FORMAL REPORT

ANALYTICAL CHEMISTRY II LAB-WORK

ELECTROGRAVIMETRY

Arranged By
Krisna Raditya Pratama
(13303244009)
Group 2

DEPARTMENT OF CHEMISTRY EDUCATION

FACULTY OF MATHEMATICS AND NATURAL SCIENCE
YOGYAKARTA STATE UNIVERSITY
2015

ELECTROGRAVIMETRY

A. OBJECTIVE
To separate with electrogravimetry method.
B. THEORITICAL BACKGROUND
Elektrogravimetry is a method that uses ion separation and measurement of
samples, usually of metal. In this process, the sample solution is done through
electrolysis in which the electrochemical reduction caused analyte deposited on the
cathode. The yield on the cathode is weighed before and after the experiment, and the
difference can be used to calculate the percentage of samples in solution. Electrolysis
is a process by which an electric current produces a chemical change. A solution that
can conduct electric current is called an electrolyte solution. In the electrolyte solution
always contained positive ions and negative ions. Elemental analysis by electrolysis
based on Ohm's Law and the two Faraday's law of electrolysis.
Faraday's First Lawstates that the amount of substance deposited electrodes
during electrolysis takes place in proportion to the amount of electric current flowing
through this solution
W=
which, W is the weight of a substance that is deposited (grams)
e is the equivalent weight of substances
i is a strong current (Ampere)
t is the electrolysis time (sec)
F is the Faraday number (96500 Coulomb)

Faraday's Second Law states that when a number of electric current is passed
in a solution containing for example copper sulphate and silver nitric, then the weight
of copper sulphate and silver nitric which settles an equivalent weight ratio.
Ohm's law states a strong current flowing through a conductor is inversely
proportional to custody and is directly proportional to the voltage
I=
Which, I was strong current (Ampere)
E is the electric voltage (Volt)
R is the resistance / resistance (Ohm)
(Soebagio, 2003: 168-169)
Explained voltage is outside the minimum voltage to be supplied to the
continuous electrolysis. This decomposition voltage visible when the electrolysis
current changes suddenly. Polarization voltage is the voltage that occurs after the
electrolysis was stopped. At the time stopped, turned into a means of electrolysis
current source. Tegangna excess occurs due digunaknnya higher potential than the
electrode potential is calculated by Nerst equation for the reaction to run.
Several chemical separation has a special purpose. In addition to purify the
compound, the separation is often done for the first step in an analysis of compounds.
Separation can take place both qualitatively and quantitatively. Quantitative
separation is generally used to ascertain the weight of which is an integral component
to do further calculations. Elektrogravimetry is one method of determining
quantitatively. Simply put, the analyzed components deposited on an electrode that
has been known weight and perfect after precipitation occurs weighed back electrode
and sediment. Ideally, the sediment must be strongly attached to the electrode,
meetings and smooth so that when washed, dried and weighed do not cause weight
loss. The precipitate that is formed must be fine-grained, uniform and looks like loga.
If the precipitate formed sponge, powder and lumps which are not well attached to the
electrode, it will cause less purity. The main factors that affect the physical properties

of the sediment is the current density, temperature, presence or absence of complexing

zzat. The amount of current density that will either lead to precipitate obtained perfect
<0.1 A / cm2. Precipitation along with hydrogen gas can be prevented by the addition
of a depolarization of the cathode. E.g. nitric ions:
NO3 + 10 H+ + 8e NH4+ + 3H2O
In general, the Pt electrode, the advantage is inert, can dipijarkan to remove fat,
organic matter or gas without damaging the metal Pt. For the metals Zn, Bi, and Ga
are not deposited directly on Pt electrode, but the Pt electrode to be coated first with
copper metal.
Copper deposition can be made from a solution of H2SO4 / HNO3 or a
mixture of the two, in which the electric potential of 2-3 volts are used, so that the
reaction occurs
Cathode:

Cu2+ + 2e Cu
2H+ + 2e H2

Anode :

4OH- O2 + 2 H2O + 4e

Elektrogravimetry analysis is based on the principle of electrolysis cell

wherein the determination of the amount of electricity and time variables become very
important. In general, there are three kinds of conditions that can be applied to an
electrolysis cell, namely:
a. Electrolysis is carried out at a potential price lura used (Eapp) at a fixed price
b. Electrolysis is carried out at a fixed current price
c. Electrolysis is done by maintaining the cell potential one electrode at a fixed
price.
When electric current flows into an electrochemical cell, the overall potential is
influenced by three other phenomena that arise, namely the presence of ohmic
potential, concentration polarization and polarization kinetic.
Ohmic potential is referred to as a potential fall where just of this ohmic
potential of IR. The ohmic potential can occur either on the galvanic cell and the

electrolysis cell. The effect of this is the ohmic potential can increase the potential
required to drive an electrolysis cell and vice versa can minimize the potential
measured in a galvanic cell
Ecell = Ecathode Eanode - IR
Several general terms relating to the overpotential is
a. Overpotential rise to the increase in current density
b. Overpotential decreases with increasing temperature
c. Overpotential changes to the composition of the electrode
d. Overpotential is evident in the process - the process of electrodes that produce
gases such as hydrogen or oxygen gas and overpotential apat ignored if the
form of sediment or a change in oxidation state
e. The amount of overpotential in units specified is difficult to predict precisely
because it is determined by a number of variables that can not be controlled

