ANALYTICAL CHEMISTRY II LABWORK REPORT

ELECTROGRAVIMETRY

Name : Asti Dian Arini

St.Number/Study Program : 13303241031/Chemistry Education

Class/Group : PKI 2013/2

Day of Experiment : October, 12th 2015

Deadline : October, 19th 2015

ANALITICAL CHEMISTRY LABORATORY

FMIPA

2015
 LABORATORY LABWORK REPORT

ANALYTICAL CHEMISTRY II

ELECTROGRAVIMETRY

A. PURPOSE
After doing the experiment, student can do separation by Electrogravimetry
method

B. THEORITICAL BACKGROUND

Elektrogravimetry is a method of analysis that is based on the deposition of

substances using electricity. The substance is an metal and it is precipitated by
electrolysis. In electrogravimetry experiments is used inert electrode that usually
in the form of platinum metal to avoid the occurrence of coprecipitation. (
Soebagio, 2003 : 168) Electrolysis is a process where electric current is produce
chemistry changing. Solution that can deliver the electric current is called as
electrolyte solution. Electrolyte solution is always contains of positive ions and
negatives ions.
Electrolysis cell is commonly consist of electric source that supply direct
current ( DC ), cathode ( electrode where reduction reaction is take place
because the electron is driven by negative pole from electric source so the
cathode become negatively charged (-)), anode ( electrode where oxidation
reaction is take place because electron from anode is withdrawn by positive pole
from electric source so the anode become positively charged (+)), and
electrolyte ( that is a substance that can conduct electricity that will be parsed in
electrolysis cell ). ( Chang R : 2005 )
Elemental analysis by electrolysis is done by Faraday and ohms law.
Michael Faraday discovered the relationship between substance produced from
the electrode to the amount of electricity used . The capacity of the basic unit of
electricity that states the number of electrons that pass through the electrolyte is
coulomb . Based on the charge of the electron calculation gives the price of
96500 C ( C ) is equal to 1 mol electron passage. The amount of electricity is
called with 1 Faraday. 1 Farday = 1 mol elctron = 96500 C.
I Farday law states the amount of a substance that is deposited on the electrodes
during electrolysis takes place in proportion to the amount of electric current
flowing through the solution .

e. i. t
𝑾=
F

W = mass of substance precipitated ( gram )

e = mass ekivalen of substance
i = electric current ( A )
t = electrolysis time ( t )
F = Faraday number ( 96487 s )

II Faraday's Law states that when the amount of electric current is passed in a
solution containing for example copper sulphate and silver nitrate , then the mass
of copper sulphate and silver nitrate that precipitate is the ratio of the its mass
ekivalen.
Ohm’s Law state that electric current that flow through a conductor is
opposite with the resistance and equal to the voltage.

E
𝑰=
R

I = electric current ( A )
E = Voltage ( V )
R = Resistance ( Ohm )
( Soebagio, 2003 : 168 - 169 )
Determination of copper is one example elektrogravimetri . the sample
may be an alloy of copper , dissolved in nitric acid . platinum cathode that has
been cleaned in nitric acid , rinsed , dried in an oven and weighed , put into a
solution and connected to the mains and connected with a metal clip . Clamp
 voltage is increased until the ammeter shows the current and produce cathode
copper shapes and bubbles will be seen rising from the anode . in practice , the
form of the equation for E applications at the top can not be calculated
accurately . calculated outlined what the E app and add a little tension to ensure
the electrolysis takes place . for a certain time , can be tested for perfection of
deposition by lowering the cathode and observe whether the new platinum
surface to obtain a copper plate. In the end , the cathode voltage is removed from
the solution by still light up when rinsed with distilled water . then cathode
dipped into acetone and weighed. ( Underwood, 2001 : 342-343 )
Cu -containing material must be made of salts and dissolved with HNO3 and
H2SO4 .
The reaction is :
Cathode ( reduction ) (-) : Cu2+ + 2e Cu E0 = 0.337 V
H+ +e ½ H2 E0 = 0.000 V
Anode ( oxidation ) (+) : H2O ½ O2 + 2H+ + 2e- E0 = 1.299 V
Nitrate ion that has a role as depolarisator at cathode :
NO3- + 10 H+ + 3e- NH4+ + 3 H2O
Nitrates are used must be free of nitrites in order not to complicate the
attachment of sludge on the cathode . to eliminate nitrite solution can be spiked
with urea
2HNO2 + CO ( NH2)2 2 N2 + CO2 + 3H2O
Or also it probably to add with sulfanat acid :
HOSO2NH2 + HNO2 H2SO4 + N2 + H2O
While the current efficiency can be determined by :

C. APPARATUS AND CHEMICALS

1. Apparatus
a. Analytical balance
b. A set of electrolysis tool
c. Stopwatch
 d. Pipette
e. Stirrer
f. Drop pipette
g. Test tube
2. Chemicals
a. Concentrated nitric acid ( free nitrate )
b. Diluted nitric acid
c. Acetone
d. Hexacianoferate solution
e. Sulfuric acid solution
 D. PROCEDURE

