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Experiment I
Experiment I
NaCl PURIFICATION
Date of labwork : April 28th 2015
A OBJECTIVE
1 Study the recrystallization method with the addition of impurity binder material.
2 Understand the methode of NaCl iodisation.
3 Calculate the purity levels of NaCl
B THEORETICAL BASIS
Salt or sodium chloride (NaCl) is a white solid substance which can be obtained by
evaporating and purifying sea water. it also can be obtained from the neutralization HCl
with NaOH solution. NaOH almost insoluble in alcohol, but soluble in water by absorb
heat, the change of solubility is very small with temperature. Normal salt is a salt which
does not contain hydrogen or hydroxide group which can be evicted. The aqueous
solution from normal salt is not always neutral to indicator, such as litmus. Double salt
is a salt which id formed from crytallization from an equivalen of two or more certain
salt, for example FeSO4(NH4)2SO4.6H2O and K2SO4Al4(SO4)3.24H2O.In the solution, this
salt is a mixed of any simple ions that will be ionizing when its dissolve again. So,
clearly different with complex salt that produce complex ions in the solution. (Syabatino,
2009)
Sodium chloride is one of material that widely used by people in food processing
and raw material in many chemical industries. The chemical industry that use sodium
chloride as the raw material is chlor alkaly industry. The main product of this industry is
chlorine (Cl2) and sodium chloride (NaOH), which needed by another industry, like pulp
and paper industry, textile, detergen, soap and water processing. (Lesdantina, et al., 2009)
In technical engineering solid materials are often separated from the solution or
melt, without binding the obtained impurities in its liquid phase. Also often the solid
crystalline material which contain the impurity must be cleaned or must be produced in
certain crystal form, so the crystallization process can be used. The crystal are the solid
material with the arrangement of atom or molecule regularly. The definition of
crystallization in the separation of crystal solid material from its solution or melt. The
result of crystallization from its melt often must be cooled again or reduced in size.
(Bernaseoni, 1995)
The crystallization from its solution is categorized as one of the efficient separaton
process. In general, the purpose of crystallization is to produce crystal product with the
quality as expected. The quality of produced crystal can be determined fom the product
parameters, there are crystal size distribution, the purity of crystal and the size of crystal.
One of the crystallization process requirementts is the occurence of supersaturation
condition. The supersaturation condition is the condition when the concentration of the
solution up to its solubility. This condition can be reached by evaporating, colling or the
combination of both. There are two important phenomena in crystallization process is the
formation of crystal nucleous (nucleation) and crystal growth. (Shevla, G., 1989)
The crystallization is a methode for purifying a substance with a solvent followed
by the precipitation process. In organic compound crystallization is affected by the
solvent. The crystallize solvent is a solvent that carried by the solute that forming the
precipitate and depending on its solute crystal structure. (Oxtoby, 2001)
Recrystallization is one of the purifying solid methode that plural used, in which
these substances dissolved in a solvent then recrystalled. This methode is depend on the
solubility of substance in the solvent when the temperature increase. Because of the total
impurities concentration commonly smaller than the concentration of the purified, if
cold, so the impurities concentration low but in the solution the product that has hight
concentration will form precipitate. (Arsyad, 2001)
Reccrystallization events accociated with the precipitation reaction. The precipitate
is a substance that separate as a solid phase and comes out from the solution. the
precipitate formed if the solution become too saturated with the concerned substance.
The solubility (S) of a precipitate according to the definition is equal with the molar
concentration of its saturated solution. the solubility depends on various condition such
as temperature, pressure, the other concentration of substance in the solution, and the
solvent composition. (Keenan, 2009)
The influence of the decreasing temperature in the crystal formation process :
a. If the decreasing temperature run faster, so the nucleous will formed faster than the
formation of crystal so the crystal obtained is small, fragile, and much.
b. If the decreasing temperature run slower, so the formation of crystal will run faster
than the formation of the nucleous so the crystal will be freed big, tough and elastic.
(Austin, 1986)
The precipitate is a substance that separate as a solid phase, out from the solution.
