) + H2O CaCl2(s) + 2Na+ + 2OH

Ion Ca2+ will react with substances Ca2+ pollutter because the nature of
carbonate ions capable of binding or sulphate . Calcium carbonate can settles for smaller
than the ksp his 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.
Reaction:

CaO Ca2+ + O2
Ca2+ + CO32- CaCO3 (s)

Ca2+ + SO42- CaSO4 (s)

(Vogel, 1990)

Solution is then percolated with paper strain. Then added drops filtrat produced
for the drops with solution Ba(OH)2 dilute not to precipitate formed again and to prove
that contained in a solution of ions Cl- has bonded with Ba2+ all the sediment and so
produces BaCl2. The purpose of the addition of Ba(OH)2 to separate Cl from CaCl2.
The reaction:

2NaCl(aq) + CaO(s) + Ba(OH)2(aq) + H2O BaCl2(s) + Na+ + 4OH- + Ca2+

Ba(OH)2 will experience the decipherment of being Ba2+ and OH- , OH- it

serves bind polutter Fe2+ and Mg2+ of the remaining.

The reaction was:

Ba(OH)2 Ba2+ + 2OH

Reaction between OH- with Fe2+ and Mg2+

Fe2+ + 2OH- Fe(OH)2(s) Ksp = 4,8 x 10-16

Mg2+ + 2OH- Mg(OH)2(s)

Ksp = 3.4 x 10-11

The next step is the addition of Ba(OH)2 which was later continued with the
addition of (NH4)2CO3 functioning ion binding to Ba2+ and Ca2+ contained in solution in
excess so that retrieved the white deposits back. Reaction equation:
BaCl2(s) + Na+ + 4OH- + Ca2+ + (NH4)2CO3 BaCO3 + NH3(g) + Na2CO3 + CaCl2(s)

After addition (NH4)2CO3 last solution then strained. The solution is a solution
that is alkaline with an acid counteraction so that there should have been. Counteraction
serves to salt can be formed, because basically salt is neutral. After neutral, filtrat
volatilized to dry to deprive NH4+ and H2O and other ions volatile, so formed crystalline
NaCl pure white ones clean with heavy 1,503 grams and randemen product produced as
much as 60,12 %.

Then determine levels of salt dirty and salt pure or salt that is separate from
substances polllutter who has previously done a recrystallization. On experiments we did
AgNO3 we use already standaritation formerly namely 0,1791 N. In the process of
titrating argentometri this will precipitate formed AgCl that white if plus AgNO3 would
react to form the sediment Ag2CrO4 in red brick. After the process of titrating obtained the
results of the salt content is of krosok 94,72 % .While pure salt content of the results of a
recrystallization, the content of 96,48%.

Compared according to the theory, the results of experiments conducted what

we are doing is the result of that has no fitting with the theory. On the theory it was stated
that the results of the level of NaCl that has been recrystallized will have levels of larger
than salt that has not been recrystallized. But in fact a group of us precisely the level of a
salt or NaCl that after a process of a recrystallization is declining.This is possibly because
the we, praktikan decided to use solution AgNO3 who have standaritation formerly
without new repeated do. In addition when process of titrating happened to leakage in
buret it was predicted that many AgNO3 that is spilled.

H. CONCLUSION
Of experiments on inconclusive take:
Dirty salt pollutter is still there. Pollutter the existing in crystal consisting of two
categories is pollutter existing in the crystal and pollutter in the crystal. Pollutter that it '
s coming from the surface of a crystal that are brought to the surface of a solid during

the process of separation from their parents while being carried away in crystalline salt

is usually derived from ions Ca2+, Mg2+, Al3+, Fe3+, SO42-, I- dan Br-.
Recrystallization is a method used to purify the solids with the principle differences
dissolve power between substances of purified by pollutter in a particular solvent heated

and then evaporated back.

Dirty salt recrystallized that has been clean more visible, crystalline NaCl pure white
ones clean with heavy 1,503 grams, and rendemen purity of salt 94,72 % and rendemen

of salt a recrystallization 96,48 %.

I. SUGGESTION
Advice that can be given to the purification of NaCl on trial next praktikan:
Praktician need to know who will practiced elementary lab work.
Fellow group members can work same time and each other.
Every praktician should ensure that materials in accordance with a substance needed
especially normality.

J. REFERENCE
Fessenden. 1983. Kimia Organik. Jakarta : Erlangga
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.

Syabatini, Annisa. 2008. Pemurnian Bahan Melalui Rekristalisasi (Purification of

Material Through Recrystallization).

(http://annisanfushie.wordpress.com/2008/12/26/pemurnian-bahan-melaluirekristalisasi/)
Banjarmasin: Kimia FMIPA Universitas Lambung Mangkurat.
Diunduh pada Rabu, 16 April 2014 Pukul 10.45 WIB.

Tim Dosen Kimia Anorganik. 2014. Petunjuk Praktikum Kimia Anorganik.

Semarang : Laboratorium Kimia Anorganik Jurusan Kimia FMIPA UNNES
Vogel. 1990. Analisis Anorganik Kualitatif Makro dan Semimikro. Jakarta : PT
Kalman
Media Pustaka.