Electro
de Diluted
Washed HNO3 25 mL of sample solution Cu ( II )

Rinsed Electrode Aceton 2 mL of Electrode 1 mL of

concentrat HNO3
ed H2SO4

Using aquades until 25 Diluted

mL

Electrolyzed in 3 Volt

Write the strating time

Take some drop of sample Hexacyanoferat ( II ) reagen

Negative result Possitive result

Stop the electrolysis

(write the time)

using
Washed electrode Diluted HNO3

Dried the elctrode

Weighted the electrode and nickel bowl

E. SKETCH OF APPARATUS

F. DATA OF EXPERIMENT
Observation Data
Voltage ( V ) 3V
Electric current ( I ) 0.2 A
58 minutes
Electolysis time ( t )
( 3480 seconds )
Mass of initial Pt 0.677 gram
Mass of Pt after electrolysis 0.521 gram
Relative atomic mass of Cu 63.5
Mass of initial nickel crush 54.570 gram
Mass of crush + precipitate
54.834 gram
(after electrolysis )
Valence 2
Volume of sample 50 mL
Color of solution Clear turquoise
Color of precipitate Crimson

G. CALCULATION
1. Mass of copper ( Cu ) based on theory

i . t . Ar Cu
𝑾=
96500 valence

0.2 A .3840 seconds . 63.5

=
96487 . 2
 44196
=
192974

= 0.229 gram
2. Mass of copper mass based on experiment
 Mass of all precipitate = ( mass of nickel crush + precipitate ) – mass
of empty nickel crush
= 54.834 gram - 54.570 gram
= 0.264 gram

Because there’s a mass reduction of Pt Electrode, so the precipitate

that was formed from Cu is increasing because of the precipitate of Pt,
so the precipitate of Cu can be determined :

 Mass of Pt precipitate = Mass of initial Pt - Mass of Pt after

electrolysis
= 0.677 gram - 0.521 gram
= 0.156 gram
 Mass of Cu precipitate = mass all of precipitate – mass of Pt
Precipitate
= 0.264 gram – 0.156 gram

= 0.108 gram

3. Precentage of copper ( Cu ) in sample

100 Mass of Cu precipitate
Precentage of Cu = x x 100 %
25 volume of sample
100 0.108
= x x 100 %
25 50

= 0.864 %
4. Current Efficiency
mass of Cu precipitate based on experiment
Current efficiency = x 100 %
mass of Cu precipitate based on theory
0.108 gram
= 0.229 gram x 100 %

= 47.16 %

H. DISCUSSION
 This experiment entitled “Electrogravimetry” was done at Oct, 12th 2015. The
purpose of this experiment do separation by electrogravimetry method.
Elektrogravimetry is a method of analysis that is based on the deposition of
substances using electricity. The substance is an metal and it is precipitated by
electrolysis. In electrogravimetry experiments is used inert electrode that usually
in the form of platinum metal to avoid the occurrence of coprecipitation