The precipitate is formed if the solution become too saturated with the concernned
substance. The solubility (S) of a precipitate according to the definition is equal with the
molar concentration from its saturated solution. The solubility is deppend on various
condition, such as temperature, pressure, concentration of another substance in its
solution, and the compotion of the solvent.
The solid organic compounds from the isolated organic reaction rarely in pure
form. Its compound are ussually contamined with a little another compound (impurities)
which formed during the reaction occured. The impurities in salt include hygroscopic
compound, there are MgCl2, CaCl2, MgSO4, and some reductor substance, there are Fe,
Cu, Zn and organic compounds. Its impurities can be reacted with hydroxil ion (OH -) so
it form white precipitate Ca(OH)2 and Mg(OH)2. The purification of impure compound id
ussually done by recrystallization with various solvent or mixture solvent. (Bahruddin,
et, al, 2003)
The purification of solid with the recrystallization based upon the differences in the
solubility in current solvent or mixed solvent. There are some definition about the
recrystallization, there are : 1. A process where the metal grains which is deformed is
replaced by the new grains that are not deformed which its nucleous grow until the
original grains included therein. 2. The change of crystal structure due to the heating at
critical temperature. 3. The formation of new structure of the grains through the grow of
nucleous by heating. (Anwar, 1994)
To reduce the salt impurities can be done with the combination froom the leaching
process and dissolving quickly at the process of making salt. While the removal of
impurities from the salt product can be done by chemical process, there is by reacting
with Na2CO3 and NaOH to form CaCO3 ang Mg(OH)2 precipitate. The addition of
Na2CO3 and NaOH is an important process in purifying salt process. To avoid the
occured of precipitate breaking which caused by the flagile metal hydroxide
characteristic, so Na2CO3 and NaOH added simultaneously and react together. The both
precipitation of CaCO3 and Mg(OH)2 will occured faster than the precipitation of
hydroxide. The good result also can be obtained if the Na 2CO3is added first before the
addition of NaOH. (Berseoni, 1995)
C METHODE
Equipment
Analytical balance
Bunsen burner
Burette 50 mL
Material
Dirty salt
CaO powder
Ba(OH)2 solution 1 M
Erlenmeyer 25 mL
Volumetric flask 100 mL
Volume pipette
Evaporating basin
Dropping pipette
Watch glass
Beaker glass
Spatula
Stirrer
Filter paper
Universal pH indicator paper
Methode
1. Purification of NaCl
Weight 2.5 gram
dirty salt with
analytical balance
Heat 25 mL aquades
in beaker glass up to
boil
Filter the
precipitate formed
Evaporate the
solution up to dry in
evaporating basin
Filter the
precipitate
Move it into
erlenmeyer
Add 1 mL
indicator K2CrO4
5%
Take 10 mL of
solution put into
erlenmeyer
Reperat the
titration two times
and record the
volume of AgNO3
D OBSERVATION DATA
a Color of the salt before purified : dirty white.
b Structur of salt crystals before purified : big, rought.
c Color of the salt after purified : clear white.
d Structure of salt crystals after purified : smooth.
e Volume of Ba(OH) required is : 3 mL
2
g
h
i
1.295 gram
2.50 gram
x 100%
= 51.8 %
j
Titration data :
Standarisation of NaCl p.a.
Volume of NaCl p.a.
Volume of AgNO3
10 mL
4.50 mL
10 mL
4.40 mL
Average volume
4.45 mL
Determination of N AgNO3
VNaCl . N NaCl = V AgNO3 . N AgNO3
0.25 gram
1000
10 . 58.46 gram/mol x 100 mL x 1 ekivalen = 4.45 mL . N AgNO3
0.4276 molek/mL
= 4.45 mL . N AgNO3
N AgNO3 = 0.0961 molek/mL
Titration of dirty NaCl
Volume of AgNO3
3.52 mL
3.50 mL
3.51 mL
Volume of AgNO3
4.18 mL
4.26 mL
4.22 mL
x 100%
x 10 x 100%
= 78.87 %
l
x 100%
x 10 x 100%
= 94.83 %
m Reactions :
The reaction between NaCl and CaO
CaO(aq)
Ca2+ (aq) + O2-(aq)
2+
2Ca (aq)+ CO3 (aq) CaCO3(s)
Ca2+(aq)+ SO42-(aq) CaSO4(s)
CaO, but Ba(OH)2 is used to remove the Mg2+ and Fe3+ ion as an impurities and form
white precipitate. The white precipitate are Fe(OH)2(s)and Mg(OH)2(s) . Fe(OH)2(s)and
Mg(OH)2(s) can be precipitated because the Qc of both is smaller than its Ksp. The
occured reactions in this process are:
Ba(OH)2(aq)
Ba2+(aq) + 2OH-(aq)
Fe2+(aq) + 2OH-(aq) Fe(OH)2(s)
Ksp = 4.8 x 10-16
as 0.25 gram of salt and then dissolved in 100 ml aquades. Then take 10 mL of the
solution and add with K2Cr2O4 as indicator. Titrate it with AgNO3 until the color
become red brick. Based on the experiment, the average volume of AgNO 3 is 4.22
mL and based on the calculation the purity levels of this salt is 94.83 %.
