A.

Title
: Electrogravimetry
B. Date
: Monday, 20th May 2013
C. Purpose of experiment :
Separating and determining degree of Cu 2+ and Zn2+ in quotation using
electrogravimetry
D. Basic theory
:
Electrogravimetry is a method used to separate and quantify ions of a substance, usually
a metal. In this process, the analyte solution is electrolyzed. Electrochemical reduction
causes the analyte to be deposited on the cathode. The cathode is weighed before and
after the experiment, and weighing by difference is used to calculate the amount of
analyte in the original solution. Controlling the potential of the electrode is important to
ensure that only the metal being analyzed will be deposited on the electrode.
The process is similar to electroplating.It is known that in the phenomenon of
polarization the products of electrolysis exerts a back emf, which reduces the actual emf
of the cell. Thus electrolysis of an electrolyte is possible only when this back emf is
overcome. Let us consider a case in which two more platinum electrodes are placed in a
dilute solution of copper sulfate. If a source of potential is applied, no appreciable
current will flow through the system, until some minimum potential is applied after
which the current will increase as the applied potential increases. The applied voltage
which is just sufficient to overcome the back emf due to polarization and also to bring
about the electrolysis of an electrolyte without any hindrance is known as
decomposition potential.
In gravimetric analysis determination of metal concentration is depends on the
weighing process of the metal. But in electrogravimetery the metal concentration is
determined by using electrochemistry. It is an easy and accurate method. The
Electrogravimetric analysis is done by depositing the metal (whose concentration to
determine) on a pre-weighed electrode, and the concentration can be calculated from
the weight gained by that electrode.
For example determination of copper is the most important application of
electrogravimetery. The whole process is carried out in an electrolytic cell, which
consists of two electrodes an anode and a cathode with an external electrical energy
supply. On Cathode deposition of the metal takes place due to the reduction of metal,

and it is connected to the ve terminal of the energy source. On Anode oxidation occurs,
and it is connected to the +ve terminal of the energy source.
Now a days one of the electrode is used as a stirrer for stirring the analyte solution.
Fisher electrodes are used in this process.

Types of Electrogravimetric Analysis, There are two types Electrogravimetric

methods:
Constant Current Electrolysis:
In this process the current is kept constant, and potential is increased. Here no
control of the potential of the working electrode is exercised, and the applied cell
potential is held at a more or less constant level but provides a large enough current
to complete the electrolysis in a reasonable length of time. And a fixed amount of
the current can be passing between the anode and cathode. The limitation of
constant current electrolysis is it cannot be used for the separation of ion in a
solution containing single species.
Constant Potential Electrolysis:
It is the simplest way of performing an analytical electrolysis is to maintain the
applied cell potential at a constant value. It is more used in the separation of the
components from a mixture in which the decomposition potentials are not widely
separated.
For example the determination of copper from an acidic solution (either nitric acid
or sulphuric acid solution or mixture of two acids) at constant current. Suppose an
emf of 2-3 V is applied then the reaction taking place are given below.
At cathode:
Cu2+ + 2e- Cu

2H+ + 2e- H2
At anode:
4OH- O2 + 2H2O + 4eElectro deposition is governed by Ohm's law and Faraday's two laws of
electrolysis.
From ohms law the relation between current, voltage and resistance is given by,

Faraday's law states that,

a) In electrolysis the amount of substances liberated at the electrodes of a cell is
directly proportional to the amount of electricity which passes through the
solution.

Where:
m is the mass of the substance liberated at the electrode,
Z is the electrochemical equivalent,
I is the current in ampere,
t is the time in seconds.
b)The mass of substances liberated is directly proportional to the relative
equivalent weights of those substances at a particular quantity of electricity
applied.
In electrogravimetery the determination of metal is carried out by above two
procedures,
at constant
Wire
of Cu current or with controlled potential procedure. But constant
current is limited.
Cut the wire 2 piece @ 20 cm
E. Procedure

Polish with sand paper

1st wire is form as coil

Coil of Cu
Weigh it

Coil of Cu

Straight Wire

W0

Coil of
Cu
Connect with cable of electroanalyzer as
reduction part
Plug in the cable into source of current
The process do 3 minutes
Plug out the cable
Observe what happen in that coil
F. Tools and material

Syringe with H2O

Dip into acetone

Name
Amount
W1
Trafo Oven
500mA 2 minutes with 150
1 oC
Dioda, resistor and elco
1 set
Weigh
it
AC and DC cable
As needed
Beaker glass
100mLthe process with1 different time
Repeat
Crocodile nipper
1
Oven
1
Analytical weight
1
Copper plat
40 cm
CuSO4 0,01M
100mL
Aceton
Aquadest

G. Result of experiment
Procedure
Cathode

Anode

Hold
Hold
with
with
straight
spiral
electro
electrode
de
Turn on the
electroanaliser
Put the cathode and
anode into beaker
glass that had been
filled with NaOH
Set the potential 270
V
Do the electrolysis
3 minutes
Take the cathode
Put into acetone
Balance the weight
Result

Result
Mass of cathode
Wo = 2.728 gram

Hypothesis

W=

Conclusion
The amount of Cu that form
is 0.010 gram.

Wa1 = 2.735 gram

Wa2 = 2.744 gram
Wa3 = 2.754gram

So % of redemen is

Wa4 = 2.754 gram

Wa5 = 2.764 gram
W = Wa W0
W1 = 2.735 2.728
= 0.007 gram
W2 = 2.744 - 2.735
= 0.009 gram
W3 = 2.754 - 2.744
= 0.010 gram
W4 = 2.754 - 2.754
= 0 gram
W5 = 2.764 - 2.754
= 0.010 gram

= 0,0304 gram

32.8947%.