Before doing experiment, the platinum electrode and nickel bowl was
washed using nitric acid and then rinsed by acetone. Cleaning platinum
electrodes and nickel bowl is to eliminate compounds which are left in the cup
electrode and nickel . Dilute nitric acid solution is used because it can stabilize
the ions inside the cup eletroda and nickel . While rinsing using acetone aimed at
dissolving compounds which are non polar compounds that are not soluble in
dilute nitric acid solution .
The sample solution which was used was 25 mL sample solution of Cu (
II ) were combined with 2 mL concentrated acid and 1 mL HNO3, then diluted
with aquades to 100 mL . The addition of sulfuric acid is used to make the
solution under acidic conditions. Whereas the addition of concentrated nitric
acid serves as depolarisator at the cathode . nitric acid used should be free of
nitrites in order not to complicate attachment nitrite sludge on the cathode .
before electrolysis , clear turquoise.
Sample solution was electrolyzed using 3 V. Electrolysis is done by
connecting the nickel bowl ( cathode ) on the adapter while the negatively
charged anode in the form of platinum metal plate is then dipped into a solution
but must not be attached to the cathode . the sample solution is used by 50 mL .
a suite of tools associated with voltmeter and ammeter .
Working principle of electrolysis is to connect the negative pole of the
power source to the cathode and the anode to the positive pole. Negative pole
which come from electric source will drive electrons flow to the cathode so that
the negatively charged cathode ( - ) . While the positive pole from electric source
will pull electrons from the anode to the anode becomes positively charged ( + )
. Cathode which has a negative charge will attract positive ions in the electrolyte
( Cu2+ ions ) that will be obtained half the reduction reaction . Whereas the anode
which has a positive charge will attract negative ions in the electrolyte . this
causes oxidation half reaction.
Cathode ( reduction ) (-) : Cu2+ + 2e Cu E0 = 0.337 V
H+ +e ½ H2 E0 = 0.000 V
Anode ( oxidation ) (+) : H2O ½ O2 + 2H+ + 2e- E0 = 1.299 V
The number of E0 for sulphate ion oxidation 2SO42- S2O82- +2e- is 21 V.
This number of E0 sulphate ion is greater adn more positive than the voltage that
is needed to oxidize water as solven. That is the reason why sulphate ion is not
electron active species in aqueous solution.
The number of potential reaction for copper is greather and more positive than
the half reaction of hydrogen so copper ( II ) wil be easier reduced rather than
hydrogen ion. The whole reaction that was occur at electrolysis cell is
Cu2+ + H2O Cu + ½ O2 + 2H+
Concentration of Cu2+ was lowered by electroreduction so the charge of cathode
became more negative so reduction of nitrate than occur as follow :
NO3- + 10H+ + 8e- NH4+ + 3 H2O
This will lead to the stability of the potential at the cathode , where the cathode
not be negative enough to then reduce certain metals other metals that may be
present in the sample . also can prevent the reduction of H + unwanted . in this
case due to the concomitant hydrogen evolution tends to result in deposition of
copper and does not stick .
During the process of electrolysis , stirring constantly . this is done so
that the concentration is always homogeneous , especially on the electrode
surface . metal that was precipitated was stick at nickel bowl as a pink layer
covering the surface . By using the potential difference of 3 V , the electric
current of 0.5 A legible.
Electrolysis is done until there are no Cu2+ ions in solution . To
determine whether there are Cu2+ or not in solution , then used hexacioanopherat
( II ) solution to test it. If the solution turns brown then there is still a Cu2+ in
solution. The reaction is :
2 Cu2+ + [ Fe(CN)6]4- Cu2[Fe(CN)6](s)
Brown
The colour substance that produced is the precipitate from of Cu2[Fe(CN)6] This
electrogravimetry process that used electrolysis principal is finish if the result
show negative result or means the color of solution after dropped with reagen is
not change to brown.
In this experiment, electrolysis process was done for 58 minutes or 3840
second although the result of test was not show the negative result yet because of
the time limitation of the experiment. But but already formed pretty much
precipitate. At the end of the electrolysis process, the color of the solution is
blackish green, this color is because there is hexaquonickelat ( II ) complex, [ Ni
( H2O)6] 2+ or usually considered as nickel ( II ) ion. Presence of sulfuric acid in
the electrolyte solution will dissolve the nickel to form hydrogen.
Ni + 2H+ Ni2+ + H2

After electrolysis is complete , the remaining solution was poured and the
cup electrode nickel washed with acetone . It is no need to wipe because acetone
is volatile and when wiped electrode deposition may be lost ( carried over ).
After drying, the nickel cup is then weighed and the result amounted to 54 834
grams . From the data obtained , it can be done a few calculations . The first
calculation is to calculate the masses of sediment Cu ( II ) in theory by the
formula :
i . t . Ar Cu
𝑾=
96500 . valence

W = mass of Cu ( II ) precipitate based on theory ( gram )

i = electric current ( A )
t = electrolysis time ( t )
F = Faraday number ( 96487 s )
Precipitate of copper ( II ) obtained through theoretical calculation that is equal
to 0.229 gram. After that, calculating the precentage of Cu in the sample using
the formula:
 The percentage of Cu from the calculation above is 0.864 %. Then the last
calculation is counting the electricity efficiency by formula :

And obtained the number of electricity efficiency is 47.16 %.

The different result that was obtained by the calculation based on theory
and experiment, also the electricity efficiency that was not reach 100 %, is
probably caused by :
1. sulfuric acid that used is too concentrated so that precipitate can not be
attached properly
2. not all Cu terelektrolisis perfectly
3. The time for doing the elctrolysisi is too fast so the electrolysis process are
not done perfectly so not all Cu electrolyzed perfectly
4. Not all the incoming electric current can all be used to precipitate the Cu2+
ions in solution
I. CONCLUSION
1. The separation of Cu and its solution was done by electrogravimetry.
Electrogravimetry is the method of separation where the substance observed
is a metal that was precipitated by electrolysis.
2. Mass of Cu based on theory = 0.229 gram
Mass of Cu based on experiment = 0.108 gram
The percentage of Cu in sample = 0.864 %
Current efficiency = 47.16 %
J. ASSIGNMENT
Precentage of copper ( Cu ) in sample
100 Mass of Cu precipitate
Precentage of Cu = x x 100 %
25 volume of sample
100 0.108
= x x 100 %
25 50

Current Efficiency
Current efficiency
= 0.864 %
mass of Cu precipitate based on experiment
= x 100 %
mass of Cu precipitate based on theory
 0.108 gram
= 0.252 gram x 100 %

= 47.16 %
K. REFERENCES
Chang, R., 2005. Kimia Dasar. Erlangga, Jakarta
Khopkar, S.M. 1990. Konsep Dasar Kimia Analitik. Jakarta: UI Press.
Soebagio, et al . 2005. Kimia Analitik II. Malang: UM Press.
Underwood. 1985. Analisi Kimia Kuantitaif. Jakarta: Erlangga.
Vogel. 2002. Kimia Analisis Kuantitatif Anorganik. Jakarta. FGC