This is accordance with the theory that the purity levels after recrystallization
is bigger than the purity levels of dirty salt. The structure of the pure salt become
smooth and the colour become clearl white. The occured reaction is this process are :
AgNO3(aq) + NaCl(aq) NaNO3(aq) + AgCl(s)
(white)
2AgNO3(aq) + K2CrO4(aq) 2KNO3(aq) + Ag2CrO4 (s) (red brick)
F CONCLUSION
The principal method of the NaCl purification is recrystallization with the
evaporation and with the addition of some solutions such as CaO, Ba(OH) 2, and
(NH4)2CO3 to bind the impurities like Ca2+, CO32-, SO42-, Mg2+ and Fe2+ions.
The purity levels of NaCl ditry salt is 78.87% and the purity levels of NaCl pure salt
from recrystallization is 94.83%.
The NaCl salt after the purification process has smooth structure and the color
become clear white because the impurities has gone.
G SUGGESTION
Be carefull with dangerous material such as AgNO3 and use gloves when use it.
Be careful when add some binder material.
Do the titration accurately and carefully.
Observe the experiment result accurately.
H LITERATURE
Anwar, C. 1994. Pengantar Praktikum Kimia Organik I. Yogyakarta :FMIPA UGM..
Arsyad, M. Natsir. 2001. Kamus Kimia dan Penjelasan Istilah. Jakarta : Gramedia.
Austin, G. T. 1996. Industri Proses Kimia, Edisi Kelima. Jakarta : Erlangga.
Bahruddin, Zulfansyah, Aman, Ilyas Arin, Nurfatihayati. 2003. Penentuan Rasio Ca/Mg
Optimum pada Proses Pemurnian Garam Dapur. Jurnal Natur Indonesia 6(1):
16-19.
Bernaseoni,G. 1995. Teknologi Kimia. Jakarta : PT Padya Pranita.
G. Svehla. 1979. Buku Teks Analisis Anorganik Kualitatif Makro dan Semi Mikro Bagian
I. Jakarta : PT Kalman Media Pustaka.
G. Svehla. 1985. Buku Teks Analisis Anorganik Kualitatif Makro dan Semi Mikro Bagian
I. Jakarta : PT Kalman Media Pustaka.
Keenam.1979. Kimia Universitas Jilid 2.Jakarta:Erlangga.
Lesdantina, D., dan Istikomah, 2009. Pemurnian Nacl Dengan Menggunakan Natrium
Karbonat. Seminar Tugas Akhir S1 Teknik Kimia UNDIP.
Oxtoby, D. W. 2001. Kimia Modern. Jakarta : Erlangga.
Saito, Taro. 1996. Muki Kagoku. Tokyo : Iwanami Shoten Publisher
Syabatini, A.,. 2009. Pemurnian Bahan Melalui Rekristalisasi. http://annisanfushie.
wordpress.com. Diakses tanggal 28 April 2015.
APPENDIX
1 Purification of NaCl
Boiling aquades
Impurities
Filtrate + CaO
White precipitate
Residue
Filtrate
Residue
Filtrate
Ba(OH)2
Filtrate
Check pH
Filtrate +Ba(OH)2
dropwise
Filtrate + (NH4)2CO3
Standarisation AgNO3
Check pH