H. Analysis
The aim of this experiment is to separate and determine degree of Cu2+ and Zn2+ in
quotation using electrogravimetry. The first thing that we did is arrange the tools, that
consist of trafometer 500mA, AC and DC cable, beaker glass, resistor, and crocodile
nipper.
In this experiment we use Cu as an electrode, there are two electrode Cu, each of them
has 20 cm long. One of the electrode make as coil and the other one is straight. The
straight shape copper placed on the positive pole as oxidation side (anode), while coilshaped copper placed on the negative pole as reduction side (cathode). But, before we
use it, the copper as anode must be rubbed by sandpaper until the copper color more
shine, than the copper is washed by using aquadest and aceton, so the impurities
contained in the copper lost because aceton is volatile so the impurities can easily
volatile. After that, weight the copper and we got 2.728 g for the initial weight. This
coil is connect

in the cable of electroanalyzer

in reduction side. And the other

electrode in oxidation side. The solution that we used is CuSO4 0.001 M that flows
electricity have current 0.5 A by 4.5 volt. The time is 180 second.
The reaction that happened is electrolysis process is on:
Anode

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

Cathode

: Cu2+(aq) + 2e Cu(s)

After 180 second, put the coil-sharped electrode and dipped in acetone solution. Then
weight as W1. Repeat this step as many as 4 times and in different time is: t 2 = 600 se, t3
= 720 sekon, t4 = 840 sekon, t5 = 960 sekon.
Based on data result experiment, we get Wcu :

t = 3 menit Wcu = 0.007

t = 10 menit Wcu = 0.009
t = 12 menit Wcu = 0.010
t = 14 menit Wcu = 0
t = 16 menit Wcu = 0.010

Based on data result of experiment, we can calculate the WO2 dan WCu by formula :

I.

Diskusi
Based on data result of experiment that have been done to compare amount of
electron O2 and Cu through experiment by amount of electron that occur in reaction.
In this experiment, there are some differences of weight Cu based on experiment and
theory. In our experiment, we get the changing of weight in experiment is 0.007
gram, 0.009 gram, 0.010 gram, 0 gram, and 0.010 gram, but in our calculation we
should get the changing of weight is 0.03 gram, 0.102 gram, 0.122 gram, 0.1423
gram, and 0.1626 gram. It is happened because there are many mistakes. In this
experiment, we dip cathode in acetone. The characteristic of acetone can solute many
of compound even the compound is synthetic polymer. So, it is possible if the metal
is losing when it is dipped in acetone.
Besides that in experiment that we have done, in the certain time mass of Cu not
increase. This thing can influence to seek weight of electron Cu that involve in the
experiment.
Arrange the electrolysis tools that are less precise, or when do electrolysis process is
less true or less sanding the copper electrode by sandpaper are made result less
precise.

J.

Conclusion
Based on data result experiment that we have done, the weight that we have got is
not suitable with the theory. The weight of copper that we have gotten is 0.007 gram,
0.009 gram, 0.010 gram, 0 gram, and 0.010 gram. The average of weight copper we
have gotten is 0.0072 gram. While weight copper based on theory is 0.03 gram, 0.
102 gram, 0.122 gram, 0.1423 gram, 0.1626 gram. The average of weight copper
based on theory is 0.112 gram. So % of redemen is 32.8947%.

K. Reference
Azizah, Utiya. dkk. 2007.Panduan Praktikum Mata Kuliah Kimia Analitik II: DasarDasar Pemisahan Kimia. Surabaya: Universitas Negeri Surabaya.
Svehla, G. 1979. Vogel: Buku Teks Analisis Anorganik Kualitatif Makro dan
Semimikro. Edisi Kelima. Terjemahan oleh Ir. L. Setiono dan Dr. A. Hadyana
Pudjaatmaka. 1985. Jakarta: PT. Kalman Media Pustaka.

Underwood, A. L. dkk. 1986. Analisis Kimia Kuantitatif.

Erlangga.

L. Attachment
Weight of copper
Wo = 2.728 gram
Wa1 = 2.735 gram
Wa2 = 2.744 gram
Wa3 = 2.754gram
Wa4 = 2.754 gram
Wa5 = 2.764 gram
W = Wa W0
W1 = 2.735 2.728 = 0.007 gram
W2 = 2.744 - 2.735 = 0.009 gram
W3 = 2.754 - 2.744 = 0.010 gram
W4 = 2.754 - 2.754 = 0 gram
W5 = 2.764 - 2.754 = 0.010 gram
t 1= 180 sekon

PO2 = XO2 x P0O2 = 0,33 x 0,67 = 0,223 atm

t2 = 600 sekon

Edisi Keenam. Jakarta:

PO2 = XO2 x P0O2 =

x 0,67 = 0,2227 atm

t3 = 720 sekon

Tekanan oksigen PO2 = XO2 x P0O2 =

t4 = 840 sekon

x 0,67 = 0,5583 atm

PO2 = XO2 x P0O2 =

x 0,67 = 0,2206 atm

t5 = 960 sekon

PO2 = XO2 x P0O2 =

x 0,67 = 0,223 atm

M.

Pictures

Gambar 1.
Set of tools to do
electrogravimetry

Gambar 2.
Dipped electode into CuSO4
solution

Gambar 2.
Electode

Gambar 2.
Balancing

Saat penimbangan
Saat penimbangan