Elektrogravimetry principle of analysis is similar to gravimetric analysis. Only

here there elektrogravimetry substance to be determined will settle or stick to the
electrodes during the process eletrolisis using an electric current. Metals that will be
determined in the solution should be in the form of cations. Simply put, the analyzed
components deposited on an electrode that has been known to weigh and after the
deposition of known weight and perfect after precipitation occurs weighed again.

C. TOOLS, APPARATUS AND MATERIALS

1. Tools and Apparatus
a. Analytical Balance
b. Set of Electrolysis Apparatus
c. Stopwatch
d. Measuring Pippette
e. Stirrer of Glass
f. Dropped Pippette
g. Beaker Glass
h. Nikel bowls

2. Materials
a. Sample of CuSO4 solution
b. Nitric acid concentrated (free of nitric)
c. Nitric acid diluted
d. Acetone
e. Sulphate acid concentrated solution
f. Pt electrode
D. PROCEDURE
Electrode

Diluted of
Nitrate Acid

Acetone
dried

weighted

50 mLsample solution
of Cu (II)

Analytical
Balance
2 mL of sulphate acid

Beaker Glass
diluted until 100
mL with
aquades

Nikel bowls

2 mL of concentrated
HNO3

weighted

Electrolysis

Potential 3 V

Stop the Electrolysis Process

Dried the Electrode

Weighted with
Analytical
Balance

E. EXPERIMENT SCHEME

F. DATA OF EXPERIMENT
Observation

Data

Voltage (V)

Electricity Current (I)

Time of Electrolysis (t)

Molecular Mass (Mr)

Valence

Mass of initial Pt

0,907 grams

Mass of Pt after electrolysis

0,172 grams

Mass of initial Nikel bowls

Mass of Nikel bowls after

electrolysis
Volume of sample

Color of the precipitate

Mass of precipitate

3V
0,2 A
52 minutes
63, 54 grams/mole
2

54,558 grams
55,712 grams

50 mL
red brick
1,154 grams

G. CALCULATION
1. Mass of Cu based on Theory
W

=
=
=
= 0,21 grams

Mass of Cu based on Experiment

Mass of Precipitate

= (Mass of Nikel bowls+precipitate) Mass of Nikel

Bowls
= 55,712 grams 54,558 grams
= 1,154 grams

Because there was decreasing of mass of Pt electrode, so, a precipitate which

produced was mixed with Pt electrode. So, mass of precipitate of Cu can be
determined as below :

Mass of Pt metals = (mass of initial Pt) - (mass of Pt after electrolysis)

= 0,907 grams 0,172 grams
= 0,735 grams

Mass of Cu precipitate

= (mass of precipitate) (mass of Pt)

= 1,154 grams 0,735 grams
= 0,419 grams

Percentage of Cu in sample
Percentage of Cu

= 100 x 0,419 x 100 %

25
50
= 3,352 %

2. Current Efficiency
Current Efficiency

= mass of precipited based on experiment x 100%

mass of precipited based on theory
= 0,419 x 100 %
0,210
= 199,52 %

H. DISCUSSION
An Analytical Chemistry II Lab-Work which had have been did on November
2, 2015 at Analytical Chemistry Laboratory of Yogyakarta State University was about
Electrogravimetry. The objective of this experiment was to do separation with
electrogravimetry method. Elektrogravimetry is a way in which substances are
investigated in the form of a metal deposited on the cathode by electrolysis. In this
experiment used electrodes in the form of nickel metal bowls as aluminum as the
cathode and the anode. As for the sample solution was used a solution of Cu (II) or
CuSO4.
In this elektrogravimetry experiment, the first thing to do is to clean the
electrode with dilute nitric acid, and then rinsing it with acetone and drain electrodes.
The next step is to weigh Nickel bowls / electrodes with analytical balance. Of the
weighing process, the mass obtained by 54,588 grams Nickel bowls. The next is to
make the sample solution CuSO4 by using a pipette 50 mL solution of Cu (II) light
blue clear and incorporated into the glass beaker which was then added 2 mL of
concentrated sulfuric acid and 1 mL of concentrated nitric acid and diluted with
distilled water to a volume of exactly 100 mL. The purpose of the addition of sulfuric
acid is to create an atmosphere of acid in solution. While the purpose of the addition
of concentrated nitric acid is as polarizer and prevent the occurrence of hydrogen gas
at the cathode which can disrupt the formation of a precipitate Cu. The reaction is as
follows:
NO3 + 10 H+ + 8e NH4+ + 3H2O
It should be noted that the nitric acid used should be free of nitrite and acid
levels also should not be too high because if the excess sludge occurs not want
attached. Saetelah make CuSO4 sample solution, then the next step is to perform
electrolysis. inserted into the sample solution nickel bowls until approximately 1/4
portion of the aluminum submerged by the sample solution. Aluminium is entered this
not to touch the walls of Nickel bowls because it will affect the flow measurement.
Metal aluminum adapter that is connected to the positive charged while connected to
the adapter Nickel bowls negatively charged. After that, start electrolysis by adjusting
the potential of 3 volts and a strong current of 0.2 A. read current flowing should not
be too large because later the resulting sediment deposition rough. But in the trial
resulting electrolysis for 52 minutes, the electrolysis was terminated. Adapaun
equation that occurs in this electrolysis are as follows :
Cathode:

Cu2+ + 2e Cu
2H+ + 2e H2

Anode :

2H2O (l) 4H+ (aq) + O2 (g) + 4e

During the process of electrolysis, also conducted tests on tembaga.Caranya is

by taking a few drops of solution which is then put into a test tube. Testing is done by

adding a reagent hexacyanoferrate (II). If at the time of testing, the solution changes
to brown, then still a positive solution containing Cu. Tests conducted until a solution
is not brown anymore, which means negative for Cu metal and the electrolysis was
stopped. Negative test for Cu is when it may no longer exist Cu (Cu sedimented all).
If the test indicates positive, then the reaction is :
2Cu2+ (aq) + [Fe(CN)6]4- (aq) Cu[Fe(CN)6] (s)
After testing for copper and show a negative result, then the next step is to
rinse the electrode with acetone and clean it with a dilute nitric acid solution, then dry.
The final step is to weigh Nickel bowls along with sediment by calculating the
difference between the weight of the sediment + Nickel minus nickel empty bowls
weighing so heavy precipitate obtained by 1,154 grams. Sediment weight is different
from the heavy deposition of Cu in theory, namely 0.21 grams. This difference is
probably due to:
1. Concentrated nitric acid is added too excessive so that sediment does not want
to stick and remain in solution
2. Aluminum metal dipped frequently into contact with the walls of Nickel bowls
3. Time used for electrolysis long enough as long as 52 minutes when tested with
a solution of hexacyanoferrate (II) still showed positive results (not all of Cu
precipitates)
4. The voltage that setted on 3 V was not stable
For current effiency can be calculated with formule below :
Current Efficiency

= mass of precipited based on experiment x 100%

mass of precipited based on theory
= 0,419 x 100 %
0,210
= 199,52 %

and we got a current effiency was about 199,52 %. The result of current effiency was
not common because the result more than 100%. That cause by the electrolysys
process of Pt wasnt completely happened, and also there was some Pt electrode
which broken and going down into the bottom of solution.

As for calculating the Cu content in the sample, using the formula below :
Percentage of Cu

= 100 x 0,419 x 100 %

25
50
= 3,352 %

Finally, we got percentage of Cu was about 3,352 %.

I. CONCLUSION
From the result of this experiment, we can conclude :
1. In an electrogravimetry process, metal of Cu precipitated in cathode with
electrolysis method.
2. The current eficiency which we got about 199,52 %.
3. Mass of precipitate of Cu about 0,419 grams.

J. TASKS
1. Mass of Cu based on Theory
W

=
=
=
= 0,21 grams

Mass of Cu based on Experiment

Mass of Precipitate

= (Mass of Nikel bowls+precipitate) Mass of Nikel

Bowls
= 55,712 grams 54,558 grams
= 1,154 grams

Because there was decreasing of mass of Pt electrode, so, a precipitate which

produced was mixed with Pt electrode. So, mass of precipitate of Cu can be
determined as below :

Mass of Pt metals = (mass of initial Pt) - (mass of Pt after electrolysis)

= 0,907 grams 0,172 grams
= 0,735 grams

Mass of Cu precipitate

= (mass of precipitate) (mass of Pt)

= 1,154 grams 0,735 grams
= 0,419 grams

Percentage of Cu in sample
Percentage of Cu

= 100 x 0,419 x 100 %

25
50
= 3,352 %

2. Current Efficiency
Current Efficiency

= mass of precipited based on experiment x 100%

mass of precipited based on theory
= 0,419 x 100 %
0,210
= 199,52 %

K. REFERENCES
Basset, J. dkk. 1994. Buku Ajar Vogel Kimia Analisis Kuantitatif Anorganik. Jakarta:
Penerbit Buku Kedokteran EGC.
Day, R.A. 2002. Kimia Analitik II. Malang : UM Press.
Soebagio, dkk. 2003. Kimia Analitik II. Malang: UM Press.
Sudjadi. 1980. Metode Pemisahan. Yogyakarta : Kanisius.
Tutik P, Regina. 2010. Petunjuk Praktikum Kimia Analisis II. Yogyakarta: FMIPA
UNY.
Vogel. 1990. Buku Teks Analisis Anorganik Kuantitatif Makro dan Semimikro.
Jakarta: Kolman Media Pustaka.